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    • 专利摘要:
    The present invention provides a method for producing an aqueous dispersion suitable for use as a fire retardant additive to wood composite panels.
    公开号:BE1024872B1
    申请号:E2017/5167
    申请日:2017-03-17
    公开日:2018-07-31
    发明作者:Pieter Daeseleire；Herman Meynaerts
    申请人:Ecochem International, Naamloze Vennootschap；
    IPC主号:
    专利说明:

    (30) Priority data:
    30/12/2016 BE BE2016 / 5997 (73) Holder (s):
    ECOCHEM INTERNATIONAL, a public limited company
    2250, OLES
    Belgium (72) Inventor (s):
    DAESELEIRE Pieter 2250 OLEN Belgium
    MEYNAERTS Herman
    2250 OLES
    Belgium (54) A method of producing aqueous dispersion for use as a fire retardant additive for wood composite panels
    X : i (57) The present invention provides a method of producing an aqueous dispersion suitable for use as a fire retardant additive on wood composite panels.
    BELGIAN INVENTION PATENT
    FPS Economy, K.M.O., Self-employed & Energy
    Intellectual Property Office
    Publication number: 1024872 Filing number: BE2017 / 5167
    International classification: C09K 21/04 Date of issue: 31/07/2018
    The Minister of Economy,
    Having regard to the Paris Convention of 20 March 1883 for the Protection of Industrial Property;
    Having regard to the Law of March 28, 1984 on inventive patents, Article 22, for patent applications filed before September 22, 2014;
    Having regard to Title 1 Invention Patents of Book XI of the Economic Law Code, Article XI.24, for patent applications filed from September 22, 2014;
    Having regard to the Royal Decree of 2 December 1986 on the filing, granting and maintenance of inventive patents, Article 28;
    Having regard to the application for an invention patent received by the Intellectual Property Office on 17/03/2017.
    Whereas for patent applications that fall within the scope of Title 1, Book XI, of the Code of Economic Law (hereinafter WER), in accordance with Article XI.19, § 4, second paragraph, of the WER, the granted patent will be limited. to the patent claims for which the novelty search report was prepared, when the patent application is the subject of a novelty search report indicating a lack of unity of invention as referred to in paragraph 1, and when the applicant does not limit his filing and does not file a divisional application in accordance with the search report.
    Decision:
    Article 1
    ECOCHEM INTERNATIONAL, public limited company, Industrielaan 25, 2250 ÖLEN Belgium;
    represented by
    BRANTS Johan Philippe Emile, Pauline Van Pottelsberghelaan 24, 9051, GHENT;
    a Belgian invention patent with a term of 20 years, subject to payment of the annual taxes as referred to in Article XI.48, § 1 of the Code of Economic Law, for: Process for producing aqueous dispersion for use as a fire-retardant additive for wood composite panels.
    INVENTOR (S):
    DAESELEIRE Pieter, Industrielaan 25, 2250, OLEN;
    MEYNAERTS Herman, Industrielaan 25, 2250, OLEN;
    PRIORITY:
    30/12/2016 BE BE2016 / 5997;
    BREAKDOWN:
    Split from basic application:
    Filing date of the basic application:
    Article 2. - This patent is granted without prior investigation into the patentability of the invention, without warranty of the Merit of the invention, nor of the accuracy of its description and at the risk of the applicant (s).
    Brussels, 31/07/2018,
    With special authorization:
    BE2017 / 5167
    METHOD FOR PRODUCING AQUEOUS DISPERSION
    FOR USE AS A FIRE RETARDANT ADDITIVE FOR
    WOODEN COMPOSITE PANELS
    TECHNICAL AREA
    The invention relates to the technical field of methods of producing aqueous dispersions for use as a fire retardant additive for wood composite panels.
    BACKGROUND
    Wood composite panels are widely used in the construction industry. Both wood and these wood-based materials must meet high requirements for refractory properties. Various standards and requirements have been introduced in Europe that allow the fire properties of building materials to be compared (eg Euro classes). Characteristics such as non-flammability, flammability, flame spread, caioric value as well as the development of smoke and flaming droplets of the material are taken into account when classifying building materials in these classes.
    In order to meet these requirements and meet the highest quality standards, composite panels are often referred to during production as having compositions with fire retardant properties and optional! smoke suppressants.
