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    • 专利摘要:
    The present invention relates to a process for the preparation of calcium monohydrogenphosphate comprising an attack in an aqueous medium, for a predetermined period of time, of a phosphate source by an acid with formation of a pulp comprising an aqueous phase containing phosphate of calcium in solution and a solid phase containing impurities, a first separation between said aqueous phase and said solid phase, during a predetermined period of time, a neutralization of said aqueous phase at a pH sufficient to obtain a precipitation of said calcium monohydrogenphosphate, a second separation between said aqueous medium and said calcium monohydrogenphosphate, characterized in that said predetermined period of time of said digestion step a) is greater than that of said step b).
    公开号:BE1024582B1
    申请号:E2017/5458
    申请日:2017-06-27
    公开日:2018-04-17
    发明作者:Tibaut THEYS；Thomas Henry
    申请人:Prayon Technologies；
    IPC主号:
    专利说明:


    1024582 Bl economy
    FPS Economy, SMEs, Middle Classes & Energy Intellectual Property Office
    Date of issue: 17/04/2018
    PATENT
    Priority date: 06/28/2016
    International classification: C01B 25/22, C01B 25/32, C05B 7/00, C05B 11/12, A23L 33/16 Filing number: BE2017 / 5458 Filing date: 06/27/2017
    Holder:
    PRAYON TECHNOLOGIES
    4480, ENGIS
    Belgium
    Inventor:
    THEYS Tibaut
    5340 FAULX-LES-TOMBES Belgium
    HENRY Thomas 3870 HEERS Belgium
    PROCESS FOR THE PREPARATION OF CALCIUM MONOHYDROGENOPHOSPHATE
    The present invention relates to a process for the preparation of calcium monohydrogen phosphate comprising an attack in an aqueous medium, for a predetermined period of time, of a source of phosphate by an acid with formation of a pulp comprising an aqueous phase containing phosphate calcium in solution and a solid phase containing impurities, a first separation between said aqueous phase and said solid phase, for a predetermined period of time, neutralization of said aqueous phase at a pH sufficient to obtain precipitation of said calcium monohydrogen phosphate, a second separation between said aqueous medium and said calcium monohydrogenphosphate, characterized in that said predetermined period of time of said step a) of digestion is greater than that of step b) above.
    BELGIAN INVENTION PATENT
    FPS Economy, SMEs, Middle Classes & Energy
    Publication number: 1024582 Deposit number: BE2017 / 5458
    Intellectual Property Office International Classification: C01B 25/22 C01B 25/32 C05B 7/00 C05B 11/12 A23L 33/16 Date of issue: 04/17/2018
    The Minister of the Economy,
    Having regard to the Paris Convention of March 20, 1883 for the Protection of Industrial Property;
    Considering the law of March 28, 1984 on patents for invention, article 22, for patent applications introduced before September 22, 2014;
    Given Title 1 “Patents for invention” of Book XI of the Code of Economic Law, article XI.24, for patent applications introduced from September 22, 2014;
    Having regard to the Royal Decree of 2 December 1986 relating to the request, the issue and the maintenance in force of invention patents, article 28;
    Given the patent application received by the Intellectual Property Office on 27/06/2017.
    Whereas for patent applications falling within the scope of Title 1, Book XI of the Code of Economic Law (hereinafter CDE), in accordance with article XI. 19, §4, paragraph 2, of the CDE, if the patent application has been the subject of a search report mentioning a lack of unity of invention within the meaning of the §ler of article XI.19 cited above and in the event that the applicant does not limit or file a divisional application in accordance with the results of the search report, the granted patent will be limited to the claims for which the search report has been drawn up.
    Stopped :
    First article. - It is issued to
    PRAYON TECHNOLOGIES, Rue Joseph Wauters 144, 4480 ENGIS Belgium;
    represented by
    GEVERS PATENTS, Holidaystraat 5, 1831, DIEGEM;
    a Belgian invention patent with a duration of 20 years, subject to payment of the annual fees referred to in article XI.48, §1 of the Code of Economic Law, for: PROCESS OF PREPARATION OF
    CALCIUM MONOHYDROGENOPHOSPHATE.
