• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
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  • 优先权
    • 专利摘要:
    a method of cleaning equipment in place includes a plurality of cleaning cycles and, optionally, a rinse, where each cleaning cycle includes applying a first cleaning solution from a first supply tank through a first set of nozzles; and applying a second cleaning solution from a second supply tank through a second set of nozzles. the first cleaning solution can be applied for about (20) s to about (10) min. and the second cleaning solution for about 1 min. at about (60) min. the cleaning cycle can be repeated from (5) to (150) times and the first and second cleaning solutions can be recirculated during the process.
    公开号:BR112018002002B1
    申请号:R112018002002-8
    申请日:2016-07-29
    公开日:2021-09-08
    发明作者:Peter J. Fernholz；Christopher Nagel；Eric Schmidt；Anthony W. Erickson
    申请人:Ecolab Usa Inc.；
    IPC主号:
    专利说明:

    [001] This application is being filed July 29, 2016 as an International PCT application and claims the benefit of US Provisional Application Serial No. 62/199,616, filed July 31, 2015, which is incorporated by reference here in its entirety. FIELD
    [002] The present disclosure relates to clean-in-place methods and systems and compositions for use in clean-in-place methods. In particular, the present disclosure relates to clean-in-place methods that include applying a first and second cleaning composition to the surface being cleaned. FUNDAMENTALS
    [003] Clean-in-Place (“CIP”) protocols and methods are used to clean the internal surfaces and other internal components of equipment that cannot be easily disassembled. Examples of equipment that are typically cleaned using CIP methods include various tanks, evaporators, heat exchangers, pipes and other process equipment. CIP methods are particularly useful in industries that use feed stocks that spoil easily and/or that require a high level of hygiene, such as food and beverage, pharmaceuticals, cosmetics, brewery, fuel ethane and other similar industries. Dirt that contaminates equipment surfaces in these industries is characterized by its carbohydrate content (including cellulosic materials, monosaccharides, disaccharides, oligosaccharides, starches, gums, etc.), proteins, fats, oils, minerals and other materials and mixtures of complex materials that , when dried and/or heated, can form dirt and residues that are difficult to remove.
    [004] When the equipment is cleaned using a CIP protocol, the normal process must be stopped and the equipment emptied of any process materials. Therefore, CIP causes process downtime and, particularly with equipment that requires long cleaning times (up to 10 to 12 hours), performing CIP can place a large load on normal plant operations. Therefore, faster and more efficient CIP processes would be beneficial. It is against this foundation that the present disclosure is made. SUMMARY
    [005] A method for cleaning equipment in place includes a plurality of cleaning cycles and optionally a rinse where each cleaning cycle includes applying a first cleaning solution from a first supply tank through a first set of nozzles; and applying a second cleaning solution from a second supply tank through a second set of nozzles. The first cleaning solution can be applied for about 20 s to about 10 min. and the second cleaning solution for about 1 min. to about 60 min. The cleaning cycle can be repeated 5 to 150 times and the first and second cleaning solutions can be recirculated during the process.
    [006] The concentration of active ingredients in the first cleaning solution may be higher than the concentration of active ingredients in the second cleaning solution. The first and/or second cleaning solutions may include agents that provide a soil-stop effect. In some embodiments, the first and/or second cleaning solutions include a gas generating agent. BRIEF DESCRIPTION OF THE DRAWINGS
    [007] FIG. 1A is a spray dryer with a CIP system.
    [008] FIG. 1B shows a schematic representation of a CIP system.
    [009] FIG. 2 is a flowchart of a CIP method according to an embodiment.
    [0010] FIG. 3A shows a schematic representation of a CIP system used in the method of FIG. two.
    [0011] FIG. 3B shows a schematic representation of a CIP system used in the method of FIG. two.
    [0012] FIG. 4 is a graphical representation of the results of Example 2. DETAILED DESCRIPTION
    [0013] The present disclosure relates to clean-in-place methods and systems and compositions for use in clean-in-place methods. In particular, the present disclosure relates to clean-in-place methods which include alternately spraying a first composition and a second composition onto the surface being cleaned. In some embodiments, the first composition includes a gas generating composition.
    [0014] The term "about" is used herein in conjunction with numerical values to include normal variations in measurements as expected by those skilled in the art and is understood to have the same meaning as "approximately" and to cover a typical margin of error, such as + 5% of the declared value.
    [0015] The methods of the present disclosure may be particularly suitable for systems that include two or more spray systems, for example, a first spray system that is used to spray a product during normal operation and a second spray system that is used to spray cleaning solution during a CIP cleaning. The methods may also be suitable for systems that include a spray system that can be configured to extract from one or more storage containers, for example, a storage container that is used to store product in normal operation and a second storage container that is used to store cleaning solution.
    [0016] Many industrial processes that use CIP methods for cleaning experience difficult-to-remove soils that require long cleaning times. CIP processes can take several hours to complete, causing undesirable downtime as the production process cannot be operated simultaneously with the CIP process. Many food and beverage soils are particularly difficult to remove if the soil is thermally degraded because the material has been heated during processing. For example, products may have been heated to cook (eg to pasteurize), condense or dry. The term “thermally degraded” is used to refer to material that has been exposed to heat and, as a result, has undergone changes in the material's chemical structure, such as denaturation and crosslinking reactions of proteins, carbohydrates, fats and oils. Most food and beverage products include either protein, fat, carbohydrates or a combination thereof.
    [0017] A particularly challenging CIP cleaning application is a large vertical spray dryer used to dry dairy products (eg to produce dry powdered milk) or starch. These dryers are often tapered in shape and can be as large as 60 to 90 feet high and 12 to 18 feet in diameter at the top. In particular, spray dryers used to dry dairy products can accumulate large amounts of dry cooked product that includes protein, fat and carbohydrates on the inner walls of the dryer chamber. A schematic drawing of a typical spray dryer 100 is shown in FIGURE 1A. The wet product is introduced through spray nozzles 127 at the top of the drying chamber 110, where the product is atomized into small droplets. As the droplets fall into drying chamber 110, hot air (typically about 250°F) is counter-drained from the bottom to dry the wet particles. Dry particles are collected at the bottom of the drying chamber and can be removed for further processing (eg in a cyclone or fluid bed dryer). However, during the process, part of the product settles and remains on the walls 111 of the chamber 110, rather than falling to the bottom and over time develops a difficult-to-remove layer of cooked dirt.
