CN102530899A - Method for preparing high-concentration phosphoric acid by raffinate phosphoric acid - Google Patents
Method for preparing high-concentration phosphoric acid by raffinate phosphoric acid Download PDFInfo
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- CN102530899A CN102530899A CN2012100467626A CN201210046762A CN102530899A CN 102530899 A CN102530899 A CN 102530899A CN 2012100467626 A CN2012100467626 A CN 2012100467626A CN 201210046762 A CN201210046762 A CN 201210046762A CN 102530899 A CN102530899 A CN 102530899A
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Abstract
The invention discloses a method for preparing high-concentration phosphoric acid by raffinate phosphoric acid, comprising the following steps of: taking raffinate phosphoric acid as raw acid, settling and filtering, collecting filtrate, carrying out de-magging and defluorination pretreatment, carrying out reduced pressure concentration, and obtaining phosphoric acid product. The method disclosed by the invention has simple process, unharsh technological conditions and easy control. H3PO4 content of the raw acid is lower and the raw acid contains more impurities, but cost is relatively low; high-concentration phosphoric acid is prepared while product cost is reduced, the product can be taken as fertilizer additive or raw material used for producing high-concentration fertilizer and also can replace orthophosphoric acid and polyphosphoric acid, thus be widely used, and a product with higher additional value can be produced.
Description
Technical field
The present invention relates to a kind of preparation method of high-concentration phosphoric acid; Being specifically related to by product with wet phosphoric acid purifying prepared technical grade, the food grade phosphoric acid gained surplus phosphoric acid that comes together is raw material acid, after pre-treatment, concentrates the method for preparing high-concentration phosphoric acid under certain condition.
Technical background
Phosphoric acid is a kind of very important intermediates in the phosphorous chemical industry industry, is widely used in the industries such as fertilizer, food, medicine.
Name phosphoric acid that thermal phosphoric acid and phosphoric acid by wet process are arranged according to working method in the industry at present.Thermal phosphoric acid is produced as raw material with yellow phosphorus, and product purity is high, and foreign matter content is low; But production cost is high, energy consumption is high, and phosphoric acid by wet process is produced with sour decomposing phosphate rock, has the advantage that energy consumption is low, production cost is low with respect to thermal phosphoric acid; But according to the different purposes of product; The finished product acid impurity is required inequality, generally need use in industry through operations such as removal of impurities, purification, technical process is longer relatively.The progress of Wet-process Phosphoric Acid Production method mainly comes purifying phosphoric acid through the extraction mode with improving; Can obtain technical grade and food grade phosphoric acid; Make phosphoric acid by wet process also can be used for preparing the high added value phosphorus chemical product; Surplus phosphoric acid foreign matter content is high but the by product of gained comes together, and has influenced its further utilization at present.
The surplus phosphoric acid that comes together is compared with fertilizer phosphoric acid, and the by product for preparing technical grade, food grade phosphoric acid gained with the fertilizer phosphoric acid purification serves as that its phosphorus acid content of the surplus phosphorus of collection is lower, and mass percent concentration is 55～65% (with H
3PO
4% meter), wherein impurity fluorine, Mg content are higher, and the fluorine mass percent concentration is 0.3～0.6%, and magnesia amount percentage concentration is 2～3%, and is mobile poor, is difficult for directly concentrating the production high-concentration phosphoric acid, need could prepare high-concentration phosphoric acid after treatment.
This patent is to this present situation; Proposition will be come together after surplus phosphoric acid heavy clear filtration the through certain hour, concentrate the preparation high-concentration phosphoric acid through pre-treatment de-magging, defluorinate, to reach the utilization again of waste material; Product can be used as fertilizer additive or the high concentration fertilizer raw material is produced in conduct; Also can replace ortho-phosphoric acid, polyphosphoric acid and be widely used, produce and have more high value-added product, have favorable economic benefit.
Summary of the invention
The objective of the invention is to invent utilization and go to prepare the method for high-concentration phosphoric acid with the by product of wet phosphoric acid purifying prepared technical grade, the food grade phosphoric acid gained surplus phosphoric acid that comes together.
