CN105174239A - Method for preparing disodium hydrogen phosphate by means of phosphoric acid obtained by wet process - Google Patents
Method for preparing disodium hydrogen phosphate by means of phosphoric acid obtained by wet process Download PDFInfo
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- CN105174239A CN105174239A CN201510606518.4A CN201510606518A CN105174239A CN 105174239 A CN105174239 A CN 105174239A CN 201510606518 A CN201510606518 A CN 201510606518A CN 105174239 A CN105174239 A CN 105174239A
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Abstract
The invention relates to the technical field of preparing sodium phosphates by means of phosphoric acid obtained by a wet process, in particular to a method for preparing disodium hydrogen phosphate by means of phosphoric acid obtained by wet process. According to the method, the content of sulfate radicals in the phosphoric acid obtained by wet process is analyzed, ground phosphate rock is added based on the ratio of sulfate radicals to ground phosphate rock being 1.1-1.2 for mixed reaction for 30-60 min, pH is adjusted by means of ammonia gas or ammonia water, sodium is added to slurry after filtration, vacuum degree is controlled to be 0-0.01 MPa, evaporative crystallization is conducted at the temperature of 85-95 DEG C, so that sulfate radicals, Fe, Al, F, Si and other impurities in the phosphoric acid obtained by wet process are removed remarkably during preparation of disodium hydrogen phosphate, and then the effect of sodions and impurities is reduced, sodion consumption is reduced, and production cost is reduced; crystallization velocity is controlled by controlling vacuum degree, so that crystallization end point is controlled effectively, the defect of poor purity caused by excessive crystallization is avoided, and end point control difficulty during crystallization is reduced.
Description
Technical field
The present invention relates to wet process phosphoric acid for preparing sodium phosphate salt technical field, especially a kind of phosphoric acid by wet process prepares Sodium phosphate dibasic method.
Background technology
Sodium phosphate dibasic is easy-weathering in atmosphere, is positioned in air and loses about 5 crystal water and form seven water things, lose whole crystal water and form anhydride when being heated to 100 DEG C during normal temperature, decomposes and become trisodium phosphate when 250 DEG C.As water-softening chemicals, fabric weighting agent, fireproofing agent, and for glaze, welding agent, medicine, pigment, foodstuffs industry and produce other phosphoric acid salt and be used as industrial water quality treatment agent, printing and dyeing washing composition, quality improver, neutralizing agent, microbiotic nutrient chemical, biochemical treatment agent, Food Quality modifying agent etc.
In prior art, the preparation technology for Sodium phosphate dibasic mainly adopts phosphoric acid and sodium salt to carry out reaction and produces Sodium phosphate dibasic product.And the acquisition pattern of phosphoric acid mainly contains phosphoric acid by wet process and thermal phosphoric acid, because the production cost of thermal phosphoric acid is higher, energy consumption is comparatively large, and then the production of phosphoric acid by wet process obtains promotion and application in a big way.But, phosphoric acid by wet process adopts phosphorus ore and mineral acid to carry out hybrid reaction acquisition, because phosphorus ore is at home mainly low-grade phosphorus ore, and then cause the inferior quality of the phosphoric acid adopting phosphorus ore to prepare, foreign matter content is more, and the composition of impurity comparatively horn of plenty, and then cause the purity adopting phosphoric acid by wet process to prepare Sodium phosphate dibasic to be difficult to ensure, and can with the processing parameter in work preparation technology, crystallization degree, and the purity of phosphoric acid by wet process adopted and the difference of reactions steps, cause the purity of product different; The control of the crystallization velocity in the content of the impurity component especially in phosphoric acid by wet process and the kind of impurity component and crystallisation process, will impact the purity of Sodium phosphate dibasic product, also can make the impurity component effect in sodium ion and phosphoric acid by wet process simultaneously, and then causing the consumption of that element to increase, cost prepared by Sodium phosphate dibasic product is larger.
Based on this, this investigator, in conjunction with long-term production practice, adopts Wet-process Phosphoric Acid Production to provide a kind of new approaches to Sodium phosphate dibasic.
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 Sodium phosphate dibasic method.
Be achieved particular by following technical scheme:
A kind of phosphoric acid by wet process prepares Sodium phosphate dibasic 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) sodium hydroxide is got, sodium hydroxide is joined in slip, the mol ratio controlling the amount of Vanadium Pentoxide in FLAKES in the add-on of sodium hydroxide and phosphoric acid by wet process is 4:1, and after it has fed intake, control vacuum tightness 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 Sodium phosphate dibasic.
Described Sodium phosphate dibasic, its purity is 98.3-98.8%.
Described washing, the washing lotion of generation is back in step (1) and mixes with phosphoric acid by wet process.
Described filter residue sends to composite fertilizer production line; Described mother liquor sends to composite fertilizer production line.