    These compositions are often added as a dispersion during the production of these panels. However, fire retardant additives are known to have poor dispersion stability; relatively fast agglomeration can result in sedimentation, causing problems for both dispersion storage and piping dispersion. Thus, this poor dispersion stability requires the dispersion to be produced on-site, which requires panel manufacturers to have strict work schedules and further requires them to provide their own equipment for producing such dispersions themselves.
    BE2017 / 5167
    EP 2 585 849 A2 describes an aqueous dispersion comprising a flame retardant, a method of producing said dispersion and the use of said dispersion as a fire retardant additive for products having fire retardant properties. The products mentioned include wooden composite panels.
    However, there is a constant need in the area for fire-retardant dispersions with increasingly better stability. Finally, this would make it possible to produce the aforementioned ready-to-use dispersions at a central location, and then transport them to the individual manufacturers of composite wood panels. Increasing dispersion stability would allow these manufacturers to maintain a temporary stock of the dispersion, allowing for a more streamlined production process that is less susceptible to external factors. Ideally, a process would be engineered that allows the production of such stable dispersions that have a stability of at least two days or longer.
    In addition, European Patent EP 2 585 849 A2 states that the inclusion of a flame retardant tends to decrease certain mechanical properties of wood composite panels. European patent EP 2 585 849 A2 therefore describes the need in the prior art for a form of dispersion that reduces this tendency. A rather simple solution, which has been proposed by European patent EP 2 585 849 A2, is to reduce the content of flame retardants in the panels, which leads to an interaction, resulting in improved fire retardant properties, with only moderate deterioration of the mechanical characteristics.
    The present invention relates to aqueous dispersions suitable for use as fire retardant additives for wood composite panels. There is a need in the art for a method of producing such dispersions wherein the stability of said dispersions is at least two days. Furthermore, there is a need in the art for a method of producing such dispersions, the composition of which is such that the fire retardant, when incorporated into composite wood panels, has a lesser or even no influence on the mechanical properties of the wooden panels. The present invention aims to provide a method of producing such dispersions. On this
    BE2017 / 5167 way, the present invention solves at least some of the above
    Problems on.
    SUMMARY OF THE INVENTION
    The present invention provides a method of producing an aqueous dispersion suitable for use as a fire retardant additive for wood composite panels according to claim 1. Dispersions of fire retardant compositions usually have the drawback of not remaining stable for a very long time . Consequently, when dispersions are desired during the manufacturing process of wood composite panels, they are often produced on site at the sheet metal fabrication facility. This is a drawback for many manufacturers. By providing a system in which a premix is first produced, after which the premix is further treated by an inline rotor stator mixer, a very fine dispersion is obtained, which is stable for at least two days, or longer. Consequently, the dispersion can be offered ready to use to customers who can immediately apply it in their panel production process. This is a great advantage and cost effective.
    In a second aspect, the present invention is also directed to a stable dispersion according to claim 11.
    DESCRIPTION OF THE FIGURES
    Figure 1 shows a production plant scheme describing an embodiment of the production plant used in producing the aqueous dispersion according to an embodiment of the method.
    BE2017 / 5167
    DETAILED DESCRIPTION OF THE INVENTION
    The invention relates to a method of producing aqueous dispersions for use as a fire retardant additive for wood composite panels. The present invention also relates to an aqueous dispersion of this kind produced, for example, by the said method.
    Unless otherwise defined, all terms used in the description of the invention, including technical and scientific terms, have the meaning generally understood by one skilled in the art to which this invention pertains. Furthermore, the definitions of the terms are included to better understand the description of the present invention. As used here, the following terms have the following meanings:
    One, the and the as used here refer to both the singular and the plural unless the context indicates otherwise. A compartment refers, for example, to one or more than one compartment.
    Approximately as used herein, which refers to a measurable value such as a parameter, an amount, a time period and the like, is intended to include variations of +/- 20% or less, preferably +/- 10% or less, more at preferably +/- 5% or less, even more preferably +/- 1% or less, and even more preferably +/- 0.1% or less of the specified value, to the extent that such variations are suitable to perform in the described invention. It will be understood, however, that the value to which the modifier relates approximately is itself also specifically described.
    Include, comprising and includes and consisting of as used herein, are synonymous with contain, contain or contain and are inclusive or open terms that specify the presence of what includes e.g. a component and exclude the presence of additional, unlisted components, features do not eliminate elements, parts, steps which are well known in the art or described therein.
    Claiming numerical ranges by endpoints includes all cases and fractions included within that range, as well as said endpoints.
