CN113716537A - Preparation method of powdery solid phosphoric acid - Google Patents
Preparation method of powdery solid phosphoric acid Download PDFInfo
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- CN113716537A CN113716537A CN202111008508.2A CN202111008508A CN113716537A CN 113716537 A CN113716537 A CN 113716537A CN 202111008508 A CN202111008508 A CN 202111008508A CN 113716537 A CN113716537 A CN 113716537A
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- phosphoric acid
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 174
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 80
- 239000007787 solid Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 35
- 238000002425 crystallisation Methods 0.000 claims abstract description 28
- 230000008025 crystallization Effects 0.000 claims abstract description 28
- 239000013078 crystal Substances 0.000 claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 17
- DLYUQMMRRRQYAE-UHFFFAOYSA-N phosphorus pentoxide Inorganic materials O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 8
- 230000001965 increasing effect Effects 0.000 claims abstract description 8
- 239000000411 inducer Substances 0.000 claims abstract description 6
- 230000009466 transformation Effects 0.000 claims abstract description 6
- 239000012043 crude product Substances 0.000 claims abstract description 5
- 238000010008 shearing Methods 0.000 claims abstract description 3
- 229920000137 polyphosphoric acid Polymers 0.000 claims description 23
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 claims description 10
- 229940005657 pyrophosphoric acid Drugs 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- UEZVMMHDMIWARA-UHFFFAOYSA-N Metaphosphoric acid Chemical compound OP(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 230000001939 inductive effect Effects 0.000 claims description 2
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000000047 product Substances 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000005259 measurement Methods 0.000 abstract 1
- 235000011007 phosphoric acid Nutrition 0.000 description 70
- 239000007788 liquid Substances 0.000 description 6
- 238000005406 washing Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- -1 feeds Substances 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000007805 chemical reaction reactant Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 229940048084 pyrophosphate Drugs 0.000 description 1
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 description 1
- 229940048086 sodium pyrophosphate Drugs 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- RYCLIXPGLDDLTM-UHFFFAOYSA-J tetrapotassium;phosphonato phosphate Chemical compound [K+].[K+].[K+].[K+].[O-]P([O-])(=O)OP([O-])([O-])=O RYCLIXPGLDDLTM-UHFFFAOYSA-J 0.000 description 1
- 235000019818 tetrasodium diphosphate Nutrition 0.000 description 1
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/234—Purification; Stabilisation; Concentration
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
Abstract
The invention discloses a preparation method of powdery solid phosphoric acid, and relates to the technical field of solid phosphoric acid production. With P2O5Polyphosphoric acid with the mass fraction of 81-86 percent is taken as a raw material, water is added under full stirring, and P is added2O5The mass fraction is adjusted to 77-81 percent; synchronously adding a crystallization inducer to control the temperature of the reaction materials to be 40-75 ℃ to initiate the crystallization of the reaction materials, and obtaining a crude product of solid phosphoric acid containing crystals; then, continuously cooling the reaction materials, controlling the temperature of the reaction materials to be kept at 30-55 ℃, and fully stirring to promote the crystallization and transformation of the reaction materials; after the viscosity of the reaction material is increased to be difficult to flow, the crystallized solid phosphoric acid is subjected to crystallization promotion and crushing treatment by adopting an intensified stirring or shearing method to obtain powdery solid phosphoric acid. The preparation method has the advantages of simple preparation process, easy control, low energy consumption and cost, good repeatability and stable product quality, is favorable for realizing industrial production, and simultaneously the prepared solid phosphoric acid product is convenient for transportation and measurement.
Description
Technical Field
The invention relates to the technical field of solid phosphoric acid production, in particular to a preparation method of powdery solid phosphoric acid.