    [0018] The spray dryer 100 may include a cleaning system 130 which is used for CIP cleaning. A simplified schematic of cleaning system 130 is shown in FIGURE 1B. A similar cleaning system 130 can be used with other types of equipment such as other types of dryers (eg fluid bed dryers, cone dryers or drum dryers), tanks, evaporators, heat exchangers, tubes, separators , homogenizers, pasteurizers, cooling towers, cabinet ovens, combi ovens, belt sprayers, paper mill equipment, refinery distillation towers and other process equipment. The cleaning system 130 may include a cleaning fluid supply tank 131 that is connected to spray nozzles 138 by line 135. The spray nozzles 138 may be constructed to spray cleaning fluid at high pressure on the inner walls 211 of the 210 container for cleaning cooked dirt. The exemplary spray dryer system in FIGURE 1A includes spray nozzles 137 on the sides and a central spray nozzle 136 in the middle of chamber 110.
    [0019] The cleaning fluid can be supplied to the spray nozzles 136, 137 or 138 at a high pressure supplied by a pump 133. The pump 133 must be selected to supply a pressure required by the particular spray nozzles. For example, a rotating spray nozzle typically requires a higher pressure than regular spray nozzles. Nozzle configuration can be modified to optimize nozzles for selected cleaning solution. Movable nozzles can be used to ensure coverage of hard-to-reach areas of the equipment such as bends, elbows or corners.
    [0020] Cleaning can be done at a temperature of about 100°F or higher, depending on the dirt to be removed. The cleaning system can include a heater to bring the cleaning solutions to the desired temperature.
    [0021] The spent cleaning fluid from the CIP spray is collected at the bottom and can be circulated back to the supply tank 131 through a recirculation line 139. The spent cleaning fluid can be filtered before reuse. In some embodiments, the recirculation line 139 may further comprise a screen or filter to remove particulate matter, e.g., dirt particles removed by the cleaning fluid.
    [0022] A typical CIP cycle to clean a dairy spray dryer using existing methods can take as long as 12 to 18 hours, during which a cleaning solution of about 0.5 to 2% caustic is circulated through the CIP system . Due to the larger size of the drying chamber, the CIP system consumes large amounts of water. In some applications, the cleaning solution cannot be effectively recirculated because of the type of dirt being removed. For example, soils that include high concentrations of starch (eg in a starch spray dryer) cause starch-based and starch-based reaction products (eg gelatinized starch) to accumulate in the cleaning solution, so that the cleaning solution cannot be recirculated.
    [0023] The methods of the present disclosure can be particularly useful for cleaning soils containing proteins, carbohydrates and/or fats in spray dryers or other equipment. In accordance with one embodiment and generally shown in the flowchart of FIGURE 2, the method includes a CIP cycle of applying a first cleaning solution from a first spray system, applying a second cleaning solution from a second spray system, and repeating the cycle. CIP until a desired level of cleanliness is reached. Before starting the CIP cycle, the system (eg, the product supply tank) is emptied of any product that could be left in it, and the dryer or other equipment can be pre-rinsed with water or other solvent. Pre-rinsing by product nozzles can also help to remove remaining product from product nozzles. The process can also include any other contact step in which a fluid, acidic or basic rinse solvent or other cleaning component, such as hot water, cold water, etc., can be contacted with the equipment at any step or between steps during the process. The CIP cycle can also include a final rinse step, for example with water or a composition comprising an antimicrobial agent, to prepare the system for subsequent food grade production. If the dirt load of the recirculating cleaning solution becomes too high, the fill tank can be drained and refilled with fresh cleaning solution.
    [0024] Beneficially, the first cleaning solution can provide a dirt stopping effect making the second cleaning solution more effective. The term “dirt stop effect” is used here to refer to loosening, destroying and/or displacing dirt on a surface. Without wishing to be bound by theory, it is believed that when the first cleaning solution penetrates a layer of dirt, the cleaning action generated by the first cleaning solution interrupts the dirt matrix, breaks the dirt layer and loosens the surface. The interrupted dirt can then be removed by using the second cleaning solution providing high pressure impact forces. In some embodiments, the soil-stop effect is brought about by a reaction between active ingredients in the first cleaning solution and the second cleaning solution. In some embodiments, the cleaning action is generated by bubbles or foaming.
    [0025] According to at least one embodiment, the first cleaning solution can be applied from a first supply tank and the second cleaning solution can be applied from a second supply tank. For example, in some embodiments used to clean a spray dryer, the first cleaning solution is drawn from product supply tank 121 and sprayed through product spray nozzles 127 on top of a spray dryer for a first duration of time and the second cleaning solution is drawn from the CIP supply tank (cleaning fluid supply tank 131 in FIGURE 1A) and sprayed through the CIP cleaning nozzles 136, 137 for a second duration of time. The vertical spray dryer (shown in FIGURE 1A) lends itself well to the present method because it already includes two sets of spray nozzles. Other types of equipment such as other dryers, tanks, evaporators, heat exchangers, tubes, separators, homogenisers, pasteurizers, cooling towers, cabinet ovens, combi ovens, belt sprayers, paper mill equipment, distillation towers refinery and other process equipment could be equipped with a second set of spray nozzles to accommodate the present cleaning method. Alternatively, the spray nozzles can be adapted to extract cleaning solutions from two separate supply tanks.
    [0026] The first and second cleaning solutions can be independently applied at room temperature or at an elevated temperature. The first and second cleaning solutions can also be independently at an elevated temperature. For example, if a high pressure CIP cleaning nozzle is used, the solution applied through the nozzle can be applied at a pressure ranging from 50 psi up to and exceeding 150 psi. In some embodiments, the second cleaning solution is applied through CIP cleaning nozzles at a pressure of about 100 to about 500 psi, or about 150 to about 300 psi. Product spray nozzles 127 in a typical spray dryer may be non-pressurized and are not necessarily adapted to obtain complete coverage of the inner walls 111 of drying chamber 110. However, counter-flow air may optionally be used to improve coverage. the walls with the cleaning solution (eg the first cleaning solution). The nozzle configuration can also be adapted, or the system can be equipped with different types of nozzles to achieve a desired cleaning result, such as better coverage, high pressure, spin or foaming nozzles.