    BE2017 / 5167
    The term weight percent, throughout and throughout the description unless otherwise indicated, refers to the relative weight of the respective component based on the total weight of the formula.
    The term wood composite panels refers to a range of derived wood products produced by bonding or fastening the strands, particles, fibers or veneers or wood boards, together with adhesives or resins, to form composite materials. Engineered wood products are usually made from the same types of heartwood and softwood that are used to produce lumber. Wood saw waste and other wood waste can be used for engineered wood consisting of wood particles or fibers, but whole blocks are usually used for veneer wood, such as laminated wood, MDF or chipboard. Some engineered wood products, such as oriented strand board (OSB), can use trees of the poplar family, a common but non-structural species.
    Alternatively, it is also possible to produce similarly engineered bamboo from bamboo; and similarly engineered cellulose products from other lignin-containing materials such as rye straw, wheat straw, rice straw, hemp straws, kenafs or sugarcane residue, in which case they do not contain real wood, but rather vegetable fibers.
    Wood composite panels can therefore include, but are not limited to, the following: laminated wood, fiberboard, oriented strand board (OSB) laminated wood or veneer, chipboard, sheet material, or medium density fiberboard.
    The term aqueous as used herein in connection with a composition of the invention means that the composition is at least partially dissolved in a solvent such as water, or that a dispersion has been produced.
    The term dispersion as used herein refers to an aqueous system in which particles are dispersed in a continuous phase of a different composition (or status), in the present case, solid particles in a liquid.
    The term fire retardant as used herein is to be understood as a means that when added to the wood composite
    BE2017 / 5167 material, can provide fire retardant properties to said material. Fire retardancy is defined as the reduction of energy release, flame propagation and rate of flame propagation during a fire.
    The term smoke suppressant is to be understood as an agent which, when added to a wood composite material, may reduce the smoke production or density of the material when heated or burned.
    In a first aspect, the present invention describes a method of producing an aqueous dispersion suitable for use as a fire retardant additive for wood composite panels, said method comprising the following steps of providing a distribution tank with a first, internal wet milling system and externally connected, via an outlet valve, to a second inline wet milling system, when said outlet valve is closed, where water and at least one flame retardant are in the form of granules and / or particles, and internal wet grinding system is enabled, giving a premix,
    - then opening the outlet valve and turning on the inline wet milling system, and adding to said premix at least one pH adjuster, at least one inorganic thickener, and optionally at least one smoke suppressant, while turning on both Wet milling systems are maintained until a dispersion is obtained.
    Wet grinding systems generally include a broad class of Systems that can reduce particle sizes (and size distributions) of particles and granules suspended in liquid. More specifically, said liquid is aqueous in nature for the present invention. The mechanism of action of such Systems is based on physically breaking down larger particles into smaller ones. In particular, some wet grinding systems allow particle sizes to be reduced to the micron or even submicron range. Different types of Wet Milling Systems exist, including, but not limited to: rotary wet milling systems,
    BE2017 / 5167 Vibrating Wet Milling Systems, Stirred Wet Milling Systems, and any combination thereof.
    Rotating Wet Turning Systems are a first type of wet milling systems. Such Systems include a vessel that can be set to rotate in its entirety about its axis. In the case of the aforementioned internal wet milling system, said vessel could be the distribution tank itself. In case of the aforementioned inline wet milling system, said vessel could be externally connected to said dispensing tank, via the outlet valve. The said axis of the vessel (also the axis of rotation) is hereby oriented essentially horizontally. When switched on, the rotational speed of the barrel is chosen so that the contents of the barrel rotate continuously, due to gravity. On the one hand, said content comprises an aqueous suspension comprising water and the particles / granules. On the other hand, this content is indicated with the so-called grinding medium. Their respective volume ratios are about 25% and 50% of the total internal volume of the vessel. Examples of grinding media are balls or rods; they are made from materials such as, but not limited to, silicon nitride and chrome steel. During its revolving movement, said grinding medium crushes the particles both between them and against the wall of the vessel. The particles are hereby subjected to normal forces, oblique forces and / or shearing forces, as a result of which they break. Alternatively, the larger grains even serve as a grinding medium, and there is no need for additional balls or rods. The vessel wall is usually reinforced. The vessel wall is optionally internally equipped with so-called linings, for example, but not limited to: smooth coatings, Osborn coatings, El Oro coatings and / or Forbes coatings. Rotational speeds of the drum for rotating wet milling systems are somewhere between 5 rpm and 200 rpm. It is easier to define such rotational speeds relative to the so-called critical speed. The said critical speed is the rotational speed at which the grinding medium no longer rotates in the rotating vessel: the centrifugal force acting on it begins to exceed gravity. Typical rotational speeds are between 50% and 85% of the said critical speed.