Background
Phosphoric acid is a basic chemical raw material, is widely applied to various industries, is used in the industries of food additives, feeds, pesticides, washing, electronics, medicines, water treatment, smelting, flame retardants, chemical fertilizers and the like, and can also be used for pigments, electric forging, rust prevention, a vegetation agent, an antioxidant synergist, a flavoring agent and the like. Phosphoric acid is generally classified into fertilizer grade, industrial grade, food grade and electronic grade according to the amount of impurities contained in the phosphoric acid. Phosphoric acid is classified into liquid phosphoric acid and solid phosphoric acid according to the state, wherein the liquid phosphoric acid is a colorless viscous liquid, P2O5The content is 50-70%; the solid phosphoric acid is colorless glass-like, P2O5The content is 70-90%, and the product has strong hygroscopicity. Compared with liquid phosphoric acid, the solid phosphoric acid is more convenient to transport, the safety of the transport process is higher, and the use is more convenient.
Patent CN101269804A discloses a method for producing high-purity orthophosphoric acid crystal, which comprises the specific process of H3P04Phosphoric acid with the mass percent of 96.5-99% is used as a raw material, when the temperature of the material is controlled to be 28-42 ℃, seed crystals accounting for l-10% of the mass of the raw material acid are added, the temperature is kept for 0.1-2 h, then the temperature is reduced to 26-35 ℃, the temperature is kept for 0.5-2.5 h, centrifugal filtration is carried out, the obtained crystals are washed, orthophosphoric acid crystals are obtained, and recrystallization and purification are carried out to obtain the high-purity orthophosphoric acid crystals. The method for producing the phosphoric acid crystal has the advantages that the yield of the product is reduced due to the need of washing the crystal, and meanwhile, acid-containing wastewater is generated in the washing process in the process and needs to be additionally treated. The phosphoric acid crystal obtained by recrystallization cannot be controlled in crystal size, and needs to be crushed when in use, so that the taking and the use are troublesome.
Patent CN103569980A discloses a method for producing solid phosphoric acid, which comprises stirring and mixing phosphoric acid and phosphorus pentoxide, keeping a certain temperature (80-150 ℃), continuously adding phosphorus pentoxide, immediately packaging when the concentration of phosphoric acid reaches 118-128%, cooling to normal temperature, and solidifying to obtain lump solid phosphoric acid. In the method, after phosphoric acid is cooled and solidified, the prepared solid phosphoric acid is fixed to the shape of a container during cooling, crushing treatment is required during use, and the solid phosphoric acid with the fixed size is inconvenient to meter during use.
Patent CN101544360A discloses a method for preparing crystalline phosphoric acid, which comprises directly cooling 85% phosphoric acid or concentrating and cooling, adding seed crystal, stirring, slowly cooling, growing crystal, and centrifuging to obtain crystalline phosphoric acid. The crystalline phosphoric acid prepared by the method is limited by the concentration of the raw material, and high-concentration solid phosphoric acid is not easy to prepare. Also, the method requires washing of the crystals, which results in a decrease in product yield, and also requires additional treatment of acid-containing wastewater generated during the washing process. The crystal size of the crystallized phosphoric acid crystal cannot be controlled, and the phosphoric acid crystal needs to be crushed when in use, so that the phosphoric acid crystal is troublesome to take and use.
German patent No.925465 proposes a process for preparing solid phosphoric acid having a pyrophosphate concentration of 92%, in which P2O5The mixture obtained by dissolving in water or orthophosphoric acid at a temperature of at most 200 ℃ is cooled to effect crystallization to obtain solid pyrophosphoric acid. The use of high temperatures in the process may introduce impurities from the reaction vessel into the acid. In addition, a relatively long time is required to achieve crystallization.
As mentioned in U.S. Pat. No.5700700, solid phosphoric acid is added to liquid polyphosphoric acid and a water-insoluble dispersion at a temperature below the melting point of pyrophosphoric acid and stirred until the polyphosphoric acid is converted to pyrophosphoric acid. In order to obtain a high-purity solid phosphoric acid, the mixture is filtered and then treated under vacuum to remove the non-aqueous solvent adhering to the pyrophosphoric acid, requiring complicated and costly operations to obtain a pure solid phosphoric acid.