    INVENTOR (S):
    THEYS Tibaut, Route de Jausse 25, 5340, FAULX-LES-TOMBES;
    HENRY Thomas, Nieuwe Steenweg 83/001, 3870, HEERS;
    PRIORITY (S):
    06/28/2016 BE 2016/5482;
    DIVISION:
    divided from the basic application: filing date of the basic application:
    Article 2. - This patent is granted without prior examination of the patentability of the invention, without guarantee of the merit of the invention or of the accuracy of the description thereof and at the risk and peril of the applicant (s) ( s).
    Brussels, 04/17/2018, By special delegation:
    B E2017 / 5458
    The present invention relates to a process for the preparation of calcium monohydrogen phosphate or dicalcium phosphate
    Including your steps of:
    a) digestion in an aqueous medium, for a first period of time, of a phosphate source with an acid with the formation of a pulp comprising an aqueous phase containing calcium phosphate in solution and a solid phase containing impurities,
    b) a first separation between said aqueous phase containing calcium phosphate in solution and said solid phase containing impurities, during a second period of time,
    c) neutralization of said aqueous phase containing calcium phosphate in solution at a sufficient pH to obtain precipitation in an aqueous medium of insoluble calcium phosphate as the above-mentioned calcium monohydrogen phosphate, and
    d) a second separation between said aqueous medium and said calcium monohydrogenphosphate,
    2Q The attack on a source of phosphate, such as phosphate ore, by an acid has been known for many years, for example from patents US 3304157 and GB 105 15 21.
    The document WO 2004002388 discloses a process for the manufacture of calcium monohydrogen phosphate (DGF) and also a process for the production of phosphoric acid from the DCP obtained according to the process described in this patent document,
    This document provides for an attack on a phosphate ore in a digestion tank with a hydrochloric acid solution, having a concentration of the order of 5% by weight, to form a pulp comprising an aqueous phase containing calcium phosphate.
    B E2017 / 5458 and chloride sounds in solution and a solid phase containing impurities.
    Passing the above-mentioned pulp through a filter press makes it possible to separate the aqueous phase containing calcium phosphate and chloride ions in solution from the solid phase containing impurities.
    Neutralization of the separated aqueous phase containing calcium phosphate and chloride ions is carried out by means of the addition of a calcium compound to precipitate the DCP insoluble in the aqueous phase, following a rise in pH.
    An additional separation is carried out to recover a wet cake of DCP at the end of the process.
    Concerning the production of a phosphoric acid using the DCP thus obtained, this is carried out by a liquid-liquid extraction and requires several stages of implementation.
    It is, in fact, necessary to carry out a step of dissolving the wet DCP cake, obtained according to the method described above, by a new attack with more concentrated hydrochloric acid which can range up to 20% by weight. This solubilization allows the formation of an aqueous solution containing phosphate ions, calcium ions and chloride ions, to be extracted with an organic extracting agent,
    More precisely, this extraction step is carried out in an extraction column using an organic solvent and makes it possible to produce an aqueous extraction phase containing chloride ions © calcium tones and an organic extraction phase containing phosphoric acid,
    The organic extraction phase containing phosphoric acid is re-extracted using an aqueous re-extraction agent so as to isolate an aqueous re-extraction phase containing phosphate ions.
    Finally, a concentration of the aqueous re-extraction phase allows the formation of an aqueous solution of phosphoric acid.
    B E2017 / 5458 <5
    This process for producing phosphoric acid is complex and requires several expensive steps to provide a phosphoric acid of sufficient quality for the intended applications.
    In addition, the use of organic extraction solvents makes such a process unattractive on an ecological impact farm.
    The document WO 2005 066 070 relates to a process for attacking phosphate ore with an aqueous hydrochloric acid solution having an HCl concentration of less than 16% by weight, with the formation of a pulp consisting of an aqueous phase containing calcium phosphate in solution and chloride ions and an insoluble solid phase containing impurities.
    The above-mentioned aqueous phase is neutralized at a first pH at which a significant proportion of calcium phosphate is maintained in the aqueous phase in order to precipitate impurities,
    Then, the aforementioned insoluble solid phase is separated from the aqueous phase while the precipitated impurities are isolated.