    [0027] According to an alternative embodiment used in a cleaning system 230 shown in FIGURE 3A, the first cleaning solution is provided in a first supply tank 121 and the second cleaning solution is provided in a second supply tank 131 and each tank is connected to and is in fluid communication with the nozzles 138 through lines 125, 135. The system 330 may include a switch 410 (e.g., a switch valve) for switching the supply to the nozzles 138 of the first fuel tank. supply 121 to the second supply tank 131 and back. During cleaning, the nozzles 138 may first be filled with the first cleaning solution from the first supply tank 121 for a first duration of time, then with the second cleaning solution from the second supply tank 131 for a second duration of time. .
    [0028] In another alternative embodiment shown in FIGURE 3B, the cleaning system 330 includes two or more separate circuits 331, 332, each with a supply tank 121, 131, pump 123, 133, supply line 125, 135, spray nozzles 128, 138 and optionally recirculation line 129, 139. The first cleaning solution can be supplied in the first supply tank 121 of the first cleaning circuit 331 and the second cleaning solution in the second supply tank 131 of the second cleaning circuit 332. In a typical spray dryer system, only the second circuit 332 (generally the CIP circuit) includes a recirculation line 139. Cleaning solution from the first supply tank 121 would be recirculated to the second circuit 332 through of the recirculation line 139. In some embodiments, the first circuit 332 also includes a recirculation line 139 and the first and second cleaning solutions can be recirculated to r the first supply tank 121.
    [0029] CIP tanks supplied in typical spray dryer systems can be large, up to hundreds of gallons in size. Any chemical that is included in a cleaning solution in the CIP fill tank is diluted with a large volume of water and therefore needs to be included in a substantial amount. Supplying the chemistry at a high concentration in the large tank can be cost prohibitive. By providing a cleaning solution in a separate supply tank (ie, the first supply tank), the solution can be supplied at a higher concentration because the distribution flow rate is typically much lower than the CIP supply tank . The present method provides a cost-effective way to supply a concentrated heavy duty cleaner for the CIP cycle.
    [0030] The first and second solutions may comprise different chemistries, different concentrations or be the same. In one embodiment, the first cleaning solution has a different and more concentrated chemistry than the second cleaning solution and is supplied to nozzles 138 for a shorter duration of time than the second cleaning solution. In another embodiment, the first cleaning solution comprises the same chemistry as the second cleaning solution. However, the first cleaning solution may have a higher concentration of active ingredients than the second cleaning solution or vice versa. The first and second cleaning solutions can also be applied at different temperatures and one or both cleaning solutions can be applied at either ambient or elevated temperatures. The temperature of each cleaning solution can be adjusted based on the dirt to be removed and/or the chemistry in the cleaning solution.
    [0031] In one embodiment, the first and second cleaning solutions have the same chemistry, but the first cleaning solution is more concentrated than the second cleaning solution. Used cleaning solution can be collected after spraying, optionally filtered to remove solid particles and directed to one of the supply tanks, eg the second supply tank. If the first cleaning solution is more concentrated and the used solution is collected and directed to the second supply tank, mixing the first cleaning solution used with the second cleaning solution in the tank would make the second cleaning solution more concentrated in all the plurality of cycles.
    [0032] In one embodiment, the first and second cleaning solutions have different chemistries and the first cleaning solution may also comprise a higher concentration of active ingredients than the second cleaning solution. If the first used cleaning solution is collected after spraying and optionally filtered and directed to the second supply tank, the components (eg the active ingredients) of the first cleaning solution may react with the components (eg the active ingredients) of the second cleaning solution and/or may outweigh the components of the second cleaning solution. For example, if one of the first and second cleaning solutions is basic and the other is acidic, the acid and base can react together when mixed. In such a case, the second cleaning solution can be replenished during or after the cleaning procedure.
    [0033] In certain embodiments, a third, fourth or subsequent cleaning solution can be used. For example, in a first part of the cleaning cycle, the first and second cleaning solutions are applied and after applying the first and second cleaning solutions to the surface, the supply tanks can be emptied and provided with third and/or fourth cleaning solutions to be applied in a second part of the cleaning cycle. Alternatively, additional supply tanks can be provided and third, fourth, or consecutive cleaning solutions can be provided in the additional tanks.
    [0034] The chemistry in the cleaning solutions can be selected based on the dirt to be removed. For example, a combination of peroxide and surfactant followed by alkali can be effective in cleaning solids that contain protein, carbohydrates and/or starch. Grease-containing solids can benefit from adding a solvent to the cleaning solution. Enzymes can be used to scavenge solids containing, for example, protein or starch.
    [0035] In the case of the dairy spray dryer (FIGURE 1A), a typical CIP solution is a relatively dilute caustic that is sprayed at high volume to clean chamber 110. However, according to one embodiment of the present method, because Since product spray nozzles 127 are connected to a product supply tank 121, a different and advantageously more concentrated chemistry can be applied through product spray nozzles 127. In an exemplary embodiment, a concentrated pretreatment chemistry is applied from the product supply tank 121 through the product spray nozzles 127 on the walls 111 of the dryer chamber and a dilute cleaning solution (e.g., a CIP solution comprising 0.1 to 2% caustic) is then applied from cleaning fluid supply tank 131 through CIP spray nozzles 136, 137. Pretreatment cycle and CIP application can be repeated multiple times and can m optionally be followed by a clean water rinse. TIME
    [0036] The present method preferably includes a plurality of application or cleaning cycles, where each cycle comprises applying the first cleaning solution for a first duration of time and applying the second cleaning solution for a second duration of time. The plurality of application cycles can be any suitable number of cycles, such as 3 to 200 cycles, 5 to 150 cycles, 10 to 100 cycles, 20 to 75 cycles, or 30 to 60 cycles.