The preparation method of the solid phosphoric acid mostly comprises the steps of treating the phosphoric acid, placing the treated phosphoric acid for crystallization and solidification, wherein the shape of the solidified solid phosphoric acid is the shape of a container during crystallization, and although the solid phosphoric acid in the state solves the transportation problem, the solid phosphoric acid is inconvenient to measure and use during taking and can be accurately measured after being crushed.
Disclosure of Invention
The invention aims to provide a preparation method of powdery solid phosphoric acid, which solves the problems that the production process of the solid phosphoric acid is complex and the solid phosphoric acid obtained by crystallization and solidification can be measured only after being crushed in the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme: the preparation method of the powdery solid phosphoric acid is characterized by comprising the following steps of:
s1. with P2O5Polyphosphoric acid with the mass fraction of 81-86 percent is taken as a raw material and added into a reactor, water is added into the polyphosphoric acid under full stirring, and P is added2O5The mass fraction is adjusted to 77-81%. Polyphosphoric acid can be accurately diluted into reaction raw materials with different concentrations according to requirements, so that the reaction raw materials are convenient to accurately control, and P2O5The reaction raw materials with the mass fraction of 77-81% are easier to crystallize. The reactor may employ a kneader having mixing and crushing functions.
S2, synchronously adding a crystallization inducer into the reaction material in the water adding process, controlling the temperature of the reaction material to be 40-75 ℃ under the condition of fully stirring to initiate the reaction material to crystallize, and crystallizing for 0.5-2 hours to obtain a solid phosphoric acid crude product containing crystals. The reaction temperature is controlled by a temperature control system of the kneader device, and crystallization is easier in this temperature range after water is sufficiently mixed with polyphosphoric acid.
S3, after obtaining the crude product of the solid phosphoric acid, continuously cooling the reaction materials, and controlling the temperature of the reaction materials to be kept at 30 ℃
Fully stirring at 55 ℃ to promote the crystallization and transformation of the reaction materials, wherein the crystallization and transformation time is 2-4 hours. Too low a temperature retards the crystallization transition and too high a temperature destroys the crystallization.
S4, after the viscosity of the reaction material is increased to be difficult to flow, performing crystallization promotion and crushing treatment on the crystallized solid phosphoric acid for 0.5-1 hour by adopting an intensified stirring or shearing method, and discharging after crushing is completed to obtain powdery solid phosphoric acid.
The further technical proposal is that the crystallization inducing agent in the step S2 is one or more of pyrophosphoric acid with purity of more than 80%, crystalline polyphosphoric acid with purity of 109-111%, metaphosphoric acid and phosphorous acid.
The further technical proposal is that the addition amount of the crystallization inducer in the step S2 is 3-15% of the mass of the raw material polyphosphoric acid.
The further technical scheme is that the purity of the powdery solid phosphoric acid is 95-100%, the content of polyphosphoric acid is higher than 95%, and the particle size is 0.05-10 mm.
Compared with the prior art, the invention has the beneficial effects that: the preparation method is simple, and the powdery solid phosphoric acid is produced in one step by using polyphosphoric acid as a raw material and crystalline polyphosphoric acid, pyrophosphoric acid, metaphosphoric acid and the like as crystallization inducers through the steps of crystallization initiation, crystallization transformation promotion and crushing. The preparation process is simple, easy to control, low in energy consumption and cost, good in repeatability and stable in product quality, and is beneficial to realizing industrial production.
Drawings
FIG. 1 is a schematic representation of a solid powder phosphoric acid thus prepared.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
Weighing P2O5Adding 65kg of polyphosphoric acid with the mass fraction of 84% into a reactor, setting the rotating speed to be 35r/min, then adding 3.25kg of water into the reactor, controlling the temperature of the material to be 45 ℃, continuously adding 5.85kg of pyrophosphoric acid, stirring for 1h, setting the temperature of the reactor to be 26 ℃, after 3h, increasing the viscosity of the material, and adjusting the rotating speed to be 10r/min until solid powder with the purity of more than 98% is obtainedThe particle size of the powdery phosphoric acid is 0.2-1.5 mm, the sample state object diagram is shown in figure 1, and the prepared fixed phosphoric acid is powder and is obviously different from bulk or irregularly-shaped crystal phosphoric acid.