    Vibrating Wet Turning Systems are a second type of wet milling systems. These Systems include a similar vessel, which is set to vibrate rather than rotate. Grinding media such as bullets and rods crush again
    BE2017 / 5167 the grains and particles that are brought to the said vessel, causing them to break.
    Stirred Wet Turning Systems are a third type of wet milling systems. The system now again comprises a vessel into which an aqueous suspension is introduced or prepared. The said vessel is not necessarily rotated or vibrated, but it is internally provided with one or more stirrers. For example, the vessel is internally provided with at least one rotary axis on which one or more pins, discs and / or a rotatable agitator head are mounted. The said axis of rotation can be oriented horizontally, vertically or in any other direction. Such wet grinding systems can be used with or without grinding media.
    On the one hand, if no grinding media are used, the particle size reduction is mainly due to the grinding action of the agitator itself. The axis of rotation drives, for example, one or more rotors, blades with saw teeth and / or rotor / stator working heads. Alternatively, in the case of an inline stirred wet milling system, such rotors, sawtooth blades and / or rotor / stator working heads may be provided in an outlet of the distribution tank.
    On the other hand, in agitated ball systems for wet grinding, the agitator starts the movement of the contents of the vessel, said contents including grinding media of the ball type. Particle size reduction is then mainly due to the crushing of the particles, between balls and / or between balls and the vessel wall. The grinding media (balls) can be rather small, up to tenths of a micron. On the other hand, rotational speeds can be quite high, up to 20000 rpm or higher. The agitator itself may also have a particle size reducing effect.
    An advantage of wet grinding, as opposed to dry grinding, is that it is possible to obtain a particle size distribution with a significant proportion of particles the size of a submicron. A reduced overall particle size results in an increased dispersion stability.
    Another advantage of wet grinding, in contrast to dry grinding, is that the fine particles are directly incorporated in an (aqueous) dispersion, so that no dust is formed. The technique can therefore be much safer because some
    BE2017 / 5167 types of dust give rise to health risks. In addition, when mixed with ambient air or oxygen, some types of dust have explosive behavior. Another advantage is that material losses are significantly reduced because fine particles cannot escape in the form of dust. Dosing of wet substances is also easier and therefore more precise than dosing of dry substances, which is an additional advantage.
    Thus, the present process is a two-step process: in a first step, a uniform premix is prepared, the premix comprising water and at least one flame retardant, in the form of granules and / or particles. This premix is partially divided, but it still contains large particles and is not stable. However, the premix is sufficiently homogeneous to be received by the inline wet milling system during the second step of the process. The premix is further distributed. Also during this second step, other agents such as at least one pH adjuster, at least one inorganic thickener and optionally at least one smoke suppressant are added to the contents of the dispensing tank while maintaining the engagement of both distributors.
    An advantage of using the two-step process is that the fire retardant can be added in any form. For example, the fire retardant is added in the form of prills in the order of millimeters. In the first step, the contents of the distribution tank are transformed into a homogeneous premix, using the internal distributor. The particles and / or granules of the fire retardant are thereby disintegrated into both optically detectable solid particles and non-optically detectable solid particles.
    Another advantage is that two different types of Wet Milling Systems can be synergistically combined. It is therefore possible to obtain a final particle size distribution that is smaller.
    The inline wet milling system is preferably used in a loop configuration, with its outlet connected to the distribution tank.
    According to a further preferred embodiment of the method, said internal wet milling system is rotary and / or stirred
    BE2017 / 5167 lies system for wet grinding; the associated rotational speed when engaged between 5 rpm and 20000 rpm.
    According to a further preferred embodiment of the method, said internal wet milling system is an internal stirred wet milling system, such as an internal blade or rotor / stator type distributor; the associated rotation speed at start-up is between 500 rpm and 3600 rpm.
    In a non-limiting, alternative embodiment, the internal wet milling system comprises at least one low speed scraper and / or one stirrer, operating at a rotation speed between 50 and 6000 rpm. Said system advantageously increases the homogeneity of the premix, thereby avoiding phase separation. Even if it causes only a limited or insignificant drop in particle size, such a scraper / stirrer (or scraper / stirrer assembly) is still designed as a possible embodiment of the internal wet milling system. According to a non-limiting further embodiment, the fire retardant is micronized to form a powder before being placed in the dispensing tank. Such a previous micronization process includes, but is not limited to, dry milling of the grains and / or particles. The internal wet milling system then has no significant influence on the particle size distribution. The inline wet milling system, on the other hand, further reduces said particle size distribution.
