CN105217591A - 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 PDFInfo
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- CN105217591A CN105217591A CN201510606956.0A CN201510606956A CN105217591A CN 105217591 A CN105217591 A CN 105217591A CN 201510606956 A CN201510606956 A CN 201510606956A CN 105217591 A CN105217591 A CN 105217591A
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Abstract
The present invention relates to phosphoric acid by wet process and prepare Tripotassium phosphate technical field, especially a kind of phosphoric acid by wet process prepares Tripotassium phosphate method, by analyzing the content of the sulfate radical in phosphoric acid by wet process, adding again in conjunction with ground phosphate rock, make sulfate radical, iron, the positively charged ions such as aluminium and fluorine, the negatively charged ion such as silicon form precipitation, pass into ammonia more wherein or add ammoniacal liquor, adjust ph is after 3-7, it is made to form ammonium phosphate salt solution, again through filtering, the precipitation formed is made to be filtered in slag liquid, phosphoric acid by wet process is purified, ensure that the purity of the Tripotassium phosphate product of subsequent production, after reacting in conjunction with ammonium phosphate salt slip and potassium hydroxide or saleratus, salt of wormwood again, again it is carried out evaporative crystallization under negative pressure pressure is 0 ~ 0.01MPa, and then make the crystal mass of Tripotassium phosphate product more excellent, purity is higher, and reduce the consumption of potassium ion, reduce Tripotassium phosphate production cost, avoid the waste of resource.
Description
Technical field
The present invention relates to phosphoric acid by wet process and prepare Tripotassium phosphate technical field, especially a kind of phosphoric acid by wet process prepares Tripotassium phosphate method.
Background technology
Tripotassium phosphate, it is applied to multi-field, as agricultural etc.; Its production method mainly neutralisation adopted at present, namely adopts phosphoric acid and potassium hydroxide or saleratus, after salt of wormwood reacts, by the control of reaction end, again neutralizer is carried out concentrated after, removing insolubles, and then cooled post crystallization, centrifugation is dry, obtained product.But, because phosphoric acid is divided into thermal phosphoric acid and phosphoric acid by wet process, the principle that phosphoric acid by wet process mainly utilizes phosphorus ore and mineral acid to produce weak acid according to strong acid is carried out, even if employing mineral acid, as sulfuric acid to leach phosphoric wherein, make sulfate radical and other elements, after calcium constituent formation calcium sulfate insolubles, filtration obtains, , because the quality of phosphorus ore will impact the quality of phosphoric acid by wet process, the quality of phosphoric acid product prepared by phosphoric acid by wet process is unstable, simultaneously, also make the foreign matter content in the phosphoric acid obtained higher, purity is lower, make when the phosphoric acid using phosphoric acid by wet process to prepare is to produce phosphoric acid potassium salt product, it not only can make the purity of potassium phosphate salt lower, quality is unstable, also can make to cause in preparation process the potassium hydroxide or salt of wormwood that add simultaneously, potassium ion in saleratus and other impurity element effects form insolubles, and then cause the waste of potassium ion, cause potassium hydroxide, the add-on of salt of wormwood or saleratus increases, and then cause preparation cost higher, resource consumption is larger.
Based on this, this investigator, for above-mentioned defect, the basis of existing Tripotassium phosphate preparation technology is studied, and then provides a kind of new approaches for Tripotassium phosphate preparing technical field.
Summary of the invention
In order to solve the above-mentioned technical problem existed in prior art, the invention provides a kind of phosphoric acid by wet process and preparing Tripotassium phosphate method.
Be 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 Vanadium Pentoxide in FLAKES concentration is 15-35% is got, by analyzing the content of sulfate radical wherein, and add ground phosphate rock wherein, the add-on of ground phosphate rock is be (1 ~ 1.2) with the mass ratio of the content of sulfate radical: 1, after its reaction 30-60min, then add ammoniacal liquor wherein or pass into ammonia, adjust ph is 3 ~ 7, filter, obtain slip and filter residue;
(2) potassium hydroxide is got, potassium hydroxide is joined in slip, the mol ratio controlling the amount of Vanadium Pentoxide in FLAKES in add-on and the phosphoric acid by wet process of potassium hydroxide is 6:1, and after it has fed intake, control negative pressure pressure is 0-0.01MPa, temperature is adopted to be 85-95 DEG C of evaporative crystallization, treat in solution, to occur a large amount of crystal, stop evaporation, cool to room temperature, filter, obtain 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, the washings that its washing produces returns in step 1 and mixes with phosphoric acid by wet process.