    An additional neutralization of the aqueous phase is carried out at a second higher pH at the above-mentioned first pH to precipitate
    DCP which is then separated from the aqueous medium.
    This process is limited by the fact that! Should use an aqueous solution of hydrochloric acid have a concentration less than 16% by weight.
    More recently, a process for attacking a phosphate source with an aqueous hydrochloric acid solution has been the subject of patent application WO 2015 082 468,
    According to this disclosure, digestion of the rock in the presence of the aqueous hydrochloric acid solution makes it possible to form a pulp consisting of an aqueous phase containing calcium phosphate and chterous ions in solution, and of an insoluble solid phase containing Impurities.
    B E2017 / 5458
    The aqueous phase is then separated from its solid phase by filtration so that the aqueous phase can be neutralized at a sufficient pH to form an aqueous medium comprising chloride ions and in order to precipitate the calcium phosphate in the form of said phosphate salt. Subsequent separation isolates the phosphate salt.
    According to this process, the etching and filtration steps are carried out at a temperature between 50 ° C and 70 ° C and the first aqueous hydrochloric acid solution has a lower or even HCl concentration of 15% by weight.
    Unfortunately, the known methods are impractical for industrialists since they do not have an extraction yield of P; € q which is sufficient compared to the amount of P 2 O 5 present in the starting phosphate source. and that the phosphate salt obtained is not sufficiently pure, which nevertheless determines its use potential in several fields of application, such as agriculture or food and technical applications with high added value. real need to provide a process for manufacturing calcium mcnohydrogenphosphate which ultimately solves this problem linked to the purity of calcium monohydrogenphosphate, while limiting the losses in ILCL in the waste generated by the process in order to improve their performance of the process.
    The object of the invention is to provide a process for the manufacture of calcium monohydrogenphosphate which can be simple to implement, reliable and rapid. The digestion and the filtration must allow a high extraction yield per PzOg, while taking due account of the compress between the desired degree of purity of the calcium monohydrogenphosphate obtained at the end of the process and the limitation of losses of P2O5 ·
    To solve this problem, there is provided according to the invention a method as indicated at the beginning, characterized in that said first
    B E2017 / 5458 time period of said step a) of digestion is greater than said second time period of step b) of the above-mentioned first separation.
    Surprisingly, it has been observed that when step a) of digestion has a longer period of time than the period of time linked to step b) of the above-mentioned first separation, the process has a yield of P ^ G S interesting, while guaranteeing the DCP an optimal degree of purity for the intended applications in the field of agriculture and food.
    More precisely, it appeared that said period dt said step e) of digestion which is greater than that of step b) of first separation makes it possible to considerably reduce the period of temple linked to the first separation. Ceia is particularly advantageous in that the first separation step is no longer restrictive for the user since it only involves reduced cleaning of the separation means, such as a filter, which can be used to carry out filtration, corresponding to said first separation. In this way, the first separation step is quick and efficient. Ceia has the consequence that the process according to the present invention is sufficiently profitable since it does not require repeated and consequent washing of the separation means.
    In practice, whether according to a continuous or discontinuous process, these advantages provided by the process clearly reduce the filtration area required. Thus, the first separation step is simpler and more efficient, which ultimately makes it possible to provide a more profitable method than the methods known from the prior art.
    It is also noted that the longer the digestion step is carried out over a long period of time, the more the first separation stage can take place during a short period of time.
    As explained, the calcium monohydrogen phosphate obtained according to the process of the present invention can be used in the field of agriculture, food or even in a composition
    B E2017 / 5458 intended for agriculture or food. The field of agriculture notably includes fertilizers, such as fertilizers. It can also be used for the production of phosphoric acid.
    Thus, it has been found that the method according to the invention allows
    S to obtain an extraction yield of P2O5 for the aforementioned steps a and b which can range up to 95% and makes it possible to provide a final product which has a degree of purity such that it is suitable for quality use in the field of rahmenfaire or of the agriculiure, like the fertilizers.
    Advantageously, the aforementioned steps a) and b) are carried out in a duration of less than 2 hours, preferably a duration of between 30 and 100 minutes, preferably between 30 and 70 minutes, more preferably around 40 and 55 minutes.