Described evaporative crystallization, the dilute phosphoric acid that the gas produced in this process adopts returns in step (1) and mixes with phosphoric acid by wet process after carrying out absorption process.
Described dilute phosphoric acid, its concentration is 15-35%.
The granular size of above-mentioned ground phosphate rock is 60-130 order.
The content of the Vanadium Pentoxide in FLAKES in above-mentioned ground phosphate rock must not lower than 9%.
Above-mentioned sodium hydroxide is that solid joins in ammonium phosphate salt solution, also can for sodium hydroxide be mixed with liquid after add.
Above-mentioned sodium hydroxide can adopt sodium carbonate to replace, and can also adopt sodium bicarbonate to replace.
Compared with prior art, technique effect of the present invention is embodied in:
By analyzing the sulfate radical content in phosphoric acid by wet process, and be 1:1 ~ 1.2 hybrid reaction 30-60min according to the ratio of sulfate radical and ground phosphate rock wherein, ammonia or ammoniacal liquor regulate pH again, after refiltering, sodium composition is added in slip, control vacuum tightness is 0-0.01MPa, temperature 85-95 DEG C of evaporative crystallization, make in the preparation process of Sodium phosphate dibasic product, sulfate radical in phosphoric acid by wet process, iron, aluminium, fluorine, the impurity such as silicon obtain a large amount of removings, and then reduce the effect of sodium ion and impurity, reduce the consumption of sodium ion, reduce production cost, and by vacuum degree control, crystallization velocity is controlled effectively, and then the terminal of effective crystallization control, avoid the defect that excessive the caused purity of crystallization is poor, also reduce the terminal point control difficulty in crystallization.
The present invention, by the control of above-mentioned processing step and processing parameter, makes the purity preparing Sodium phosphate dibasic product reach 98.3-98.8%.
There is not the discharge of waste liquid, waste gas, waste residue in whole technique of the present invention, and the mother liquor reclaimed and excessively filter residue are used for the production of composite fertilizer, it can meet the indices of composite fertilizer; Also the washings after washing is returned step 1 simultaneously, in conjunction with adopting dilute phosphoric acid to return step 1 to the ammonia absorption evaporated, and then making phosphoric, ammonium radical ion etc. be recycled utilization, reducing resource consumption, reducing the production cost of Sodium phosphate dibasic.
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 Sodium phosphate dibasic 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) sodium hydroxide is got, sodium hydroxide is joined in slip, the mol ratio controlling the amount of Vanadium Pentoxide in FLAKES in the add-on of sodium hydroxide and phosphoric acid by wet process is 4:1, and after it has fed intake, control vacuum tightness 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 Sodium phosphate dibasic.
Described Sodium phosphate dibasic, its purity is 98.3%.
Described washing, the washing lotion of generation is back in step (1) and mixes with phosphoric acid by wet process.
Described filter residue sends to composite fertilizer production line; Described mother liquor sends to composite fertilizer production line.
Described evaporative crystallization, the dilute phosphoric acid that the gas produced in this process adopts returns in step (1) and mixes with phosphoric acid by wet process after carrying out absorption process.
Described dilute phosphoric acid, its concentration is 15%.
The granular size of above-mentioned ground phosphate rock is 60 orders.
The content of the Vanadium Pentoxide in FLAKES in above-mentioned ground phosphate rock must not lower than 9%.
Embodiment 2
A kind of phosphoric acid by wet process prepares Sodium phosphate dibasic 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) sodium hydroxide is got, sodium hydroxide is joined in slip, the mol ratio controlling the amount of Vanadium Pentoxide in FLAKES in the add-on of sodium hydroxide and phosphoric acid by wet process is 4:1, and after it has fed intake, control vacuum tightness 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 Sodium phosphate dibasic.
Described Sodium phosphate dibasic, its purity is 98.8%.
Described washing, the washing lotion of generation is back in step (1) and mixes with phosphoric acid by wet process.
Described filter residue sends to composite fertilizer production line; Described mother liquor sends to composite fertilizer production line.
Described evaporative crystallization, the dilute phosphoric acid that the gas produced in this process adopts returns in step (1) and mixes with phosphoric acid by wet process after carrying out absorption process.
Described dilute phosphoric acid, its concentration is 35%.
The granular size of above-mentioned ground phosphate rock is 130 orders.
The content of the Vanadium Pentoxide in FLAKES in above-mentioned ground phosphate rock must not lower than 13%.
Above-mentioned sodium hydroxide is add after sodium hydroxide is mixed with liquid.
Embodiment 3
A kind of phosphoric acid by wet process prepares Sodium phosphate dibasic 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 4, filter, obtain slip and filter residue;
(2) sodium hydroxide is got, sodium hydroxide is joined in slip, the mol ratio controlling the amount of Vanadium Pentoxide in FLAKES in the add-on of sodium hydroxide and phosphoric acid by wet process is 4:1, and after it has fed intake, control vacuum tightness 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 Sodium phosphate dibasic.
