CN105217591B - A kind of phosphoric acid by wet process prepares tripotassium phosphate method - Google Patents

A kind of phosphoric acid by wet process prepares tripotassium phosphate method Download PDF

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CN105217591B
CN105217591B CN201510606956.0A CN201510606956A CN105217591B CN 105217591 B CN105217591 B CN 105217591B CN 201510606956 A CN201510606956 A CN 201510606956A CN 105217591 B CN105217591 B CN 105217591B
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phosphoric acid
wet
tripotassium phosphate
potassium hydroxide
prepares
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CN105217591A (en
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廖吉星
刘琼
朱飞武
张伟
徐圆
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Guizhou Kailin Group Co Ltd
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Guizhou Kailin Group Co Ltd
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Abstract

Tripotassium phosphate technical field is prepared the present invention relates to phosphoric acid by wet process, especially a kind of phosphoric acid by wet process prepares tripotassium phosphate method, it is analyzed by the content to the sulfate radical in phosphoric acid by wet process, in conjunction with the addition of ground phosphate rock, so that sulfate radical, iron, the cations such as aluminium and fluorine, the anion such as silicon form precipitation, it is passed through ammonia thereto again or adds ammoniacal liquor, regulation pH value be 37 after, so that it forms ammonium phosphate salt solution, again by filtering, so that the precipitation for being formed is filtered in slag liquid, so that phosphoric acid by wet process is purified, ensure that the purity of the tripotassium phosphate product of subsequent production;After being reacted in conjunction with ammonium phosphate salt slurry and potassium hydroxide or saleratus, potassium carbonate, it is evaporated crystallization in the case where negative pressure pressure is 0~0.01MPa again, and then cause that the crystal mass of tripotassium phosphate product is more excellent, purity is higher, and reduce the consumption of potassium ion, reduce tripotassium phosphate production cost, it is to avoid the waste of resource.

Description

A kind of phosphoric acid by wet process prepares tripotassium phosphate method
Technical field
Tripotassium phosphate technical field is prepared the present invention relates to phosphoric acid by wet process, especially a kind of phosphoric acid by wet process prepares tripotassium phosphate Method.
Background technology
Tripotassium phosphate, it is applied to multi-field, such as agricultural;Its production method for using at present is mainly neutralisation, After being reacted using phosphoric acid and potassium hydroxide or saleratus, potassium carbonate, by the control of reaction end, then will neutralize After liquid is concentrated, insoluble matter is removed, crystallized after being then cooled to again, centrifugation is dried, product is obtained.But, due to Phosphoric acid is divided into thermal phosphoric acid and phosphoric acid by wet process, and phosphoric acid by wet process mainly uses phosphorus ore that the original of weak acid is produced according to strong acid with inorganic acid Reason is carried out, even if using inorganic acid, such as sulfuric acid to leach P elements therein so that sulfate radical and other elements, such as calcium constituent shape Into after calcium sulfate insoluble matter, what filtering was obtained;But, because the quality of phosphorus ore will be impacted to the quality of phosphoric acid by wet process, So that the quality of the phosphoric acid product of phosphoric acid by wet process preparation is unstable, meanwhile, also cause that the impurity content in the phosphoric acid for obtaining is higher, Purity is relatively low so that when the phosphoric acid prepared using phosphoric acid by wet process is to produce phosphoric acid potassium salt product, it can not only cause potassium phosphate The purity of salt is relatively low, and quality is unstable, at the same can also cause to be caused in preparation process the potassium hydroxide that adds or potassium carbonate, Potassium ion in saleratus forms insoluble matter with other impurities element interaction, in turn results in the waste of potassium ion, causes hydrogen-oxygen Change potassium, the addition of potassium carbonate or saleratus increases, in turn result in that preparation cost is higher, resource consumption is larger.
Based on this, this researcher is directed to drawbacks described above, is studied on the basis of existing tripotassium phosphate preparation technology, And then for tripotassium phosphate preparing technical field provides a kind of new approaches.