    [0037] The application time duration of the first and second cleaning solutions can be adjusted based on the chemistries used in each cleaning solution, the concentration of the chemical used, and the type and amount of dirt that needs to be removed. In some modalities, the first time duration is shorter than the second time duration. For example, the first cleaning solution can be applied for about 30 s to about 20 min., about 45 s to about 15 min., about 1 to about 10 min., about 90 s to about 5 min. or any suitable length of time. In some modes, the first time duration is at least 20 s, 30 s, 40 s, 50 s, 60 s, 90 s, 2 min., 2 min. 30 s, 3 min., 4 min., or 5 min. or longer. In some modalities the first time duration is not more than 60 min., 30 min., 25 min., 20 min., 15 min., 10 min., 8 min., 7 min., 6 min., 5 min. 4 min., 3 min., 2 min. 30 s or 2 min.
    [0038] The method may optionally include a soak time (i.e. a delay) between the application of the first cleaning solution and the second cleaning solution. Soaking time can be from 0 to about 5 min. or from 0 to about 3 min. of duration. In some embodiments, there is essentially no delay between the application of the first cleaning solution and the second cleaning solution, except possibly for a minimal delay caused by stopping one spray system and starting another.
    [0039] The second time duration can be any time length adjusted based on the chemistry and dirt to be removed. The second length of time can be from about 1 to 150 min., about 1 to 120 min., about 1 to 90 min., about 1 to 60 min., about 2 to 45 min., about 3 to 30 min., about 5 to 20 min. or about 10 to 18 min.
    [0040] The cleaning cycle may be repeated any suitable number of times, such as 3 to 200 times, 5 to 150 times, 10 to 100 times. In an exemplary modality, the first time duration is about 3 to 5 min. and the second time duration is about 13 to 17 min. and the cycle is repeated about 40 to 50 times. The cleaning cycles follow one another in rapid succession so that the next cleaning cycle begins essentially immediately after the previous cleaning cycle is completed or a minimal delay as allowed by equipment operation. For example, the delay time can be up to about a few minutes (for example, about 1, 2, 3, 4, 5 or 6 minutes). In some cases, there is no lag time, or the lag time is virtually non-existent (ie, about 0 minutes or less than 30 seconds or less than 60 seconds). The plurality of cleaning cycles (eg 3 to 200 cycles, 5 to 150 cycles or 10 to 100 cycles) forms a CIP cleaning case, where normal use of the equipment (eg production) is interrupted for the duration of the cleaning and does not start until cleaning is complete. COMPOSITION
    [0041] Any suitable cleaning chemistries can be used to provide the first and second cleaning solutions used in the method. The first and second cleaning solutions can comprise the same or different chemicals and can have the same or different concentrations. In some embodiments, the first cleaning solution is different from the second cleaning solution and/or is more concentrated. For example, the first cleaning solution may comprise the active ingredients at a concentration of up to 20% by weight, 18% by weight, 16% by weight, 15% by weight, 14% by weight, 13% by weight, 12% by weight, 11% by weight or up to 10% by weight. In at least some of the embodiments, the first cleaning solution comprises at least 2% by weight, 3% by weight, 4% by weight, 5% by weight, 6% by weight, 7% by weight, 8% by weight, 9% by weight or at least 10% by weight of active ingredients. The term "active ingredients" is used here to refer to ingredients that actively contribute to cleansing as opposed to ingredients that are used to dilute or otherwise formulate (eg, thicken, stabilize, color, preserve, etc.) a composition. In some embodiments, the second cleaning solution comprises from 0.1 to 8% by weight, from 0.2 to 6% by weight, from 0.2 to 5% by weight, from 0.2 to 4% by weight, from 0.3 to 3% by weight, from 0.4 to 2.5% by weight or from 0.5 to 2% by weight of active ingredients. For example, the second cleaning solution can be a CIP cleaning solution including about 0.1 to 5% by weight or about 0.5 to 2% by weight caustic (NaOH) in water.
    [0042] In some embodiments, the first cleaning solution comprises an oxidizing agent or an oxidizer, such as a peroxide, peroxyacids or other peroxygen compound. The resulting solution is particularly effective against protein and starch soils. Furthermore, the reaction of oxygen compounds with dirt, especially when combined with an alkaline source, creates vigorous mechanical action on and within the dirt, which enhances dirt removal.
    [0043] Suitable oxidants include chlorites, bromine, bromates, bromine monochloride, iodine, iodine monochloride, iodates, permanganates, nitrates, nitric acid, borates, perborates and gaseous oxidants such as ozone, oxygen, chlorine dioxide, chlorine and derived from them. Peroxygen compounds which include peroxides and various percarboxylic acids, including percarbonates, are suitable.
    [0044] Peroxycarboxylic (or percarboxylic) acids generally have the formula_R(CO3H)n, where, for example, R is an alkyl, arylalkyl, cycloalkyl, aromatic or heterocyclic group, and n is one, two or three and named preceding the parent acid with “peroxy”. The R group can be saturated or unsaturated, as well as substituted or unsubstituted. In medium chain peroxycarboxylic (or percarboxylic) acids R is a C5-C11alkyl group, a C5-C11 cycloalkyl, a C5-C11arylalkyl group, a C5-C11aryl group or a C5-C11 heterocyclic group; and n is one, two or three. In short chain fatty acids, R is C1-C4 and n is one, two, or three.
    [0045] Examples of peroxycarboxylic acids include peroxypentanoic acid, peroxyhexanoic, peroxyheptanoic, peroxyoctanoic, peroxynonanoic, peroxyisononanoic, peroxidecanoic, peroxyundecanoic, peroxidodecanoic, peroxyascorbic, peroxyadipic, peroxycitric, peroxypymelic and the like.
    Branched-chain peroxycarboxylic acids include peroxy-isopentanoic, peroxy-isononanoic, peroxy-iso-hexanoic, peroxy-iso-heptanoic, peroxy-iso-octanoic, peroxy-isononanoic, peroxy-isodecanoic, peroxy-isoundecanoic, peroxyneo-hexanoic , peroxyneononanoic, peroxyneododecanoic, mixtures thereof and the like.
    Typical peroxygen compounds may include hydrogen peroxide (H2O2), peracetic acid, peroctanoic acid, a persulfate, a perborate, or a percarbonate.