    According to a further preferred embodiment of the method, said inline wet milling system is a rotary wet milling system and / or a stirred wet milling system; the associated rotation speed at start-up is between 5 rpm and 20000 rpm.
    According to a further preferred embodiment of the method, said inline stirred wet milling system is an inline stirred wet milling system such as an inline rotor / stator type distributor; the associated rotation speed at start-up is between 500 rpm and 3600 rpm.
    According to a further preferred embodiment of the method, said method comprises the following steps:
    providing a distribution tank with a divider of the internal blade type and / or of the rotor / stator type and connected externally, via a
    BE2017 / 5167 outlet valve, with an inline rotor / stator type distributor, when said outlet valve is closed, with water and at least one flame retardant in the form of granules and / or particles, and engaging the internal distributor with a rotational speed between
    500 rpm and 3500 rpm, giving a premix,
    - then opening the outlet valve and switching on the inline distributor, at a rotation speed between 500 rpm and 3500 rpm, and adding to said premix at least one pH adjuster, at least one inorganic thickener, and optionally at least one smoke suppressant while the switch-on of both distributors is maintained until a dispersion is obtained.
    In a preferred embodiment of the method, the internal distributor is a tank-mounted, blade-type distributor, comprising one or more blades on a blade shaft. These blades preferably have a sawtooth design. Even more preferably, the internal distributor includes a vertical, tank-mounted blade shaft with a single, horizontally running, sawtooth blade. The blade shaft is turned on at a rotational speed between 500 rpm and 3500 rpm, more preferably at a rotational speed between 1000 rpm and 2500 rpm, and even more preferably at a rotational speed of about 1500 rpm. The internal divider here induces moderate hydraulic shear, which means that it induces moderate velocity gradients in the fluid, thereby moderately distributing the contents of the distribution tank. "Moderate" is to be defined herein with respect to particle distribution, as stated below. In an alternative embodiment of the method, the internal distributor is a rotor / stator type tank mounted distributor, with a rotor / stator type working head as described below.
    In a further preferred embodiment of the method, the inline distributor is a rotor / stator-type distributor comprising a rotor / stator-type working head. The said working head comprises a rotor with rotor blades and a perforated stator. The rotor can be set to rotate in a stator container and / or along a stator plate, the stator being provided with perforations. The stator is stationary, while the rotor is driven at a rotation speed between 500 rpm and 3500 rpm, more preferably at a rotation speed between 2000 rpm and 3500 rpm, and even more preferably at a rotation speed of about 3000 rpm. A precise opening is provided
    BE2017 / 5167 between at least one component of the rotor and one component of the perforated stator, so that a relative rotation of both components, in close proximity to each other, is allowed. When the rotor / stator inline distributor is turned on, the rotor blades push the fluid through the perforations in the stator, resulting in a grinding action with high velocity gradients. The inline distributor thus induces a high hydraulic shear, whereby the content of the distribution tank is further distributed. The inline manifold is usually used in a loop configuration, with its outlet connected to the manifold.
    Thus, the present process is a two-step process: in a first step, a uniform premix is prepared, the premix comprising water and at least one flame retardant, in the form of granules and / or particles. This premix is partially divided, but it still contains large particles and is not stable. However, the premix is sufficiently homogeneous to be received by the inline distributor during the second step of the process. The premix is further distributed. Also during this second step, other agents such as at least one pH adjuster, at least one inorganic thickener and optionally at least one smoke suppressant are added to the contents of the dispensing tank while maintaining the engagement of both distributors.
    An advantage of using the two-step process is that the fire retardant can be added in any form. For example, the fire retardant is added in the form of prills in the order of millimeters. In the first step, the contents of the distribution tank are transformed into a homogeneous premix, using the internal distributor. The particles and / or granules of the fire retardant are thereby disintegrated into both optically detectable solid particles and non-optically detectable solid particles. As a result of the moderate hydraulic shear, the optically detectable particles hereby become sufficiently small that the said premix could be brought to the inline rotor / stator distributor.
    In this regard, a distinction must be made between a moderate hydraulic shear, which results in a moderate degree of dispersion, and a high hydraulic shear, which results in a high degree of dispersion.