The content of the invention
In order to solve above-mentioned technical problem present in prior art, the present invention provides a kind of phosphoric acid by wet process and prepares tricresyl phosphate Potassium method.
It is achieved particular by following technical scheme:
A kind of phosphoric acid by wet process prepares tripotassium phosphate method, comprises the following steps:
(1) phosphoric acid by wet process that phosphorus pentoxide concentration is 15-35% is taken, by analyzing the content of sulfate radical therein, and It is added thereto to ground phosphate rock, it with the mass ratio of the content of sulfate radical is (1~1.2) that the addition of ground phosphate rock is:1, treat that it reacts After 30-60min, then it is added thereto to ammoniacal liquor or is passed through ammonia, regulation pH value is 3~7, filtering obtains slurry and filter residue;
(2) potassium hydroxide is taken, potassium hydroxide is added in slurry, in the addition and phosphoric acid by wet process of control potassium hydroxide The mol ratio of the amount of phosphorus pentoxide is 6:1, after the completion for the treatment of that it feeds intake, control negative pressure pressure for 0-0.01MPa, use temperature for 85-95 DEG C of evaporative crystallization, treats a large amount of crystal occur in solution, stops evaporation, is cooled to room temperature, filters, and obtains mother liquor and first finished product; First finished product washing, obtains tripotassium phosphate.
Described tripotassium phosphate, its purity is 98.1~99.31%.
Described washing, mixes in the cleaning solution return to step 1 that its washing is produced with phosphoric acid by wet process.
Described evaporative crystallization, after the gas produced in crystallization process is absorbed using phosphoric acid,diluted, returns and step 1 In phosphoric acid by wet process mixing.
Described phosphoric acid,diluted, its concentration is 15-35%.
Described mother liquor sends to composite fertilizer production line;Described filter residue sends to composite fertilizer production line.
Described potassium hydroxide, it is that solid is added in slurry.
Described potassium hydroxide, it is added in slurry after potassium hydroxide is configured into solution.
Described potassium hydroxide is replaced using saleratus or potassium carbonate, during using potassium carbonate to replace, its with it is wet The mol ratio of the amount of phosphorus pentoxide is 3.8~4 in method phosphoric acid:1;During using potassium carbonate to replace, its with phosphoric acid by wet process in five The mol ratio for aoxidizing the amount of two phosphorus is 6:1.
Described ground phosphate rock, the content of its phosphorus pentoxide is to be not less than 7%.
Described ground phosphate rock, its granularity is 40-140 mesh.
Compared with prior art, technique effect of the invention is embodied in:
15-35% is defined to by the concentration to phosphoric acid by wet process in terms of phosphorus pentoxide, then to the sulfuric acid in phosphoric acid by wet process The content of root is analyzed, in conjunction with the addition of ground phosphate rock so that the anion such as the cation such as sulfate radical, iron, aluminium and fluorine, silicon Precipitation is formed, then is passed through ammonia thereto or is added ammoniacal liquor, regulation pH value is for after 3-7 so that it forms ammonium phosphate salt solution, Again by filtering so that the precipitation of formation is filtered in slag liquid so that phosphoric acid by wet process is purified, it is ensured that subsequent production The purity of tripotassium phosphate product;After being reacted in conjunction with ammonium phosphate salt slurry and potassium hydroxide or saleratus, potassium carbonate, It is evaporated crystallization in the case where negative pressure pressure is 0~0.01MPa again, and then so that tripotassium phosphate product crystal mass compared with Excellent, purity is higher, and also reduces the consumption of potassium ion, reduce tripotassium phosphate production cost, it is to avoid the wave of resource Take.
The present invention causes the control of negative pressure pressure especially by the accurate control of negative pressure pressure so that solution Degree of supersaturation is controlled, and the speed that the precipitation of tripotassium phosphate crystal is further prepared to phosphoric acid by wet process is controlled, Jin Erzhun The amount of precipitation of true positioning tripotassium phosphate, it is ensured that the purity of tripotassium phosphate product so that the purity of tripotassium phosphate product reaches 98.1~99.31%.