    [0048] The amount of oxidant in the pretreatment solution can be at least 0.01% by weight and less than 2% by weight. In some embodiments, the cleaning solution comprises from about 0.01 to 1% by weight; about 0.05 to about 0.50% by weight; about 0.1 to about 0.4% by weight, or about 0.2 to about 0.3% by weight of oxidant. If the composition also comprises an acid, suitable oxidant to acid ratios are generally 1:1 to 1:50, 1:2 to 1:40, 1:3 to 1:30, 1:4 to 1: 25, or from 1:5 to 1:20. In an exemplary embodiment, the cleaning solution comprises 0.25% by weight to 10% by weight of phosphoric acid and 50 to 5,000 ppm (0.005% by weight to 0.5% by weight) of hydrogen peroxide or, in particular , about 0.75% by weight of phosphoric acid and about 500 ppm (0.05% by weight) of hydrogen peroxide (a 1:15 ratio of oxidant:acid).
    Suitable acids include phosphoric acid, nitric acid, hydrochloric acid, sulfuric acid, acetic acid, citric acid, lactic acid, formic acid, glycolic acid, methane sulfonic acid, sulfamic acid and mixtures thereof. When the acid is used in combination with an oxidant, the cleaning solution can comprise about 0.1 to about 12% by weight, about 0.2 to about 10% by weight, about 0.3 to about from 8.0% by weight, about 0.5 to about 6.0% by weight, about 0.8 to about 4.0% by weight, about 1.0 to about 3.0% by weight or about 1.5% to about 2.5% acid.
    [0050] In an embodiment where the first cleaning solution contains hydrogen peroxide and the second cleaning solution contains sodium hydroxide, the cleaning cycle of the first cleaning solution followed by the second cleaning solution creates oxygen bubbles formed by the destruction of the hydrogen peroxide. Oxygen bubbles can be effective in breaking up cooked dirt, such as dirt formed in a spray dryer used to produce dry milk or starch.
    [0051] According to an embodiment, the first cleaning solution may include a gas generating solution that generates carbon dioxide or other gas on or in the dirt to provide the dirt-stop effect. The gas generating solution may comprise at least a first gas generating compound and a second gas generating compound, where the first and second gas generating compounds react together to generate gas. For example, the gas generating solution may comprise a source of salt producing carbon dioxide and acid. Exemplary non-carbon dioxide gases that can be generated by the gas-generating solution include chlorine dioxide, chlorine, and oxygen.
    Suitable carbon dioxide producing salts include, for example, carbonate salt, bicarbonate salt, percarbonate salt, a sesquicarbonate salt and mixtures thereof. The carbon dioxide producing salt can be a carbonate, bicarbonate, percarbonate or sesquicarbonate salt of sodium, potassium, lithium, ammonium, calcium, magnesium or propylene. In some embodiments, the salt is selected from sodium carbonate, sodium bicarbonate, sodium percarbonate, sodium sequicarbonate; potassium carbonate, potassium bicarbonate, potassium percarbonate, potassium seqicarbonate; lithium carbonate, lithium bicarbonate, lithium percarbonate, lithium sequicarbonate; ammonium carbonate, ammonium bicarbonate, calcium carbonate, magnesium carbonate, propylene carbonate and mixtures thereof. The cleaning solution may comprise about 0.1 to 7.0% by weight, about 0.2 to about 5.0% by weight or about 0.3 to about 3.0% by weight of the salt. of carbon dioxide production.
    [0053] Gas generation solutions that produce a chlorine-containing gas (eg, chlorine dioxide) may include, for example, sodium hypochlorite and an acid. In some embodiments, the gas generation solution produces two or more different gases, for example, carbon dioxide and chlorine-containing gas. Such a gas generation solution may contain, for example, a carbon dioxide producing salt (eg a carbonate salt) and sodium hypochlorite.
    [0054] The second gas generating compound can be any suitable compound that is capable of reacting with the first gas generating compound to generate gas. For example, the second gas generating compound could be an acid. Exemplary acids include phosphoric acid, nitric acid, hydrochloric acid, sulfuric acid, acetic acid, citric acid, lactic acid, formic acid, glycolic acid, methane sulfonic acid, sulfamic acid and mixtures thereof. The amount of acid can be adjusted based on various considerations, such as the acid selected, the amount and type of first gas generating compound, and the dirt to be removed. The cleaning solution may comprise from about 0.1 to about 10% by weight, from about 0.2 to about 8.0% by weight, about 0.3 to about 6.0% by weight, about 0.5 to about 5% by weight, about 0.8 to about 4% by weight, about 1.0 to about 3.0% by weight, or about 1.5 to about 2 .5% acid by weight. In an exemplary embodiment, the acid comprises a strong mineral acid, for example, phosphoric, nitric or sulfuric acid or a combination thereof and is present at about 1.0, 1.5, 2.0, 2.5 or 3 0.0% by weight.
    [0055] According to some embodiments, the first and/or the second cleaning solutions comprise a catalyst. Useful catalysts include, for example, transition metal complexes (eg, manganese, molybdenum, chromium, copper, iron or cobalt complexes). Exemplary sources of manganese ions include, but are not limited to, manganese(II) sulfate, manganese(II) chloride, manganese(II) oxide, manganese(III) oxide, manganese(IV) oxide, acetate manganese (II) and combinations thereof. An exemplary source of iron includes iron gluconate. In some embodiments, cleaning may be more efficient at a lower temperature (for example, at temperatures between 100°F and 130°F) and the inclusion of a catalyst in the cleaning solution can help induce the formation of gas bubbles . For example, when using a peroxide solution to clean starch residue, iron gluconate catalyst can be used to accelerate the degradation of peroxide compounds at lower temperatures to increase the generation of gas bubbles.
    [0056] In some embodiments, the first cleaning solution does not contain a gas generating composition. In such solutions, the cleaning effect can be achieved, for example, by a combination of one or more solvents and one or more surfactants or using one or more enzymes. In some embodiments, the first cleaning solution contains an enzyme and/or a surfactant and the second cleaning solution contains a gas generating composition.