Described Sodium phosphate dibasic, its purity is 98.4%.
Described washing, the washing lotion of generation is back in step (1) and mixes with phosphoric acid by wet process.
Described filter residue sends to composite fertilizer production line; Described mother liquor sends to composite fertilizer production line.
Described evaporative crystallization, the dilute phosphoric acid that the gas produced in this process adopts returns in step (1) and mixes with phosphoric acid by wet process after carrying out absorption process.
Described dilute phosphoric acid, its concentration is 25%.
The granular size of above-mentioned ground phosphate rock is 100 orders.
The content of the Vanadium Pentoxide in FLAKES in above-mentioned ground phosphate rock must not lower than 17%.
Embodiment 4
On the basis of embodiment 1, other steps are all with embodiment 1, and above-mentioned sodium hydroxide adopts sodium bicarbonate to replace.
Embodiment 5
On the basis of embodiment 2, other steps are all with embodiment 2, and above-mentioned sodium hydroxide adopts sodium carbonate to replace, and the addition of sodium carbonate makes Na:P=1:1.
Claims (6)
1. phosphoric acid by wet process prepares a Sodium phosphate dibasic 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) sodium hydroxide is got, sodium hydroxide is joined in slip, the mol ratio controlling the amount of Vanadium Pentoxide in FLAKES in the add-on of sodium hydroxide and phosphoric acid by wet process is 4:1, and after it has fed intake, control vacuum tightness 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 Sodium phosphate dibasic.
2. phosphoric acid by wet process as claimed in claim 1 prepares Sodium phosphate dibasic method, and it is characterized in that, described Sodium phosphate dibasic, its purity is 98.3-98.8%.
3. phosphoric acid by wet process as claimed in claim 1 prepares Sodium phosphate dibasic method, and it is characterized in that, described washing, the washing lotion of generation is back in step (1) and mixes with phosphoric acid by wet process.
4. phosphoric acid by wet process as claimed in claim 1 prepares Sodium phosphate dibasic method, and it is characterized in that, described filter residue sends to composite fertilizer production line; Described mother liquor sends to composite fertilizer production line.
5. phosphoric acid by wet process as claimed in claim 1 prepares Sodium phosphate dibasic method, it is characterized in that, described evaporative crystallization, the dilute phosphoric acid that the gas produced in this process adopts returns in step (1) and mixes with phosphoric acid by wet process after carrying out absorption process.
6. phosphoric acid by wet process as claimed in claim 5 prepares Sodium phosphate dibasic method, and it is characterized in that, described dilute phosphoric acid, its concentration is 15-35%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107804831A (en) * | 2017-12-05 | 2018-03-16 | 瓮福达州化工有限责任公司 | A kind of method for controlling purification of wet process phosphoric acid sodium ions content |
| CN108408706A (en) * | 2018-04-13 | 2018-08-17 | 江苏瑞丰医药有限公司 | A kind of preparation method of food-grade anhydrous disodium hydrogen phosphate |
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| CN1079205A (en) * | 1993-05-13 | 1993-12-08 | 王昌志 | The method of producing trisodium phosphate and ammonium salt by metathesis |
| CN1174812A (en) * | 1996-08-26 | 1998-03-04 | 四川联合大学 | Industrial monoammonium phosphate and productive method for industrial monoammunium phosphate and calcium hydrogen phosphate fodder |
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| CN102963874A (en) * | 2012-11-26 | 2013-03-13 | 四川川恒化工股份有限公司 | Method for producing industrial-grade potassium dihydrogen phosphate (KH2PO4) by wet method purified phosphoric acid and potassium sulfate |
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2015
- 2015-09-22 CN CN201510606518.4A patent/CN105174239B/en not_active Expired - Fee Related
Patent Citations (6)
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| CN1079205A (en) * | 1993-05-13 | 1993-12-08 | 王昌志 | The method of producing trisodium phosphate and ammonium salt by metathesis |
| CN1174812A (en) * | 1996-08-26 | 1998-03-04 | 四川联合大学 | Industrial monoammonium phosphate and productive method for industrial monoammunium phosphate and calcium hydrogen phosphate fodder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107804831A (en) * | 2017-12-05 | 2018-03-16 | 瓮福达州化工有限责任公司 | A kind of method for controlling purification of wet process phosphoric acid sodium ions content |
| CN108408706A (en) * | 2018-04-13 | 2018-08-17 | 江苏瑞丰医药有限公司 | A kind of preparation method of food-grade anhydrous disodium hydrogen phosphate |
| CN108408706B (en) * | 2018-04-13 | 2021-12-24 | 江苏瑞丰医药有限公司 | Preparation method of food-grade anhydrous disodium hydrogen phosphate |
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