    The fact that the method according to the invention comprises a combination of parameters according to which steps a) and b) are carried out in a duration of less than 2 hours and the period of time linked to the above-mentioned step of digestion is greater than the time period linked to the abovementioned first separation step b) makes it possible to provide an even more profitable and more efficient process in terms of PiO 5 extraction run-off compared to the prior art.
    Even more advantageously, said predetermined time period of said step o) is between 75 and 100 minutes, preferably between 80 and 95 minutes, or between 20 and 45 minutes, in particular between 24 and 40 minutes, preferably between 30 and 35 minutes.
    According to an advantageous exemplary embodiment, said first separation of said step b) is carried out at a nitration rate of at least 0.1 tonnes of PsO ^ VAP.W / day, preferably between 0.1 and 5 tonnes of PzOi / lAP / stay, more preferably between 0.15 and 3 tonnes of PO ^ 'fAP'mVjour, more preferably still between 0.3 and 0.9, in particular between 0.4 and 0.7 , ton of PsQsNâP / nrrt / day, said filtration speed being calculated according to the following equation:
    B E2017 / 5458
    VS
    Filtration speed ~ : -
    2SP Ω T f where,
    Qp2O5 corresponds to the quantity of PgOg collected in the filtrate and is expressed in tonnes, £} is the area of the filter expressed in m 2 ,
    ΔΡ is the difference between the outlet pressure of the filtrate and the pressure applied to the pulp at the time of said first separation and is expressed in bar, and
    Tf is the period of time of said first separation and is expressed in days.
    The filtration speed indicated above is calculated, in a manner known to those skilled in the art, as described in particular in Albert Rushton, Anthony S. Ward and Richard G. Holdich, Solid-Liquid Filtration and Separation Technology, p. 35-93, ed. John Wiley & Sons, 2008.
    It has been found that the process following the invention also makes it possible to carry out said step b) of first separation at a filtration speed which is particularly advantageous in that it allows, at the same time, to reduce your filtration times, while by not increasing the filtra fault, which is required for industrial application.
    In addition, surprisingly, it appeared that it was possible to obtain in a simple manner a P 2 O 5 extraction yield for steps a and b greater than 90% by weight, preferably greater than 93% by weight, advantageously greater than 95%, by applying rapid and economical filtration rates on an industrial scale.
    According to a preferred embodiment, said source of phosphate and said acid are introduced into a first reactor comprising said aqueous medium simultaneously or successively, in order to carry out said step a) of digestion, and said pulp comprising said aqueous phase containing calcium phosphate in solution and said solid phase containing
    B E2017 / 5458 impurities is transferred from the first reactor to a separation means to implement said first separation taken up in step b) of the above-mentioned first separation.
    More preferably, said separation means is located between said first reactor and a second reactor.
    Even more preferably, said separation means is present in a second reactor into which is introduced said pulp comprising an aqueous phase containing calcium phosphate in solation and a solid phase containing impurities, to implement said first separation taken up in step b) above.
    In addition, said separation means can preferably be a filter chosen from the group consisting of a rotary filter, preferably with tilting cells, filter press, band filter and drum filter.
    According to a preferred embodiment, said acid is chosen from the group consisting of hydrochloric acid (HCl), nitric acid, sulfuric acid, phosphoric acid and their mixtures.
    Advantageously, said acid is an aqueous solution of acid, in particular hydrochloric acid, having a concentration of acid Less than or equal to 15% by weight.
    Even more preferably, steps a) and b) are carried out at a temperature between 50 ° C. and 70 s C., preferably equal to 50 ° C.
    Preferably, said phosphate source is chosen from the group consisting of a phosphate rock, a phosphate ore, secondary phosphate sources, such as ash (for example from sludge from a treatment plant or from 'bone or edge of pores) or their mixtures.
    Advantageously, the neutralization step is carried out using a neutralizing agent chosen from the group consisting of calcium-based compounds, such as calcium oxide, hydroxide and carbonate and calcium salts water soluble and hydroxide.
    B E2017 / 5458
    Other embodiments of the process according to the invention are indicated in the appended claims.
    The present invention also relates to a use of the calcium monohydrogenphosphate obtained according to the present invention for producing phosphoric acid.