    [0057] In an exemplary embodiment, a dual-function surfactant can be used. A cleaning solution comprising a nonionic surfactant can be sprayed at a temperature that is below the cloud point of the nonionic surfactant, causing the cleaning solution to foam and adhere better to the surface of the equipment being cleaned, thus increasing contact time between the surface and the cleaning solution. A subsequent cleaning solution (eg second cleaning solution) can then be applied at a temperature that is above the cloud point of the nonionic surfactant changing the behavior of the nonionic surfactant to a defoamer. OTHER COMPONENTS
    [0058] The first and second cleaning solutions (collectively "cleaning solutions") may also comprise alkaline components, surfactants, solvents, builders and additional components. Suitable alkaline components include any alkaline components typically used in cleaning compositions, including NaOH, KOH, triethanol amine (TEA), diethanol amine (DEA), monoethanolamine (MEA), carbonates, bicarbonates, percarbonates, sequicarbonates, morpholine, sodium metasilicate, potassium silicate, etc.
    [0059] Suitable surfactants that can be used in cleaning solutions include anionic, cationic, nonionic and zwitterionic surfactants. The cleaning compositions can comprise about 0.01 to about 3% by weight, about 0.05 to about 2% by weight or about 0.1 to about 0.5% by weight of surfactants. The surfactant can be a combination of surfactants. In one embodiment, at least one of the surfactants is nonionic. Non-Ionic Surfactants
    [0060] In some embodiments, the surfactant comprises a non-ionic surfactant. Non-ionic surfactants improve dirt removal and can reduce the contact angle of the solution on the surface being treated.
    [0061] Examples of suitable nonionic surfactants include alkyl-, aryl- and arylalkyl-, alkoxylates, alkylpolyglycosides and their derivatives, amines and their derivatives and amides and their derivatives. Additional useful nonionic surfactants include those having a polyalkylene oxide polymer as a portion of the surfactant molecule. Such nonionic surfactants include, for example, polyoxyethylene and/or polyoxypropylene glycol ethers capped with chlorine, benzyl, methyl, ethyl, propyl, butyl and other alkyl capped with fatty alcohols; non-ionic free polyalkylene oxide, such as alkyl polyglycosides; sorbitan sucrose esters and their ethoxylates; alkoxylated ethylene diamine; carboxylic acid esters such as glycerol esters, polyoxyethylene esters, ethoxylated and glycol esters of fatty acids and the like; carboxylic amides such as diethanolamine condensates, monoalkanolamine condensates, polyoxyethylene fatty acid amides and the like; and ethoxylated amines and ether amines and other similar nonionic compounds. Silicone surfactants can also be used. Nonionic surfactants having a polyalkylene oxide polymer moiety include C6 C24 alcohol ethoxylates nonionic surfactants having 1 to about 20 ethylene oxide groups; C6-C24 alkylphenol ethoxylates having 1 to about 100 groups of ethylene oxide; C6-C24 alkylpolyglycosides having 1 to about 20 glycoside groups; C6-C24 fatty acid ester ethoxylates, propoxylates or glycerides; and C4-C24 mono or dialkanolamides.
    [0062] Examples of non-foaming, low-foaming, or defoaming nonionic surfactants include block polyoxypropylene-polyoxyethylene polymeric compounds with hydrophobic blocks on the outside (ends) of the molecule and nonionic surfactants modified by "capping" or "end" hydroxyl groups "end-blocking" by reaction with a small hydrophobic molecule or by converting terminal hydroxyl groups to chloride groups. Other examples of non-foaming nonionic surfactants include alkylphenoxypolyethoxyalkanols; polyalkylene glycol condensates; defoaming nonionic surfactants having a general formula Z[(OR)nOH]z where Z is alkoxylatable material, R is a radical, n is from 10 to 2000 and z is determined by the number of reactive oxyalkylatable groups and conjugated polyoxyalkylene compounds. Anionic Surfactants
    [0063] Anionic surfactants are useful as detersive surfactants, but also as gelling agents or as part of a gelling or thickening system, as solubilizers, and for hydrotopic effect and cloud bridge control. The composition can include one or more anionic surfactants. Suitable anionic surfactants for the present composition include: carboxylic acids and their salts, such as alkanoic acids and alkanoates, carboxylic acid esters (for example, alkyl succinates), ether carboxylic acids and the like; phosphoric acid esters and their salts; sulfonic acids and their salts, such as isethionates, alkylaryl sulfonates, alkyl sulfonates, sulfosuccinates; and sulfuric acid esters and salts thereof, such as alkyl ether sulfates, alkyl sulfates and the like. Cationic Surfactants
    [0064] Examples of suitable cationic surfactants include amines such as alkylamines and their salts, alkyl imidazolines, ethoxylated amines and quaternary ammonium compounds and their salts. Other cationic surfactants include sulfur (sulfonium) and phosphorus (phosphonium) based compounds that are analogous to amine compounds. Amphoteric and Zwitterionic Surfactants
    [0065] Amphoteric and zwitterionic surfactants include derivatives of secondary and tertiary amines, derivatives of heterocyclic secondary and tertiary amines or derivatives of quaternary ammonium compounds, quaternary phosphonium or tertiary sulfonium compounds. Ammonium, phosphonium or sulfonium compounds can be substituted by aliphatic substituents, for example, alkyl, alkenyl or hydroxyalkyl groups; alkylene or hydroxy alkylene; or carboxylate, sulfonate, sulfate, phosphonate or phosphate. Betaine and sultaine surfactants are exemplary zwitterionic surfactants for use in the present composition. builders
    [0066] Cleaning solutions may also include one or more builders. Builders include chelating agents (chelating agents), sequestering agents (sequestering agents), detergents, and the like. Builders can be used to stabilize the composition or solution. Examples of suitable builders include phosphonic acids and phosphonates, phosphates, aminocarboxylates and their derivatives, pyrophosphates, polyphosphates, ethylenediamine and ethylenetriamine derivatives, hydroxy acids, and mono, di and tricarboxylates and their corresponding acids. Other builders include aluminosilicates, nitrolacerates and their derivatives and mixtures thereof. Still other builders include aminocarboxylates, including salts of ethylenediaminetetraacetic acid (EDT A), hydroxyethylenediaminetetraacetic acid (HEDTA) and diethylenetriaminepentacetic acid. Preferred builders are water soluble. Particularly preferred builders include EDTA (including tetra sodium EDTA), TKPP (tripotassium polyphosphate), PAA (polyacrylic acid) and its salts, phosphonobutane carboxylic acid and sodium gluconate.