    BE2017 / 5167
    In a non-limiting embodiment, adjuvants are added to provide improved stabilization of the resulting dispersion. The said adjuvants counteract agglomeration of particles by steric stabilization and / or electrostatic stabilization.
    The fire retardant used in the context of the present invention is preferably selected from the general group of phosphorus and phosphate based fire retardants, inorganic fire retardants and / or nitrogen based fire retardants.
    The said phosphorus and phosphate based flame retardants cover a wide range of inorganic and organic compounds and include both reactive products chemically bonded to the polymer material and additive products integrated into the material by physical mixing only. An example of such a flame retardant is ammonium dihydrogen phosphate or ammonium polyphosphate.
    The most commonly used inorganic flame retardants mentioned are hydroxides or aluminum and magnesium and zinc compounds.
    Nitrogen-based flame retardants are believed to act through various mechanisms (i.e., salts with organic or inorganic acids or boric acid or cyanuric acid). Three chemical groups can be distinguished: pure melamine, derivatives of melamine, ie salts with organic or inorganic acids such as boric acid, cyanuric acid, phosphoric or pyro / polyphosphoric acid, and homologues of melamine, such as melam, melem and melon, the latter only for experimental use at this stage.
    The amount of the flame retardant in the dispersion is preferably between 25% and 70% by weight, more preferably between 25% and 48% by weight.
    The pH of the final dispersion will be adjusted for use in wood composite panels. It has been found that by controlling the pH of the composition to a narrow and predefined range using pH control compounds, optimum compatibility is obtained with the resins used during the production of the wood composite
    BE2017 / 5167 panels. The pH of a 10% aqueous dilution of said dispersion is usually between 5 and 7.
    For this purpose, one or more pH controllers will be added during the preparation of the dispersion. These controllers are well known in the art.
    In addition to a fire retardant compound, the dispersion may also contain a smoke suppressant. These agents will have an impact on smoke development and its density in the event of a fire. Various smoke suppressants are well known in the art such as, for example, boric acid or disodium octroborate (DOT).
    The smoke suppressant is preferably present in a concentration between 0.2% and 10% by weight, more preferably in a concentration between 0.5% and 7.5% by weight, more preferably in a concentration between 0.5 % and 7.0% by weight.
    A thickener or viscosity controller is added to adjust the viscosity of the dispersion to a predefined viscosity target. While most prior art dispersions use the stronger organic thickeners because the particle size of the dispersions is too large, the very fine particle size of the dispersion of the present invention allows the use of inorganic thickeners such as, but not limited to, clay thickeners such as bentonite or sepiolite thickeners.
    The addition of these compounds prevents the precipitation of particles in dispersions of the present invention, thereby extending the shelf life of the compositions.
    Said inorganic thickener is preferably added in such proportions to adjust the viscosity of the dispersion between 50 cP and 500 cP, more preferably between 50 and 200 cP. The thickening agent may preferably be added in a concentration between 0.01% and 10% by weight of the dispersion, more preferably between 0.01% and 5% by weight, more preferably between 1% and 5% by weight.
    BE2017 / 5167
    An advantage of the dispersion with a relatively low viscosity value, ranging from 50 cps to 200 cps, is that dosing can be carried out much more precisely. A decrease in the viscosity value of the dispersion, while at the same time maintaining or even improving the stability of the dispersion, is possible because of the very fine particle size distribution. The dispersion obtained is preferably stable for at least two days, more particularly at least three days, even more preferably at least 4, 5 or 6 days.
    The total water content of the dispersion is preferably between 30% and 60% by weight, more preferably between 30% and 55% by weight, more preferably between 30% and 55% by weight, and more preferably between 40% and 55% by weight. The water is added during the premix formation, and the temperature is at most preferably 35 ° C, more preferably between 15 and 35 ° C. In practice, the method of producing the second aspect of the present invention is preferably conducted at room temperature. Such moderate temperatures allow production without the need for a heating or cooling step.
    In a non-limiting embodiment of the invention, a defoamer may be included in the premix or added to the premix. This is preferably a non-silicone based defoamer suitable for defoaming aqueous Systems.
    In a final step of the methodology of the present invention, the dispersion will be screened, preferably using a 400 µm screen, eliminating residual large compounds that may still be present in the dispersion. This again provides the fine particle size of the present dispersion and a very homogeneous dispersion.