    Such production of phosphoric acid can involve attack by calcium monohydrogen phosphate obtained with sulfuric acid.
    Preferably, the calcium monohydrogenphosphate 10 obtained according to the process according to the present invention is used in the food industry or in the agricultural or horticultural field.
    □ other embodiments of the use according to the invention are indicated in the appended claims, □ other characteristics, details and advantages of the process 15 and of the ut-lisaiion will emerge from the description given below, without limitation.
    □ years ie within the framework of the present invention, the expression “digestion is carried out during a first period of time” must be composed to mean that digestion ends at the moment when the first separation stage is initiated, which corresponds to when the pulp is introduced into a separation means, such as a filter.
    In the context of the present invention, the expression “first separation carried out during a second period of time” must be understood to mean that the duration linked to this first separation is determined from the moment when the pulp to be filtered is introduced into a separation means, such as a filter.
    According to a practical example, a phosphate ore and an aqueous hydrochloric acid solution are introduced simultaneously or successively into an aqueous medium contained in a first
    3Q reactor.
    B E2017 / 5458
    After digestion during a first period of time, a pulp is obtained in the first reactor and is introduced into a separation means with a view to carrying out step b) of first separation during a second period of time which is less than that corresponding to step a) of digestion.
    This separation means can be present in the first reactor or in a second reactor.
    When the separation means is present in the first reactor, the latter can be in fluid communication with this reactor.
    Thus, the predetermined duration of digestion ends from the moment when the puipe is introduced into the means of separation.
    The separation means can also be present in a second reactor, possibly in fluid communication with the first reactor.
    it is erroneously possible to use a first reactor, a second reactor and a separation means which can be arranged between said first and second reactors so as to be in fluid communication with the latter.
    In all of the aforementioned cases, said source of phosphate has a residence time, in said first reactor, greater than the residence time of said puipe in said separation means, pulp consisting of an aqueous phase comprising calcium phosphate and of an insoluble solid phase containing impurities.
    In the context of the present invention, the process can be carried out continuously or discontinuously.
    The step of neutralizing said aqueous phase comprising calcium phosphate and chloride ions in solution, when the attack is carried out with hydrochloric acid, is carried out at a pH sufficient to precipitate the calcium phosphate in the form of said monohydrogenphosphate from calcium.
    B Ε2017 / 5458
    A second separation is provided between said aqueous medium comprising the chloride chlorides and the calcium monohydra-phenophosphate so as to provide the calcium monohydrogenphosphate obtained by the process according to the present invention.
    The neutralization and second separation steps are known to those skilled in the art, in particular from document WO 2015 082 488, which is incorporated by reference in the present phosphate patent application presenting the
    We start from an ore of the following table 1 aracferistics:
    Amount of phosphate 1000.0 g Humidity 1.S3% 19.3 g CaQ 48.90% 489.0 g PA 31.00% 310.0 g
    An amount of 120.8 g of demineralized water is in a bein and then an amount of 75 g of phosphate from Table 1 is added to the demineralized water, with stirring, for mixing. The bedin is then covered with a glass of mixture is brought to a temperature of 80 ° C.
    120.8 g of demineralized water are mixed with an aqueous solution of hydrochloric acid, which has an HCI concentration of 37%, so as to obtain 357.7 g of an aqueous HCI solution at 12%. The latter is then added to a hot mixture of phosphate and demineralized water.
    The digestion time is measured from the moment when the aqueous dilute acid solution is added to the hot mixture containing phosphate and demineralized water.
    After a digestion time of 30 minutes, the solution thus obtained is filtered, at a filtration temperature of 80 * 0, by means of a
    B E2017 / 5458 polyester fiber filtra having a diameter of 90 mm and a thickness of 0.17 mm placed on equipment of the Buchner type previously evacuated,
    The filtration pressure used is 0.4 bar, which represents atmospheric 1 bar.
    The filtration time corresponds to the time necessary to obtain a wet cake from the pulp formed during the previous steps. After filtration, the cake is subjected to a drying step during which the ambient air is sucked through the cake. , the drying step for 5 minutes. According to this first example of embodiment, the filtration time is 5 minutes.