Mother liquor after crystallization is also sent to composite fertilizer production line by the present invention, and then causes that the discharge capacity of waste liquid is reduced, resource It is comprehensively utilized, absorption recovery is carried out to the gas produced in evaporation and crystal process in conjunction with phosphoric acid,diluted, and be sent to step Mixed with phosphoric acid by wet process in rapid 1, and then reached the purpose for reclaiming ammonium ion, the discharge capacity and resource for reducing waste gas are disappeared Consumption, reduces production cost.
Specific embodiment
Technical scheme is further limited with reference to specific embodiment, but claimed Scope is not only limited to description.
Embodiment 1
A kind of phosphoric acid by wet process prepares tripotassium phosphate method, comprises the following steps:
(1) phosphoric acid by wet process that phosphorus pentoxide concentration is 15% is taken, by analyzing the content of sulfate radical therein, and to it Middle addition ground phosphate rock, it with the mass ratio of the content of sulfate radical is 1 that the addition of ground phosphate rock is:1, after it reacts 30min, then to Wherein add ammoniacal liquor or be passed through ammonia, regulation pH value is 3, filtering obtains slurry and filter residue;
(2) potassium hydroxide is taken, potassium hydroxide is added in slurry, in the addition and phosphoric acid by wet process of control potassium hydroxide The mol ratio of the amount of phosphorus pentoxide is 6:1, after the completion for the treatment of that it feeds intake, control negative pressure pressure for 0MPa, it is 85 DEG C to use temperature Evaporative crystallization, treats a large amount of crystal occur in solution, stops evaporation, is cooled to room temperature, filters, and obtains mother liquor and first finished product;First finished product Washing, obtains tripotassium phosphate.
Described tripotassium phosphate, its purity is 98.1%.
Described washing, mixes in the cleaning solution return to step 1 that its washing is produced with phosphoric acid by wet process.
Described evaporative crystallization, after the gas produced in crystallization process is absorbed using phosphoric acid,diluted, returns and step 1 In phosphoric acid by wet process mixing.
Described phosphoric acid,diluted, its concentration is 15%.
Described mother liquor sends to composite fertilizer production line;Described filter residue sends to composite fertilizer production line.
Described potassium hydroxide, it is that solid is added in slurry.
Described ground phosphate rock, the content of its phosphorus pentoxide is to be not less than 7%.
Described ground phosphate rock, its granularity is 40 mesh.
Embodiment 2
A kind of phosphoric acid by wet process prepares tripotassium phosphate method, comprises the following steps:
(1) phosphoric acid by wet process that phosphorus pentoxide concentration is 35% is taken, by analyzing the content of sulfate radical therein, and to it Middle addition ground phosphate rock, it with the mass ratio of the content of sulfate radical is 1.2 that the addition of ground phosphate rock is:1, after it reacts 60min, then It is added thereto to ammoniacal liquor or is passed through ammonia, regulation pH value is 7, filtering obtains slurry and filter residue;
(2) potassium hydroxide is taken, potassium hydroxide is added in slurry, in the addition and phosphoric acid by wet process of control potassium hydroxide The mol ratio of the amount of phosphorus pentoxide is 6:1, after the completion for the treatment of that it feeds intake, control negative pressure pressure for 0.01MPa, it is 95 to use temperature DEG C evaporative crystallization, treats a large amount of crystal occur in solution, stops evaporation, is cooled to room temperature, filters, and obtains mother liquor and first finished product;Just into Product are washed, and obtain tripotassium phosphate.
Described tripotassium phosphate, its purity is 99.31%.
Described washing, mixes in the cleaning solution return to step 1 that its washing is produced with phosphoric acid by wet process.