    In a second aspect, the present invention also relates to an aqueous dispersion suitable for use as a fire retardant additive for wood composite panels, which is stable for at least two days, more preferably at least three days, even more at preferably at least 4, 5 or 6 days. This ensures that the dispersion can be supplied ready for use at production sites for wooden composite panels.
    BE2017 / 5167
    Preferably, the dispersion is a 50% dispersion, which means that 50% of the dispersion will be solids in an aqueous system. Due to the formation of a premix and subsequently in-line mixing with a rotor stator, a very fine dispersion is obtained.
    The viscosity of the dispersion is preferably between 50 and 500 cP, more preferably between 50 and 200 cP. The pH of the dispersion is preferably between 3.5 and 7.5. In another embodiment, said pH of the dispersion is adjusted between 5.9 and 5.1. In another embodiment, said pH is adjusted between 5.9 and 7.1.
    Preferably said water content is between 30% and 50% by weight, the pH controller is present between 2% and 25% by weight, said flame retardant is between 25% and 48% by weight, and the smoke suppressant is between 0 , 2% and 10% by weight, more preferably between 0.5 and 7.5%.
    The dispersion is particularly useful to produce wood composite panels with fire retardant and / or smoke suppression activity, especially for use in medium density fiberboard (MDF), oriented strandboard (OSB), board material or fiberboard.
    These aspects of the present invention will be further explained by way of examples and figures, without being limited to these examples or figures.
    Figure 1 shows a production plant 1 scheme describing an embodiment of the production plant 1 used in producing the aqueous dispersion according to an embodiment of the method.
    The production installation 1 comprises a distribution tank 2 with an internal volume of approximately 20 m 3 . The distribution tank 2 is internally provided with an internal distributor 3. The said internal distributor 3 comprises a vertical, tank-mounted blade shaft 4 which is connected to an internal distribution motor 5 and which is provided with a single horizontal running sawtooth blade 6. The distribution tank 2 is externally connected to an inline distributor 7, via an outlet valve 8. This inline distributor 7 is used in a loop configuration, with its outlet reconnected to the distribution tank
    2. The inline distributor 7 comprises a rotor / stator working head 9.
    BE2017 / 5167
    About 2200 kg of water 10 at ambient temperature, preferably at a temperature of about 20 ° C, is introduced into the distribution tank 2 via the water supply 11. At this stage, the outlet valve 8 of the distribution tank 2 is closed, and none of the distributors are turned on . The said water supply 11 is controlled, for example, by means of the water supply control 12 which is at least in communication with two level sensors 13. The internal distribution motor 5 is switched on such that the blade shaft 4 is set to rotate at a rotation speed of about 1500 rpm. Thereafter, about 1700 kg of a flame retardant 14, in the form of millimeter prills, is introduced into the distribution tank 2 via the loss in weight supply 15, which is switched on by the loss in weight supply motor 16. With using the internal divider 2, the heterogeneous mixture of water and flame retardant is converted into a more uniform premix. The preparation of said premix, starting from the heterogeneous mixture of water and the fire retardant, takes about 15 minutes, regardless of the type of fire retardant 14 used.
    In a second step, the outlet valve 7 is opened and the inline distributor 9 is turned on, at a rotation speed of about 3000 rpm. In this way, the particles of the fire retardant agent 14 are further distributed using both the internal distributor 3 and the inline distributor 7. Meanwhile, other agents are added successively to the contents of the distribution tank 2. These other agents include at least one pH controller, at least one inorganic thickener, and optionally at least one smoke suppressant. A stable, aqueous dispersion 17 is thus obtained, which is suitable for use as a fire retardant additive for wood composite panels. According to the present embodiment, this stable dispersion 17 is extracted directly from the distribution tank 2 via the outlet valve 8, the outlet valve 8 being a three-way valve. In an alternative embodiment, such a three-way valve can be provided along the return line of the inline distributor 7. Finally, the stable dispersion 17 is screened using a 400 µm control screen.