    The weight of the wet cake obtained is then measured as well as the weight of the filtrate. The filtrates and the cake are then subjected to analysis
    The wet cake 5 is then dried at a temperature of
    OCTC and its weight, after drying, is also measured,
    ÏÂÜ
    Example 1 Quantity of starting phosphate .................. ........................... ....... ....... 75 grams Amount of aqueous solution12% HCI 357.7 grams Digestion temperature ofminerals 80 * C Digestion time 30 minutes Filtration temperature 60 ”C Fibration time 5 minutes Filtration speed 1.3 tonnes of P 2 0 ^ m 2 /> / & P / day
    The yield of PsG 5 in the final product obtained after steps a and b at the end of the process is equal to 94 s 03%. The yield is calculated on the basis
    B E2017 / 5458
    Get free is carried out in your same operating co-editions as those described in Example 1, with the exception of the feeling that the digestion time is 45 minutes and the filtration time is 5.5 minutes, as illustrated in Table 3 below,
    Tebte $
    Exemi ste 2 Amount of starting phosphate 75 grams Amount of HCl aqueous solution"I! Λ. ZÖ 357.7 grams Ore digestion temperature 60X Digestion time 45 minutes Nitration temperature 6Q »G Filtration time 5.5 minutes Filtration speed 1.1 tonnes of P 2 Qs / m 2 / 4AP / day
    The yield of P 2 Qg after your steps a and b of the process is 93.02%,
    Free 3
    This example is carried out under the same operating conditions as those described in example 1, with the exception that the digestion time is. 80 minutes and. that the filtration time is 4.75 minutes, as illustrated in Table 4 below.
    BE2017 / 5458
    Example 3 Amount of starting phosphate 75 grams Amount of aqueous HCi solution12% 357.7 grams Ore digestion temperature 6CVC Digestion time 60 minutes Filtration temperature eo’c Filtration time 4.75 minutes Filtration speed ï, 3 tonnes of PgOVmVMP / day
    TC efficiency; in the product after your previous steps s and b is 33.16%.
    Example 4
    This example is carried out under the same operating conditions as those described in Example 1, except that the digestion time is 90 minutes and the filtration duration is 2.33 minutes, as illustrated in the table. 5 below.
    Paintings
    Example 4........ Amount of starting phosphate 75 grams Amount of aqueous HCi solution12% 357.7 grams Ore diaeshon temperature 6O’C Dmeeuon time 90 minutes Îiitretten temperature 60 ° C Fikratten time 2.33 minutes i Sound filter speed 2.7 tonnes of PgOs / m ^ HûP / day
    B E2017 / 5458
    The yield of PgOs in the product obtained after your steps
    This exemption is carried out under the same operating conditions as those described in Example 1, except that the digestion time is 10.5 minutes and the filtration time is 25 minutes, as illustrated in the table. 8 below.
    TabteauJ
    Free 5 Amount of starting phosphate 75 grams Quantity of the aqueous solutionof KCi 12% 357.7 grams Ore digestion temperature 8Q J C Digestion time 10.5 minutes Filtration temperature 8C ° C Filtration time 25 minutes Oe filtration speed 0.3 tonnes of PsÔg / nvWâP / day
    The yield in P /% in the product obtained after steps a and b of the process is S8.33%.
    Example 6
    This example is carried out under the same operating conditions as those described in Example 1, with the exception that the digestion time is 15 minutes and the filtration time is 13 minutes as illustrated in Table 7.
    BE2017 / 5458
    Example 6 Amount of starting phosphate 75 grams Amount of HCL aqueous scuhon12% 357.7 grams Digestion temperature of the lead strc Digestion time 15 minutes Filtration temperature 50 5 C Filtration time 13 minutes Fill ration speed 0.5 tonnes of PgöV'mVVlP / day
    The yield of Ρ; Ό§ in the product obtained after your steps a and P do process is 96 J 9%.
    Free 7
    This example is carried out under the same operating conditions as those described in example t, with the exception that the digestion time is 21.5 minutes and the duration of nitration is 9 minutes, as illustrated in table 8. below.