Described evaporative crystallization, the gas produced in crystallisation process returns and mixes with the phosphoric acid by wet process in step 1 after adopting dilute phosphoric acid to absorb.
Described dilute phosphoric acid, 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 joins in slip.
Described potassium hydroxide, it joins in slip after potassium hydroxide is mixed with solution.
Described potassium hydroxide adopts saleratus or salt of wormwood to replace, and when adopting salt of wormwood to replace, in itself and phosphoric acid by wet process, the mol ratio of the amount of Vanadium Pentoxide in FLAKES is 3.8 ~ 4:1; Adopt salt of wormwood when replacing, in itself and phosphoric acid by wet process, the mol ratio of the amount of Vanadium Pentoxide in FLAKES is 6:1.
Described ground phosphate rock, the content of its Vanadium Pentoxide in FLAKES is for being not less than 7%.
Described ground phosphate rock, its granularity is 40-140 order.
Compared with prior art, technique effect of the present invention is embodied in:
By being decided to be 15-35% to phosphoric acid by wet process in the concentration limits of Vanadium Pentoxide in FLAKES, again the content of the sulfate radical in phosphoric acid by wet process is analyzed, adding again in conjunction with ground phosphate rock, the positively charged ions such as sulfate radical, iron, aluminium and the negatively charged ion such as fluorine, silicon is made to form precipitation, pass into ammonia more wherein or add ammoniacal liquor, adjust ph is after 3-7, it is made to form ammonium phosphate salt solution, again through filtering, the precipitation formed is made to be filtered in slag liquid, phosphoric acid by wet process is purified, ensure that the purity of the Tripotassium phosphate product of subsequent production; After reacting in conjunction with ammonium phosphate salt slip and potassium hydroxide or saleratus, salt of wormwood again, again it is carried out evaporative crystallization under negative pressure pressure is 0 ~ 0.01MPa, and then make the crystal mass of Tripotassium phosphate product more excellent, purity is higher, and reduce the consumption of potassium ion, reduce Tripotassium phosphate production cost, avoid the waste of resource.
The present invention is especially through the accurate control of negative pressure pressure, and then make the control of negative pressure pressure, the degree of supersaturation of solution is controlled, further prepare to phosphoric acid by wet process the speed that Tripotassium phosphate crystal separates out to control, and then locate the amount of precipitation of Tripotassium phosphate accurately, guarantee the purity of Tripotassium phosphate product, make the purity of Tripotassium phosphate product reach 98.1 ~ 99.31%.
Mother liquor after crystallization is also sent to composite fertilizer production line by the present invention, and then the quantity discharged of waste liquid is reduced, resource is fully utilized, carry out absorption in conjunction with dilute phosphoric acid to the gas produced in evaporation and crystal process again to reclaim, and sent in step 1 and mix with phosphoric acid by wet process, and then reach the object reclaiming ammonium radical ion, reduce quantity discharged and the consumed resource of waste gas, reduce production cost.
Embodiment
Below in conjunction with concrete embodiment, further restriction is done to technical scheme of the present invention, but claimed scope is not only confined to done 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 Vanadium Pentoxide in FLAKES concentration is 15% is got, by analyzing the content of sulfate radical wherein, and add ground phosphate rock wherein, the add-on of ground phosphate rock is be 1:1 with the mass ratio of the content of sulfate radical, after its reaction 30min, then add ammoniacal liquor wherein or pass into ammonia, adjust ph is 3, filter, obtain slip and filter residue;
(2) potassium hydroxide is got, potassium hydroxide is joined in slip, the mol ratio controlling the amount of Vanadium Pentoxide in FLAKES in add-on and the phosphoric acid by wet process of potassium hydroxide is 6:1, and after it has fed intake, control negative pressure pressure is 0MPa, temperature is adopted to be 85 DEG C of evaporative crystallizations, treat in solution, to occur a large amount of crystal, stop evaporation, cool to room temperature, filter, obtain mother liquor and first finished product; First finished product washing, obtains Tripotassium phosphate.
Described Tripotassium phosphate, its purity is 98.1%.