    Cleaning solutions may comprise about 0.05 to about 7% by weight, about 0.1 to about 5% by weight, about 0.2 to about 4% by weight, about 0.3 to about 3% by weight or about 0.5 to about 2% by weight of a builder. solvents
    [0068] Cleaning solutions can include one or more organic solvents. Suitable solvents include organic solvents such as esters, ether, ketones, amines, mineral alcohols, aromatic solvents, non-aromatic solvents and nitrated and chlorinated hydrocarbons. Preferred solvents include water-soluble glycol ethers. Examples of glycol ethers include dipropylene glycol methyl ether, diethylene glycol methyl ether, propylene glycol methyl ether and ethylene glycol monobutyl ether, commercially available as DOWANOL®DPM, DOWANOL®DM, DOWANOL®PM, and DOWANOL®EB, respectively, from Dow Chemical Company, Midland, MI. In certain embodiments, preferred solvents are non-flammable. Enzymes
    [0069] Enzymes can be used in cleaning solutions to break up soils such as starch, protein or oil based soils. Exemplary enzymes include proteases, amylases, lipases and other suitable enzymes. The composition can be adapted to the type of soil to be cleaned so that, for example, protein-based soils are bleached with proteases, starch-based solids with amylases and oil-based soils with lipases.
    [0070] The solutions may comprise additional components to provide desired properties or functionalities._For example, the solutions may include chelators or sequestering agents, sanitizers or antimicrobial agents, dyes, rheological modifiers (e.g., gelling agents, thickeners and the like), modifiers of pH (acids or bases), preservatives, processing aids, corrosion inhibitors or other functional ingredients.
    [0071] The pH of cleaning solutions can be adjusted based on choosing acid cleaning or alkaline cleaning for various types of dirt. In some embodiments, the first cleaning composition has a pH of 1.5 to 14. For example, if an alkaline cleaning composition is used, the pH can be in the range of 7 to 14, 8 to 13, or 9 to 12. Exemplary alkaline cleaning solutions include solutions comprising hydroxides or carbonates or other alkaline agents. In one embodiment, a first alkaline cleaning solution that contains a carbonate (eg, potassium carbonate) and has a pH above 7 may be accompanied by a second cleaning solution that is acidic (pH less than 7) that neutralizes the first cleaning solution and generates CO2 bubbles for improved mechanical cleaning action. If the used alkaline solution is directed to the second fill tank and mixed with the second cleaning solution there, the pH of the second cleaning solution can be adjusted by adding more acid throughout the process to maintain its acidic pH. If an acidic cleaning composition is used, the pH may be less than 7, less than 6.5, less than 6, less than 5.5, less than 5, less than 4 or less than 3. In some modalities the pH is between 1 and 6, or between 1.5 and 5. EXAMPLES Example 1
    [0072] The CIP method can be used to clean a large conical dairy spray dryer as shown in FIGURE 1. Various combinations of cleaning solutions can be prepared as shown in TABLE 1 In the table, each first cleaning solution is denoted “ A” and every second cleaning solution is denoted “B”. Each cleaning solution is prepared and mixed with water at the observed inclusion rate to produce a use solution. TABLE 1. Preparation of Cleaning Solutions.

    [0073] The various compositions (A/B) can also be combined so that cleaning solution A from Combination 1 can be combined with cleaning solution B from either Combination 2 or 3; cleaning solution A of Combination 3 can be combined with cleaning solution B of Combination 1 or 3 and cleaning solution A of Combination 3 can be combined with solution B of Combination 1 or 2.
    [0074] The resulting use solution concentrations are shown in TABLE 2. TABLE 2. Use solutions


    [0075] The cleaning cycle is started by emptying the product supply tank of any product, pre-rinsing the dryer with water through the product spray nozzles, filling the product supply tank with the first cleaning solution, dispensing first cleaning solution (A) from the product supply tank and applying through the product spray nozzles at about 45 gallons/min. for about 3 minutes. The second cleaning solution (B) is then delivered from a CIP supply tank and applied through CIP spray nozzles at about 100 gallons/min. and about 60 psi for about 15 minutes. Both cleaning solutions are recirculated back to the CIP fill tank. The cycle is repeated until a desired level of cleaning is reached. It is anticipated that the total cleaning time (the total duration of the plurality of cleaning cycles) is less than 10 hours, compared to the typical 12 to 18 hours using a conventional CIP method.
    [0076] In other modalities, the first cleaning solution (A) is applied for at least 20 s, 30 s, 40 s, 50 s, 60 s, 90 s, 2 min., 2 min. 30 sec, 3 min., 4 min. or 5 min. or longer and/or not more than 60 min., 30 min., 25 min., 20 min., 15 min., 10 min., 8 min., 7 min., 6 min., 5 min., 4 min., 3 min., 2 min. 30 s, or 2 min. The first cleaning solution (A) can be left to soak for 0 to about 5 min., or 0 to about 3 min. The second cleaning solution (B) is applied for about 1 to 150 min., about 1 to 120 min., about 1 to 90 min., about 1 to 60 min., about 2 to 45 min. , about 3 to 30 min., about 5 to 20 min. or about 10 to 18 min. The cleaning cycle (A+B) can be repeated any suitable number of times, such as 3 to 200 times, 5 to 150 times, 10 to 100 times or 40-50 times.
    [0077] In other embodiments, the cleaning method is used to clean other types of equipment, such as other types of dryers, ovens, tanks, cooling towers or conveyor belts. Example 2
    [0078] The cleaning method has been tested on dirt from dry milk powder. Solid Test Soil Pies (75 g each) were prepared from froth milk powder in test trays by adding 5% water to the froth milk powder and drying the mixture for 8 hours at 100°C. Test soils were treated in a pilot-scale Clean In Place (CIP) chamber to simulate cleaning conditions found in typical dairy product dryers.