The present invention is that raw material acid prepares the high-concentration phosphoric acid method with the surplus phosphoric acid that comes together, and its technology is: as raw material, after sedimentation is filtered, carry out pre-treatment de-magging, defluorinate with the surplus phosphoric acid that comes together, concentrating under reduced pressure at a certain temperature then, preparation high-concentration phosphoric acid; Settling time 10～15h, the de-magging agent that the de-magging process adopts a kind of carbon hydrocarbon compound (WF-RNS), sulfonated kerosene, solubilizing agent phosphoric acid that contains sulfonic acid group to form, by volume, de-magging agent: surplus phosphoric acid=2～3 of coming together; At 30 ℃～50 ℃, stirring velocity is de-magging 45-60min under the 200-350rpm condition, adds 0.5～1% zeyssatite defluorinate then, and the defluorinate condition is vacuum tightness 0～0.09MPa, 80 ℃～140 ℃ of temperature, time 1～3h; Concentration process vacuum tightness 0～0.09MPa, 120 ℃～240 ℃ of temperature, concentration time 2～5h.
It is 40% that the de-magging agent accounts for de-magging agent volume(tric)fraction by the carbon hydrocarbon compound (WF-RNS) that contains sulfonic acid group, and it is 55% that sulfonated kerosene accounts for de-magging agent volume(tric)fraction, and solubilizing agent is (with H
3PO
4The % meter) mass percent concentration is 40～43% phosphoric acid, and it is 5% composition that phosphoric acid accounts for de-magging agent volume(tric)fraction.
The present invention adopts the surplus phosphoric acid of collection as raw material acid---the sedimentation filtration---and filtrating---working method of pre-treatment defluorinate, de-magging---concentrating under reduced pressure---product phosphoric acid, the inventive method is simple, and processing condition are not harsh, easily control.Although raw material acid H
3PO
4Content is lower and impurity is more, but cost is low corresponding lower; Let the high-concentration phosphoric acid for preparing, reduced production cost, product can be used as fertilizer additive or as producing the high concentration fertilizer raw material, also can replace ortho-phosphoric acid, polyphosphoric acid and is widely used, and production has more high value-added product.
Embodiment
Embodiment 1
Get agent of 2.0L de-magging and 800g mass percent concentration and be 55.0% (with H
3PO
4% meter) the surplus phosphoric acid of collection is under the 250rpm behind the de-magging 60min at 30 ℃, stirring velocity, adds 4.0g zeyssatite in the phosphoric acid behind de-magging, in vacuum distillation apparatus; The speed of 5 ℃/min is warming up to 120 ℃; Vacuum tightness is 0.065MPa, and underpressure distillation 2h is 150 ℃ with the phosphoric acid solution after the defluorinate in temperature then; Vacuum tightness is to concentrate 3h under the condition of 0.075MPa, and products therefrom reduces to normal temperature after H in the testing product
3PO
4Content 89.5%, fluorine content 0.24%, Mg content 0.89%.
Embodiment 2
Get agent of 1.7L de-magging and 800g mass percent concentration and be 60.0% (with H
3PO
4% meter) the surplus phosphoric acid of collection is under the 200rpm behind the de-magging 45min at 35 ℃, stirring velocity, adds 8.0g zeyssatite in the phosphoric acid behind de-magging, in vacuum distillation apparatus; The speed of 8 ℃/min is warming up to 140 ℃; Vacuum tightness is 0.0MPa, and distillation 3h is 240 ℃ with the phosphoric acid solution after the defluorinate in temperature then; Vacuum tightness is to concentrate 3.5h under the condition of 0.0MPa, and products therefrom reduces to normal temperature after H in the testing product
3PO
4Content 93.12%, fluorine content 0.3%, Mg content 0.93%.
Embodiment 3
Get agent of 1.8L de-magging and 800g mass percent concentration and be 55.0% (with H
3PO
4% meter) the surplus phosphoric acid of collection is under the 200rpm condition behind the de-magging 45min at 40 ℃, stirring velocity, adds 6.5g zeyssatite in the phosphoric acid behind de-magging, in vacuum distillation apparatus; The speed of 4 ℃/min is warming up to 80 ℃; Vacuum tightness is 0.09MPa, and underpressure distillation 1h is 120 ℃ with the phosphoric acid solution after the defluorinate in temperature then; Vacuum tightness is to concentrate 5h under the condition of 0.09MPa, and products therefrom reduces to normal temperature after H in the testing product
3PO
4Content 91.3%, fluorine content 0.26%, Mg content 0.92%.