Described washing, the washings that its washing produces returns in step 1 and mixes with phosphoric acid by wet process.
Described evaporative crystallization, the gas produced in crystallisation process returns and mixes with the phosphoric acid by wet process in step 1 after adopting dilute phosphoric acid to absorb.
Described dilute phosphoric acid, 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 joins in slip.
Described ground phosphate rock, the content of its Vanadium Pentoxide in FLAKES is for being not less than 7%.
Described ground phosphate rock, its granularity is 40 orders.
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 Vanadium Pentoxide in FLAKES concentration is 35% is got, by analyzing the content of sulfate radical wherein, and add ground phosphate rock wherein, the add-on of ground phosphate rock is be 1.2:1 with the mass ratio of the content of sulfate radical, after its reaction 60min, then add ammoniacal liquor wherein or pass into ammonia, adjust ph is 7, filter, obtain slip and filter residue;
(2) potassium hydroxide is got, potassium hydroxide is joined in slip, the mol ratio controlling the amount of Vanadium Pentoxide in FLAKES in add-on and the phosphoric acid by wet process of potassium hydroxide is 6:1, and after it has fed intake, control negative pressure pressure is 0.01MPa, temperature is adopted to be 95 DEG C of evaporative crystallizations, treat in solution, to occur a large amount of crystal, stop evaporation, cool to room temperature, filter, obtain mother liquor and first finished product; First finished product washing, obtains Tripotassium phosphate.
Described Tripotassium phosphate, its purity is 99.31%.
Described washing, the washings that its washing produces returns in step 1 and mixes with phosphoric acid by wet process.
Described evaporative crystallization, the gas produced in crystallisation process returns and mixes with the phosphoric acid by wet process in step 1 after adopting dilute phosphoric acid to absorb.
Described dilute phosphoric acid, 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 joins in slip after potassium hydroxide is mixed with solution.
Described ground phosphate rock, the content of its Vanadium Pentoxide in FLAKES is for being not less than 10%.
Described ground phosphate rock, its granularity is 140 orders.
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 Vanadium Pentoxide in FLAKES concentration is 20% is got, by analyzing the content of sulfate radical wherein, and add ground phosphate rock wherein, the add-on of ground phosphate rock is be 1.1:1 with the mass ratio of the content of sulfate radical, after its reaction 40min, then add ammoniacal liquor wherein or pass into ammonia, adjust ph is 5, filter, obtain slip and filter residue;
(2) potassium hydroxide is got, potassium hydroxide is joined in slip, the mol ratio controlling the amount of Vanadium Pentoxide in FLAKES in add-on and the phosphoric acid by wet process of potassium hydroxide is 6:1, and after it has fed intake, control negative pressure pressure is 0.005MPa, temperature is adopted to be 90 DEG C of evaporative crystallizations, treat in solution, to occur a large amount of crystal, stop evaporation, cool to room temperature, filter, obtain mother liquor and first finished product; First finished product washing, obtains Tripotassium phosphate.
Described Tripotassium phosphate, its purity is 98.7%.
Described washing, the washings that its washing produces returns in step 1 and mixes with phosphoric acid by wet process.
Described evaporative crystallization, the gas produced in crystallisation process returns and mixes with the phosphoric acid by wet process in step 1 after adopting dilute phosphoric acid to absorb.
Described dilute phosphoric acid, 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 Vanadium Pentoxide in FLAKES is for being not less than 16%.
Described ground phosphate rock, its granularity is 100 orders.
Embodiment 4
On the basis of embodiment 1, other are all with embodiment 1, and described potassium hydroxide adopts salt of wormwood to replace, and in itself and phosphoric acid by wet process, the mol ratio of the amount of Vanadium Pentoxide in FLAKES is 3.8:1.
Embodiment 5
On the basis of embodiment 2, other are all with embodiment 2, and described potassium hydroxide adopts salt of wormwood to replace, and in itself and phosphoric acid by wet process, the mol ratio of the amount of Vanadium Pentoxide in FLAKES is 4:1.
Embodiment 6
On the basis of embodiment 3, other are all with embodiment 3, and described potassium hydroxide adopts salt of wormwood to replace, and in itself and phosphoric acid by wet process, the mol ratio of the amount of Vanadium Pentoxide in FLAKES is 6:1.