    Table B
    Free 7 Amount of starting phosphate 75 grams Amount of aqueous HCl solution12% 357.7 grams Ore digestion temperature 60 ° C Digestion time 21, o minutes Filtration temperature èœc Filtration time 9 minutes Filtering speed 0.7 tonnes of P 2 ____m% ZâP / day
    B E2017 / 5458
    The yield of PsO 5 in the product obtained after your steps has
    Free S
    This example is carried out under the same operating conditions as those given in Example 1, except that the digestion time is 25 seconds, 33 minutes and the filtration time is 7.33 minutes, as illustrated in table 9 below.
    Free S Amount of starting phosphate 5 grams Amount of RCt aqueous soluson12% 33 , 7 grams Temporärere does digestion of the minorai oh Digestion time 26.33 minutes Filtration temperature ÔÎTC Filtration time , 33 minutes filtration speed 71.3 tonnes of P ^ OymévAP / day
    The yield in P S Q ,; in the product obtained after steps a and b of the process is 95.35%.
    It is understood that the present invention is in no way ümltée in terms of embodiments described above and that many o modifications can be made without departing from the scope of the appended claims.
    BE2017 / 5458
    权利要求:
    Claims (15)
    [1]
    1. Process for the preparation of calcium monohydrogen phosphate comprising the steps of:
    a) digestion in an aqueous medium, for a first period of time, of a source of phosphate with an acid with the formation of a pulp comprising an aqueous phase containing calcium phosphate in solution and a solid phase containing impurities,
    b) a first separation between said aqueous phase containing calcium phosphate in solution and said solid phase containing impurities, during a second period of time,
    c) neutralization of said aqueous phase containing calcium phosphate in solution at a pH sufficient to obtain precipitation in an aqueous medium of insoluble calcium phosphate as the above-mentioned calcium monohydrogen phosphate, and
    d) a second separation between said aqueous medium and said calcium monohydrogenphosphate, characterized in that said first period of time in said step a) of digestion is greater than said second period of time in step b) above,
    [2]
    2. Method according to claim 1, in which the aforementioned steps a) and b) are carried out in a period of less than 2 hours, preferably a period of between 30 and 100 minutes, preferably between 30 and 70 minutes, more preferably between 40 and 85 minutes.
    [3]
    3. Method according to claim 1, in which said first time period of said step a) is between 75 and 100 minutes, preferably between 80 and 95 minutes, or between 20 and 45 minutes, in particular 24 and 40 minutes, preferably between 30 and 35 minutes.
    BE2017 / 5458
    [4]
    4. Method according to any one of the preceding claims, in which said first separation from said step b) is carried out at a filtration speed of at least 0.1 tonnes of PsOg / VâP / rre / day, preferably between 0, 1 and 5 tonnes of P 2 OgA / AP / m 2 / day, more preferably between 0.15 and 3 tonnes of PgOs / vâP / rrF / day, more preferably still between 0.3 and 0.9, in particular between 0.4 and 0.7 tonnes of PsOg / v'âP / m ^ day, said filtration speed being calculated according to the following equation:
    Filtration speed =
    VâP ft T f where,
    Qp2O5 corresponds to the quantity of P 2 Os collected in the filtrate and is expressed in tonnes,
    Ω is the area of the filter expressed in m 2 ,
    ΔΡ is the difference between the set pressure of the filtrate and the pressure applied to the pulp at the time of said first separation and is expressed in bar, and
    Ί) is the first time period of said first separation and is expressed in days.
    [5]
    5 calcium monohydrogen phosphate comprising an attack in an aqueous medium, for a predetermined period of time, of a phosphate source by an acid with formation of a pulp comprising an aqueous phase containing calcium phosphate in solution and a solid phase containing impurities, a first separation between said phase
    5 impurities, to implement said first separation repeated in step b) above.
    5. Method according to any one of the preceding claims, in which said source of phosphate and said acid are introduced into a first reactor comprising said aqueous medium simultaneously or successively, in order to carry out said step a) of digestion and in which said pulp comprising said aqueous phase containing calcium phosphate in solution and said solid phase containing impurities is transferred from the first reactor to a separation means in order to carry out said first separation taken up in step b) above-mentioned.