    Characteristics related to the figures:
    1. production plant
    2. distribution tank
    BE2017 / 5167
    3. internal distributor
    4. blade shaft
    5. internal distribution motor
    6. sawtooth blade
    7. inline distributor
    8. outlet valve
    9. rotor / stator work head
    10. water
    11. water supply
    12. water supply control
    13. level sensor
    14. Fire retardant
    15. loss in weight supply
    16.loss in weight feed motor
    17. stable dispersion
    BE2017 / 5167
    权利要求:
    Claims (15)
    [1]
    CONCLUSIONS
    A method of producing an aqueous dispersion suitable for use as a fire retardant additive for wood composite panels, said method comprising the following steps:
    providing a distribution tank with a first internal wet milling system and externally connected, via an outlet valve, to a second inline wet milling system, when said outlet valve is closed, with water and at least one flame retardant in the form grains and / or particles, and the internal wet milling system is turned on, giving a premix,
    - then opening the outlet valve and turning on the inline wet milling system, and adding to said premix at least one pH adjuster, at least one inorganic thickener, and optionally at least one smoke suppressant, while turning on both Wet milling systems are maintained until a dispersion is obtained.
    [2]
    A method according to claim 1, characterized in that said internal wet milling system is a rotary and / or stirred wet milling system; the associated rotational speed at power-up is between 5 rpm and 20000 rpm.
    [3]
    Method according to the preceding claim 2, characterized in that said internal wet milling system is an internal distributor of the blade type and / or the rotor / stator type; wherein the associated rotational speed at start-up is between 500 rpm and 3600 rpm.
    [4]
    A method according to any one of claims 1 to 3, characterized in that said inline wet milling system is a rotary wet milling system or a stirred wet milling system; the associated rotational speed at power-up is between 5 rpm and 20000 rpm.
    [5]
    Method according to the preceding claim 4, characterized in that said inline wet milling system is an inline distributor of the rotor / stator type; wherein the associated rotational speed at start-up is between 500 rpm and 3600 rpm.
    BE2017 / 5167
    [6]
    Process according to any one of claims 1 to 5, characterized in that the pH of said dispersion obtained, in a 10% water dilution, is between 5 and 7.
    [7]
    A method according to any one of claims 1 to 6, characterized in that the fire-retardant concentration in the dispersion is between 25% and 48% by weight.
    [8]
    Method according to any one of claims 1 to 7, characterized in that the temperature of said water for said premix is a maximum of 35 ° C.
    [9]
    Process according to any one of claims 1 to 8, characterized in that said fire retardant is ammonium phosphate or ammonium dihydrogen phosphate.
    [10]
    A method according to any one of the preceding claims, characterized in that the dispersion comprises a smoke suppressant in a concentration between 0.5% and 7.5% by weight.
    [11]
    A method according to any one of the preceding claims, characterized in that the total water content in the dispersion is between 30% and 55% by weight.
    [12]
    A method according to any one of the preceding claims, characterized in that said inorganic thickener is added in proportions such that the viscosity of the dispersion is between 50 cP and 200 cP.
    [13]
    Method according to any one of the preceding claims, characterized in that the dispersion is screened.
    [14]
    An aqueous dispersion suitable for use as a fire retardant additive for wood composite panels, the dispersion comprising water, a fire retardant, a pH adjuster and optionally a smoke suppressant characterized in that said dispersion is stable for at least at least two days.
    [15]
    An aqueous dispersion according to claim 14, characterized in that the viscosity of said dispersion is between 50 cps and 200 cP.
    BE2017 / 5167
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    同族专利:
    公开号 | 公开日
    EP3562910A1|2019-11-06|
    CA3046380A1|2018-07-05|
    US20200122154A1|2020-04-23|
    BE1024872A1|2018-07-26|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    US5948323A|1995-06-07|1999-09-07|Glcc Technologies, Inc.|Colloidal particles of solid flame retardant and smoke suppressant compounds and methods for making them|
    WO2007096883A2|2006-02-23|2007-08-30|Bromine Compounds Ltd.|Washing-fast smoldering-suppressing compositions|
    法律状态:
    2018-10-03| FG| Patent granted|Effective date: 20180731 |
    优先权:
    申请号 | 申请日 | 专利标题
    BEBE2016/5997|2016-12-30|
    BE201605997|2016-12-30|EP17826246.5A| EP3562910A1|2016-12-30|2017-12-26|Method for producing aqueous dispersions for use as a flame retardant additive to wood composite panels|
    US16/473,704| US20200122154A1|2016-12-30|2017-12-26|Method for producing aqueous dispersions for use as a flame retardant additive to wood composite panels|
    PCT/EP2017/084590| WO2018122222A1|2016-12-30|2017-12-26|Method for producing aqueous dispersions for use as a flame retardant additive to wood composite panels|
    CA3046380A| CA3046380A1|2016-12-30|2017-12-26|Method for producing aqueous dispersions for use as a flame retardant additive to wood composite panels|
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