Example 2
Weighing P2O5Adding 65kg of polyphosphoric acid with the mass fraction of 81% into a reactor, setting the rotating speed to be 40r/min, then adding 1.25kg of water into the reactor, controlling the temperature of the material to be 75 ℃, continuously adding 3.9kg of pyrophosphoric acid, stirring for 0.5 hour, setting the temperature of the reactor to be 50 ℃, after 4 hours, increasing the viscosity of the material, and adjusting the rotating speed to be 15r/min until solid powdery phosphoric acid is obtained, wherein the purity of the solid phosphoric acid is more than 99%, and the particle size is 0.1-1 mm.
Example 3
Weighing P2O5Adding 65kg of polyphosphoric acid with the mass fraction of 86% into a reactor, setting the rotating speed to be, then adding 4kg of water into the reactor, controlling the temperature of the material to be 65 ℃, continuously adding 5.85kg of sodium pyrophosphate, stirring for 1.5 hours, setting the temperature of the reactor to be 35 ℃, and after 3 hours, increasing the viscosity of the material, and adjusting the rotating speed to be 20r/min until solid powdery phosphoric acid is obtained, wherein the purity of the solid phosphoric acid is more than 95%, and the particle size is 0.08-1 mm.
Example 4
Weighing P2O5Adding 65kg of polyphosphoric acid with the mass fraction of 82% into a reactor, setting the rotating speed to be 40r/min, then adding 4kg of water into the reactor, controlling the temperature of the material to be 60 ℃, continuously adding 8.5kg of potassium pyrophosphate, stirring for 1 hour, setting the temperature of the reactor to be 45 ℃, after 2 hours, increasing the viscosity of the material, and adjusting the rotating speed to be 5r/min until solid powdery phosphoric acid is obtained, wherein the purity of the solid phosphoric acid is more than 98%, and the particle size is 0.5-10 mm.
Example 5
Weighing P2O5Adding 80kg of polyphosphoric acid with the mass fraction of 86% into a reactor, setting the rotating speed to be 30r/min, then adding 5.5kg of water into the reactor, controlling the temperature of the material to be 55 ℃, continuously adding 6.8kg of crystallized polyphosphoric acid, stirring for 1.5 hours, setting the temperature of the reactor to be 20 ℃, and after 3 hours, addingAnd (3) adjusting the rotating speed to 35r/min when the viscosity of the material rises until solid powdery phosphoric acid is obtained, wherein the purity of the solid phosphoric acid is more than 95%, and the particle size is 0.05-0.9 mm.
Comparative examples
Referring to example 5, the reaction starting material was changed from polyphosphoric acid to orthophosphoric acid. Specifically, orthophosphoric acid (P) is weighed2O572.45 percent by mass) of phosphoric acid is added into the reactor, the set rotating speed is 30r/min, and the orthophosphoric acid P is added into the reactor2O5The mass fraction does not reach the range (77-81%) specified in the method, concentration adjustment is not carried out without adding water, the temperature is directly increased, the material temperature is controlled to be 55 ℃, 7kg of crystallized polyphosphoric acid is added after the material temperature reaches 55 ℃, the temperature of the reactor is set to be 20 ℃ after stirring for 2 hours, the viscosity of the material in the reactor cannot rise after 9 hours, and the material state is still slightly viscous liquid acid.
Although the invention has been described herein with reference to a number of illustrative embodiments thereof, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the spirit and scope of the principles of this disclosure. More specifically, various variations and modifications are possible in the component parts or arrangements of the subject combination arrangement within the scope of the disclosure, the drawings and the appended claims. In addition to variations and modifications in the component parts or arrangements, other uses will also be apparent to those skilled in the art.