Embodiment 7
On the basis of embodiment 3, other are all with embodiment 3, and described potassium hydroxide adopts salt of wormwood to replace, and in itself and phosphoric acid by wet process, the mol ratio of the amount of Vanadium Pentoxide in FLAKES is 3.9:1.
Claims (10)
1. phosphoric acid by wet process prepares a Tripotassium phosphate method, it is characterized in that, comprises the following steps:
(1) phosphoric acid by wet process that Vanadium Pentoxide in FLAKES concentration is 15-35% is got, by analyzing the content of sulfate radical wherein, and add ground phosphate rock wherein, the add-on of ground phosphate rock is be (1 ~ 1.2) with the mass ratio of the content of sulfate radical: 1, after its reaction 30-60min, then add ammoniacal liquor wherein or pass into ammonia, adjust ph is 3 ~ 7, filter, obtain slip and filter residue;
(2) potassium hydroxide is got, potassium hydroxide is joined in slip, the mol ratio controlling the amount of Vanadium Pentoxide in FLAKES in add-on and the phosphoric acid by wet process of potassium hydroxide is 6:1, and after it has fed intake, control negative pressure pressure is 0-0.01MPa, temperature is adopted to be 85-95 DEG C of evaporative crystallization, treat in solution, to occur a large amount of crystal, stop evaporation, cool to room temperature, filter, obtain mother liquor and first finished product; First finished product washing, obtains Tripotassium phosphate.
2. phosphoric acid by wet process as claimed in claim 1 prepares Tripotassium phosphate method, and it is characterized 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 characterized in that, described washing, and the washings that its washing produces returns in step 1 and mixes with phosphoric acid by wet process.
4. phosphoric acid by wet process as claimed in claim 1 prepares Tripotassium phosphate method, it is characterized in that, described evaporative crystallization, and the gas produced in crystallisation process returns and mixes with the phosphoric acid by wet process in step 1 after adopting dilute phosphoric acid to absorb.
5. phosphoric acid by wet process as claimed in claim 4 prepares Tripotassium phosphate method, and it is characterized in that, described dilute phosphoric acid, its concentration is 15-35%.
6. phosphoric acid by wet process as claimed in claim 1 prepares Tripotassium phosphate method, and it is characterized in that, described mother liquor sends to composite fertilizer 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, and it is characterized in that, described potassium hydroxide, it is that solid joins in slip.
8. phosphoric acid by wet process as claimed in claim 1 prepares Tripotassium phosphate method, and it is characterized in that, described potassium hydroxide, it joins in slip after potassium hydroxide is mixed with solution.
9. phosphoric acid by wet process as claimed in claim 1 prepares Tripotassium phosphate method, it is characterized in that, described potassium hydroxide adopts saleratus or salt of wormwood to replace, and when adopting salt of wormwood to replace, in itself and phosphoric acid by wet process, the mol ratio of the amount of Vanadium Pentoxide in FLAKES is 3.8 ~ 4:1; Adopt salt of wormwood when replacing, in itself and phosphoric acid by wet process, the mol ratio of the amount of Vanadium Pentoxide in FLAKES is 6:1.
10. phosphoric acid by wet process as claimed in claim 1 prepares Tripotassium phosphate method, and it is characterized in that, described ground phosphate rock, the content of its Vanadium Pentoxide in FLAKES is for being not less than 7%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112390238A (en) * | 2019-08-15 | 2021-02-23 | 四川磷天化化工科技有限公司 | Production method of polyphosphoric acid trihydrotripotassium |
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| JPS627614A (en) * | 1985-07-03 | 1987-01-14 | Mitsui Toatsu Chem Inc | Condensing method for wet process phosphoric acid liquid |
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| CN104401953A (en) * | 2014-11-21 | 2015-03-11 | 贵阳中化开磷化肥有限公司 | Di-ammonium phosphate produced by wet process phosphoric acid and production method of di-ammonium phosphate |
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2015
- 2015-09-22 CN CN201510606956.0A patent/CN105217591B/en not_active Expired - Fee Related
Patent Citations (8)
| 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 |
| CN101759168A (en) * | 2010-01-08 | 2010-06-30 | 武汉工程大学 | Process for producing potassium phosphate with wet phosphoric acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112390238A (en) * | 2019-08-15 | 2021-02-23 | 四川磷天化化工科技有限公司 | Production method of polyphosphoric acid trihydrotripotassium |
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