Described evaporative crystallization, after the gas produced in crystallization process is absorbed using phosphoric acid,diluted, returns and step 1 In phosphoric acid by wet process mixing.
Described phosphoric acid,diluted, its concentration is 35%.
Described mother liquor sends to composite fertilizer production line;Described filter residue sends to composite fertilizer production line.
Described potassium hydroxide, it is added in slurry after potassium hydroxide is configured into solution.
Described ground phosphate rock, the content of its phosphorus pentoxide is to be not less than 10%.
Described ground phosphate rock, its granularity is 140 mesh.
Embodiment 3
A kind of phosphoric acid by wet process prepares tripotassium phosphate method, comprises the following steps:
(1) phosphoric acid by wet process that phosphorus pentoxide concentration is 20% is taken, by analyzing the content of sulfate radical therein, and to it Middle addition ground phosphate rock, it with the mass ratio of the content of sulfate radical is 1.1 that the addition of ground phosphate rock is:1, after it reacts 40min, then It is added thereto to ammoniacal liquor or is passed through ammonia, regulation pH value is 5, filtering obtains slurry and filter residue;
(2) potassium hydroxide is taken, potassium hydroxide is added in slurry, in the addition and phosphoric acid by wet process of control potassium hydroxide The mol ratio of the amount of phosphorus pentoxide is 6:1, after the completion for the treatment of that it feeds intake, control negative pressure pressure for 0.005MPa, use temperature for 90 DEG C of evaporative crystallizations, treat a large amount of crystal occur in solution, stop evaporation, are cooled to room temperature, filter, and obtain mother liquor and first finished product;Just Finished product is washed, and obtains tripotassium phosphate.
Described tripotassium phosphate, its purity is 98.7%.
Described washing, mixes in the cleaning solution return to step 1 that its washing is produced with phosphoric acid by wet process.
Described evaporative crystallization, after the gas produced in crystallization process is absorbed using phosphoric acid,diluted, returns and step 1 In phosphoric acid by wet process mixing.
Described phosphoric acid,diluted, its concentration is 25%.
Described mother liquor sends to composite fertilizer production line;Described filter residue sends to composite fertilizer production line.
Described ground phosphate rock, the content of its phosphorus pentoxide is to be not less than 16%.
Described ground phosphate rock, its granularity is 100 mesh.
Embodiment 4
On the basis of embodiment 1,, with embodiment 1, described potassium hydroxide is replaced using potassium carbonate for other, its with The mol ratio of the amount of phosphorus pentoxide is 3.8 in phosphoric acid by wet process:1.
Embodiment 5
On the basis of embodiment 2,, with embodiment 2, described potassium hydroxide is replaced using potassium carbonate for other, its with The mol ratio of the amount of phosphorus pentoxide is 4 in phosphoric acid by wet process:1.
Embodiment 6
On the basis of embodiment 3,, with embodiment 3, described potassium hydroxide is replaced using potassium carbonate for other, its with The mol ratio of the amount of phosphorus pentoxide is 6 in phosphoric acid by wet process:1.
Embodiment 7
On the basis of embodiment 3,, with embodiment 3, described potassium hydroxide is replaced using potassium carbonate for other, its with The mol ratio of the amount of phosphorus pentoxide is 3.9 in phosphoric acid by wet process:1.

Claims (10)

1. a kind of phosphoric acid by wet process prepares tripotassium phosphate method, it is characterised in that comprise the following steps:
(1) phosphoric acid by wet process that phosphorus pentoxide concentration is 15-35% is taken, by analyzing the content of sulfate radical therein, and to it Middle addition ground phosphate rock, it with the mass ratio of the content of sulfate radical is (1~1.2) that the addition of ground phosphate rock is:1, treat its reaction 30- After 60min, then it is added thereto to ammoniacal liquor or is passed through ammonia, regulation pH value is 3~7, filtering obtains slurry and filter residue;
(2) potassium hydroxide is taken, potassium hydroxide is added in slurry, control the addition and five oxygen in phosphoric acid by wet process of potassium hydroxide The mol ratio for changing the amount of two phosphorus is 6:1, after the completion for the treatment of that it feeds intake, control negative pressure pressure for 0-0.01MPa, it is 85- to use temperature 95 DEG C of evaporative crystallizations, treat a large amount of crystal occur in solution, stop evaporation, are cooled to room temperature, filter, and obtain mother liquor and first finished product;Just Finished product is washed, and obtains tripotassium phosphate.