Embodiment 4
Get agent of 2.2L de-magging and 800g mass percent concentration and be 65.0% (with H
3PO
4% meter) the surplus phosphoric acid of collection is under the 250rpm condition behind the de-magging 60min at 50 ℃, stirring velocity, adds 5.5g zeyssatite in the phosphoric acid behind de-magging, in vacuum distillation apparatus; The speed of 6 ℃/min is warming up to 130 ℃; Vacuum tightness is 0.08MPa, and underpressure distillation 1.5h is 200 ℃ with the phosphoric acid solution after the defluorinate in temperature then; Vacuum tightness is to concentrate 4h under the condition of 0.085MPa, and products therefrom reduces to normal temperature after H in the testing product
3PO
4Content 98.5%, fluorine content 0.21%, Mg content 0.91%.
Claims (2)
1. the surplus Phosphoric Acid Concentration of coming together prepares the method for high-concentration phosphoric acid, it is characterized in that with the surplus phosphoric acid that comes together as raw material, after sedimentation is filtered, carries out pre-treatment de-magging, defluorinate, and concentrating under reduced pressure prepares high-concentration phosphoric acid at a certain temperature then; Settling time
10～15hThe de-magging agent that the de-magging process adopts a kind of carbon hydrocarbon compound WF-RNS, sulfonated kerosene, solubilizing agent phosphoric acid that contains sulfonic acid group to form; By volume, de-magging agent: surplus phosphoric acid=2～3 of coming together are de-magging 45-60min under the 200-350rpm condition at 30 ℃～50 ℃, stirring velocity; Add 0.5～1% zeyssatite defluorinate then, the defluorinate condition is vacuum tightness 0～0.09MPa, 80～140 ℃ of temperature, time 1～3h; Concentration process vacuum tightness 0～0.09MPa, 120～240 ℃ of temperature, concentration time 2～5h.
2. according to the described method for preparing high-concentration phosphoric acid by the surplus Phosphoric Acid Concentration of collection of claim 1; It is characterized in that the de-magging agent that the de-magging process adopts is 40% by the volume(tric)fraction that the carbon hydrocarbon compound WF-RNS that contains sulfonic acid group accounts for the de-magging agent; The volume(tric)fraction that sulfonated kerosene accounts for the de-magging agent is 55%, and solubilizing agent is with H
3PO
4The % meter, mass percent concentration is 40～43% phosphoric acid, phosphoric acid accounts for 5% composition of de-magging agent volume(tric)fraction.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012100467626A CN102530899A (en) | 2012-02-28 | 2012-02-28 | Method for preparing high-concentration phosphoric acid by raffinate phosphoric acid |
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|---|---|---|---|
| CN2012100467626A CN102530899A (en) | 2012-02-28 | 2012-02-28 | Method for preparing high-concentration phosphoric acid by raffinate phosphoric acid |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265003A (en) * | 2013-05-20 | 2013-08-28 | 瓮福（集团）有限责任公司 | Demagging agent for demagging raffinate phosphoric acid |
| CN103849874A (en) * | 2014-03-03 | 2014-06-11 | 瓮福（集团）有限责任公司 | Method of preparing chemical polishing liquid for surface of aluminum alloy by residual phosphoric acid |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704518A (en) * | 2009-12-15 | 2010-05-12 | 瓮福（集团）有限责任公司 | Method for purifying raffinate acid |
-
2012
- 2012-02-28 CN CN2012100467626A patent/CN102530899A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101704518A (en) * | 2009-12-15 | 2010-05-12 | 瓮福（集团）有限责任公司 | Method for purifying raffinate acid |
Non-Patent Citations (1)
| Title |
|---|
| 毛静等: "十二烷基苯磺酸萃取分离磷酸所含镁杂质初步研究", 《四川化工》, vol. 9, no. 1, 31 December 2006 (2006-12-31) * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103265003A (en) * | 2013-05-20 | 2013-08-28 | 瓮福（集团）有限责任公司 | Demagging agent for demagging raffinate phosphoric acid |
| CN103849874A (en) * | 2014-03-03 | 2014-06-11 | 瓮福（集团）有限责任公司 | Method of preparing chemical polishing liquid for surface of aluminum alloy by residual phosphoric acid |
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Application publication date: 20120704 |