Claims (4)
1. The preparation method of the powdery solid phosphoric acid is characterized by comprising the following steps of:
s1. with P2O5Adding polyphosphoric acid with the mass fraction of 81-86 percent as a raw material into a reactor, adding water into the polyphosphoric acid under full stirring, and adding P2O5The mass fraction is adjusted to 77-81 percent;
s2, synchronously adding a crystallization inducer into the reaction material in the water adding process, controlling the temperature of the reaction material to be 40-75 ℃ under the condition of fully stirring to initiate the reaction material to crystallize, wherein the crystallization time is 0.5-2 hours, and obtaining a solid phosphoric acid crude product containing crystals;
s3, after a solid phosphoric acid crude product is obtained, continuously cooling the reaction material, controlling the temperature of the reaction material to be kept at 30-55 ℃, fully stirring to promote the crystallization and transformation of the reaction material, wherein the crystallization and transformation time is 2-4 hours;
s4, after the viscosity of the reaction material is increased to be difficult to flow, performing crystallization promotion and crushing treatment on the crystallized solid phosphoric acid for 0.5-1 hour by adopting an intensified stirring or shearing method, and discharging after crushing is completed to obtain powdery solid phosphoric acid.
2. The method for preparing solid phosphoric acid in powder form according to claim 1, wherein: the crystallization inducing agent in the step S2 is one or more of pyrophosphoric acid with purity of more than 80%, crystalline polyphosphoric acid with purity of 109% -111%, metaphosphoric acid and phosphorous acid.
3. The method for preparing solid phosphoric acid in powder form according to claim 1, wherein: the addition amount of the crystallization inducer in the step S2 is 3-15% of the mass of the raw material polyphosphoric acid.
4. The method for preparing solid phosphoric acid in powder form according to claim 1, wherein: the purity of the powdery solid phosphoric acid is 95-100%, the content of polyphosphoric acid is higher than 95%, and the particle size is 10-500 micrometers.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113896693A (en) * | 2021-09-08 | 2022-01-07 | 云南云天化股份有限公司 | Preparation method of polyphosphoric acid piperazine |
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|---|---|---|---|---|
| US3853486A (en) * | 1971-02-25 | 1974-12-10 | Knapsack Ag | Process for the manufacture of pyrophosphoric acid by crystallization |
| CA1265315A (en) * | 1985-05-08 | 1990-02-06 | Phillip D. Mollere | Process for seed crystal preparation for phosphoric acid crystallization |
| CN101525128A (en) * | 2009-04-08 | 2009-09-09 | 瓮福（集团）有限责任公司 | Production method of solid orthophosphoric acid |
| CN103569980A (en) * | 2012-08-06 | 2014-02-12 | 防城港博森化工有限公司 | Production method of solid phosphoric acid |
| CN113120875A (en) * | 2021-04-25 | 2021-07-16 | 云南云天化股份有限公司 | Production method of low-impurity wet-process phosphoric acid and high-quality alpha-hemihydrate gypsum |
-
2021
- 2021-08-31 CN CN202111008508.2A patent/CN113716537A/en active Pending
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|---|---|---|---|---|
| US3853486A (en) * | 1971-02-25 | 1974-12-10 | Knapsack Ag | Process for the manufacture of pyrophosphoric acid by crystallization |
| CA1265315A (en) * | 1985-05-08 | 1990-02-06 | Phillip D. Mollere | Process for seed crystal preparation for phosphoric acid crystallization |
| CN101525128A (en) * | 2009-04-08 | 2009-09-09 | 瓮福（集团）有限责任公司 | Production method of solid orthophosphoric acid |
| CN103569980A (en) * | 2012-08-06 | 2014-02-12 | 防城港博森化工有限公司 | Production method of solid phosphoric acid |
| CN113120875A (en) * | 2021-04-25 | 2021-07-16 | 云南云天化股份有限公司 | Production method of low-impurity wet-process phosphoric acid and high-quality alpha-hemihydrate gypsum |
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| Title |
|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113896693A (en) * | 2021-09-08 | 2022-01-07 | 云南云天化股份有限公司 | Preparation method of polyphosphoric acid piperazine |
| CN113896693B (en) * | 2021-09-08 | 2024-01-02 | 云南云天化股份有限公司 | Preparation method of piperazine polyphosphate |
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