    [6]
    6. The method of claim 5, wherein said separation means is located between said first reactor and a second reactor.
    2017/5458
    BE2017 / 5458
    [7]
    7. The method of claim 5, wherein said separation means is present in a second reactor into which is introduced said pulp comprising an aqueous phase containing calcium phosphate in solution and a solid phase containing
    [8]
    8. Method according to any one of claims 5 to 7, wherein said separation means is a filter chosen from the group consisting of a rotary filter, preferably with tilting cells, filter
    [9]
    9. Method according to any one of the preceding claims, in which said acid is chosen from the group consisting of hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid and their mixtures.
    10. The method of claim 9, wherein said acid is an aqueous acid solution having an acid concentration of 15% by weight or less, preferably in said first reactor.
    [10]
    10 aqueous and said solid phase, for a predetermined period of time, neutralization of said aqueous phase at a pH sufficient to obtain precipitation of said calcium monohydrogen phosphate, a second separation between said aqueous medium and said calcium monohydrogen phosphate, characterized in that said period
    10 press, belt filter and drum filter.
    [11]
    11. Method according to any one of the preceding claims,
    In which steps a) and b) are carried out at a temperature between 50 ° and 70 ° C., preferably equal to 80 ° C.
    [12]
    12. Method according to any one of the preceding claims, in which said source of phosphate is chosen from the group consisting of a phosphate rock, a phosphate ore,
    25 secondary phosphate sources such as ash, in particular from sewage sludge or pig bone or slurry, or mixtures thereof.
    [13]
    13. Method according to any one of the preceding claims, in which the neutralization step is carried out by means of a
    30 neutralizing agent chosen from the group consisting of calcium-based compounds such as oxide, hydroxide and
    2017/5458
    BE2017 / 5458 of calcium and water-soluble calcium salts, and
    [14]
    14. Use of the calcium monohydrogen phosphate obtained according to any one of the preceding claims for producing produire phosphoric acid,
    15. Use of the calcium monohydrogen phosphate obtained according to any one of claims 1 to 13 in the food industry or in the agricultural or horticultural field.
    2017/5458
    BE2017 / 5458
    SHORT
    PROCESS FOR THE PREPARATION OF MONOHYDROGENOPHOSPHATE
    CALCIUM
    The present invention relates to a process for the preparation of
    [15]
    15 of predetermined time of said step a) of digestion is greater than that of step b) above.
    PATENT COOPERATION TREATY
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    同族专利:
    公开号 | 公开日
    EP3509987B1|2021-04-28|
    BE1024582A1|2018-04-11|
    MA46385A|2019-07-17|
    TN2018000441A1|2020-06-15|
    EA037303B1|2021-03-09|
    BR112018076324A2|2019-03-26|
    PE20190449A1|2019-03-29|
    US20190330063A1|2019-10-31|
    MA46385B1|2021-07-29|
    EP3509987A1|2019-07-17|
    RS62043B1|2021-07-30|
    EA201892689A1|2019-04-30|
    WO2018002071A1|2018-01-04|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    FR2273760A1|1974-06-05|1976-01-02|Israel Chemicals Ltd|IMPROVED PROCESS FOR THE PREPARATION OF FOOD GRADE DICALCIUM PHOSPHATE AND PHOSPHORIC ACID|
    WO2010043262A1|2008-10-16|2010-04-22|Ecophos Sa|Process for the production of high purity phosphoric acid|
    WO2015082468A1|2013-12-02|2015-06-11|Ecophos S.A.|Source of phosphate for agriculture and the food industry|
    GB953156A|1961-08-20|1964-03-25|Makhtsavei Israel|Improvements in or relating to the recovery of phosphoric acid by solvent extraction|
    GB1051521A|1964-02-20|1966-12-14|Israel Mining Ind Inst For Res|Improvements in or relating to a process for the production of substantially iron free aqueous solution of phosphoric acid|
    BE1015013A3|2002-06-28|2004-08-03|Ecophos|Process phosphoric acid production and / or salt thereof and products obtained.|
    BE1015840A3|2003-12-24|2005-10-04|Ecophos|Process leading ore phosphate.|
    法律状态:
    2018-05-03| FG| Patent granted|Effective date: 20180417 |
    优先权:
    申请号 | 申请日 | 专利标题
    BE2016/5482|2016-06-28|
    BE201605482|2016-06-28|
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