    [0079] The test sample was treated with a pretreatment solution (cleaning solution “A”) delivered via atomizing nozzles for 10 minutes. Application through atomizing nozzles simulated application through product delivery spray nozzles in a dryer. The pretreatment solution was allowed to penetrate and act for another 10 minutes before washing. The pretreatment composition is shown in TABLE 3A. The control did not receive a pre-treatment. TABLE 3A. Pre-treatment composition (cleaning solution “A”)

    [0080] Both the test sample and the control were washed simultaneously in the CIP chamber for 45 minutes with 1.5% NaOH solution (cleaning solution “B”) at 65°C. Trays were removed, rinsed and weighed. Results are shown in TABLE 3b and FIGURE 4. TABLE 3B. Dirt Removal

    [0081] The results achieved with the control matched those observed in the real-world CIP of dairy dryer soils which are typically very challenging to remove. It was observed that application of the pretreatment composition dramatically increased dirt removal compared to NaOH alone.
    [0082] Although certain embodiments of the invention have been described, other embodiments may exist._Although the descriptive report includes a detailed description, the scope of the invention is indicated by the following claims. The features and specific acts described above are disclosed as illustrative aspects and embodiments of the invention. Various other aspects, modalities, modifications and equivalents thereof that, after reading the description in this document, may be suggested to those skilled in the art without departing from the spirit of the present invention or the scope of the claimed subject matter.
    权利要求:
    Claims (18)
    [0001]
    1. Method for cleaning equipment on site, the method characterized by the fact that it comprises a plurality of cleaning cycles, wherein the plurality of cleaning cycles comprises three or more cleaning cycles and wherein each cleaning cycle comprises: (a ) applying a first cleaning solution from a first supply tank (121) through a first set of nozzles (128); and (b) applying a second cleaning solution from a second supply tank (131) through a second set of nozzles (138).
    [0002]
    2. Method according to claim 1, characterized in that the equipment is selected from a dryer, a tank, a cooling tower, an oven or a belt.
    [0003]
    3. Method according to claim 1 or 2, characterized in that the equipment comprises a spray dryer (100).
    [0004]
    4. Method according to any one of claims 1 to 3, characterized in that step (a) comprises a first duration of time and step (b) comprises a second duration of time which is longer than the first duration of time.
    [0005]
    5. Method according to claim 4, characterized in that the first time duration is from 20 s to 10 min and in which the second time duration is from 1 min to 60 min.
    [0006]
    6. Method according to claim 4, characterized in that the first time duration is from 30 s to 5 min and in which the second time duration is from 5 min to 20 min.
    [0007]
    7. Method according to any one of claims 1 to 6, characterized in that the plurality of cleaning cycles comprises from 5 to 150 cycles, preferably from 10 to 100 cycles.
    [0008]
    8. Method according to any one of claims 1 to 7, characterized in that the first set of nozzles (128) consists of non-pressurized nozzles and that the second set of nozzles (138) comprises a high pressure nozzle.
    [0009]
    9. Method according to any one of claims 1 to 8, characterized in that the first and second cleaning solutions are recirculated to the second supply tank (131).
    [0010]
    10. Method according to any one of claims 1 to 9, characterized in that the first and second cleaning solutions comprise active ingredients and in which the first cleaning solution comprises active ingredients at a higher concentration than the second solution cleaning.
    [0011]
    11. Method according to claim 10, characterized in that the concentration of active ingredients in the first cleaning solution is between 4% and 20% by weight, preferably between 0.1% to 5% by weight.
    [0012]
    12. Method according to any one of claims 1 to 11, characterized in that the first cleaning solution comprises agents that provide a dirt-interrupting effect.
    [0013]
    13. Method according to any one of claims 1 to 12, characterized in that the first cleaning solution comprises one or more peroxygen compounds.
    [0014]
    14. Method according to claim 13, characterized in that the peroxygen compound is hydrogen peroxide, a peroxycarboxylic acid, a persulfate, a perborate, a percarbonate or a mixture thereof.
    [0015]
    15. Method according to any one of claims 1 to 14, characterized in that the first cleaning solution comprises an acid and/or a gas-forming agent.
    [0016]
    16. The method of claim 15, characterized in that the first cleaning solution comprises a gas-forming agent and wherein the gas-forming agent forms carbon dioxide or oxygen.
    [0017]
    17. Method according to any one of claims 1 to 16, characterized in that the second cleaning solution comprises a metal hydroxide.
    [0018]
    18. Method according to any one of claims 1 to 17, characterized in that one or both of the first and second cleaning solutions comprise a surfactant, a builder, and/or a solvent.
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    同族专利:
    公开号 | 公开日
    WO2017023762A1|2017-02-09|
    JP2018526200A|2018-09-13|
    MA42545A|2018-06-06|
    CO2018001471A2|2018-05-10|
    AU2016302929A1|2018-02-22|
    EP3328562A1|2018-06-06|
    PE20180469A1|2018-03-06|
    CL2018000274A1|2018-05-11|
    PH12018500244A1|2018-08-29|
    EP3328562A4|2019-06-12|
    ECSP18015365A|2018-10-31|
    RU2720001C2|2020-04-23|
    CN107847989A|2018-03-27|
    RU2018106883A3|2019-11-14|
    BR112018002002A2|2018-09-18|
    JP2021121432A|2021-08-26|
    PH12018500244B1|2018-08-29|
    US20170028449A1|2017-02-02|
    CA2994243A1|2017-02-09|
    RU2018106883A|2019-08-29|
    MX2018001382A|2018-06-15|
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    法律状态:
    2020-03-03| B06U| Preliminary requirement: requests with searches performed by other patent offices: procedure suspended [chapter 6.21 patent gazette]|
    2021-07-06| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    2021-09-08| B16A| Patent or certificate of addition of invention granted [chapter 16.1 patent gazette]|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 29/07/2016, OBSERVADAS AS CONDICOES LEGAIS. |
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    US201562199616P| true| 2015-07-31|2015-07-31|
    US62/199616|2015-07-31|
    PCT/US2016/044733|WO2017023762A1|2015-07-31|2016-07-29|Clean-place method and system and composition for the same|
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