2. phosphoric acid by wet process as claimed in claim 1 prepares tripotassium phosphate method, it is characterised in that described tripotassium phosphate, its Purity is 98.1~99.31%.
3. phosphoric acid by wet process as claimed in claim 1 prepares tripotassium phosphate method, it is characterised in that described washing, its washing Mix with phosphoric acid by wet process in the cleaning solution return to step 1 of generation.
4. phosphoric acid by wet process as claimed in claim 1 prepares tripotassium phosphate method, it is characterised in that described evaporative crystallization, After the gas produced in crystallization process is absorbed using phosphoric acid,diluted, return mixes with the phosphoric acid by wet process in step 1.
5. phosphoric acid by wet process as claimed in claim 4 prepares tripotassium phosphate method, it is characterised in that described phosphoric acid,diluted, and its is dense It is 15-35% to spend.
6. phosphoric acid by wet process as claimed in claim 1 prepares tripotassium phosphate method, it is characterised in that described mother liquor is sent to compound Fertile production line;Described filter residue sends to composite fertilizer production line.
7. phosphoric acid by wet process as claimed in claim 1 prepares tripotassium phosphate method, it is characterised in that described potassium hydroxide, its It is that solid is added in slurry.
8. phosphoric acid by wet process as claimed in claim 1 prepares tripotassium phosphate method, it is characterised in that described potassium hydroxide, its It is to be added in slurry after potassium hydroxide is configured into solution.
9. phosphoric acid by wet process as claimed in claim 1 prepares tripotassium phosphate method, it is characterised in that described potassium hydroxide is used Saleratus or potassium carbonate replaces, and during using potassium carbonate to replace, it rubs with the amount of phosphorus pentoxide in phosphoric acid by wet process You are than being 3.8~4:1;During using potassium carbonate to replace, it is 6 with the mol ratio of the amount of phosphorus pentoxide in phosphoric acid by wet process:1.
10. phosphoric acid by wet process as claimed in claim 1 prepares tripotassium phosphate method, it is characterised in that described ground phosphate rock, and it five The content of two phosphorus is aoxidized to be not less than 7%.
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Family Cites Families (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB495487A (en) * 1937-06-05 1938-11-15 Friedrich Paul Kerschbaum An improved process for the production of metal phosphates
US3338675A (en) * 1964-01-22 1967-08-29 American Cyanamid Co Clarification of concentrated wet process phosphoric acid
JPS627614A (en) * 1985-07-03 1987-01-14 Mitsui Toatsu Chem Inc Condensing method for wet process phosphoric acid liquid
CN101219781A (en) * 2007-12-07 2008-07-16 苏兆祥 Clean production of phosphate and phosphoric acid with low ore grade phosphorus ore hydrochloric acid circulation
CN101759168B (en) * 2010-01-08 2012-05-30 武汉工程大学 Process for producing potassium phosphate with wet phosphoric acid
CN102320585B (en) * 2011-09-01 2014-07-02 贵阳中化开磷化肥有限公司 Method for direct production of industrial-grade ammonium biphosphate by wet-process phosphoric acid
CN103011122B (en) * 2012-12-28 2014-08-20 金正大生态工程集团股份有限公司 Method for producing water-soluble potassium ammonium phosphate from wet-process phosphoric acid
CN104401953B (en) * 2014-11-21 2017-02-08 贵州开磷集团股份有限公司 Di-ammonium phosphate produced by wet process phosphoric acid and production method of di-ammonium phosphate

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