CN103879981B - A kind of method utilizing phosphoric acid raffinate to prepare potassium primary phosphate - Google Patents
A kind of method utilizing phosphoric acid raffinate to prepare potassium primary phosphate Download PDFInfo
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- CN103879981B CN103879981B CN201410103271.XA CN201410103271A CN103879981B CN 103879981 B CN103879981 B CN 103879981B CN 201410103271 A CN201410103271 A CN 201410103271A CN 103879981 B CN103879981 B CN 103879981B
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Abstract
The invention discloses a kind of method utilizing phosphoric acid raffinate to prepare potassium primary phosphate, take raffinate as raw material hydrogen peroxide, after gac and water remove organic impurity, PH is regulated to be 6.5 ~ 7.5 with triethylamine, then appropriate saturated potassium chloride solution is added after filtration, concentrated and drying obtains potassium primary phosphate, or after removal organic impurity, with weight content be 45% ~ 50% potassium hydroxide solution the PH of raffinate is adjusted to 6.5 ~ 7.5, with the potassium hydroxide solution that weight content is 45% ~ 50%, the PH of raffinate is adjusted to 8.5 ~ 10.5 again after filtration, filter rear weight content be 80% ~ 85% phosphoric acid solution the PH of raffinate is adjusted to 3.8 ~ 4.1, filter gained filtrate after filtration, concentrated and drying obtains potassium primary phosphate.The present invention adopts phosphoric acid raffinate preparing potassium dihydrogen phosphate, makes the utilization ratio of phosphoric acid raffinate more than 85%, improves the utilization ratio of phosphoric acid raffinate, and obtained potassium primary phosphate purity, about 98%, improves its economic benefit.
Description
Technical field
Embodiments of the present invention relate to chemical field, and more specifically, embodiments of the present invention relate to a kind of method utilizing phosphoric acid raffinate to prepare potassium primary phosphate.
Background technology
The production method of purifying phosphoric acid is with extraction agent phosphoric acid extraction from phosphoric acid by wet process, the evolution phosphoric acid of obtained technical grade and food grade, in production, phosphoric acid remaining after extraction becomes raffinate, in the process that purifying phosphoric acid is produced, impurity a large amount of in phosphoric acid by wet process enters in raffinate, and therefore, phosphoric acid raffinate is except containing P
2o
5outside 40% ~ 50%, also containing plurality of impurities: Mg, Fe, Al and other metal ions, under normal circumstances, the content of each metal ion between 0 ~ 3% not etc., phosphoric acid raffinate also contains the solid particulate of less than 6%, for a long time, the utilization ratio of phosphoric acid raffinate is low, and its recycling is all a technical barrier.
The production method of potassium primary phosphate is a lot, is roughly summarised as neutralisation, extraction process, ion exchange method, double decomposition, direct method, crystallization process and electrolytic process etc.In China, production technique many employings neutralisation, secondly also has organic extraction, double decomposition, ion exchange method.
Neutralisation, be deliver to neutralizer after Pian Zhuan caustic potash flakes or salt of wormwood are made into the solution of 30%, under agitation neutralize with the phosphoric acid solution of 50%, control temperature is at 80-100 DEG C, pH is 4-5, neutralized reaction product after filtration, concentrated, crystallisation by cooling, centrifugation, to get product after drying.Current, the throughput of national neutralisation potassium primary phosphate accounts for more than 90% of overall throughput.This method is with thermal phosphoric acid and potash for raw material, and production cost is high, is difficult to agriculturally applying, mainly for the production of the potassium primary phosphate of food, medicine and technical grade.
It is raw material that Chinese patent (patent No. 201110159163.0) discloses a kind of food grade phosphoric acid; produce the method for potassium primary phosphate; the advantage of the method is that the technical process of production potassium primary phosphate is simple, quality product is high and is convenient to industrial applications; but; the method needs expensive potassium hydroxide and food grade phosphoric acid; production cost is higher, limits large-scale production, and Recycling Mother Solution just abandons the pollution added environment 5 times.
Due to high-quality phosphoric acid shortage and existing method utilizes phosphoric acid raffinate to prepare phosphoric acid hydrogen one ammonium and Secondary ammonium phosphate, quality product is not high, greatly reduces the utilization ratio of raffinate, is badly in need of a kind of method to improve the utilization ratio of raffinate.
Summary of the invention
Instant invention overcomes the deficiencies in the prior art, provide a kind of embodiment utilizing phosphoric acid raffinate to prepare potassium primary phosphate, the method prepares potassium primary phosphate using phosphoric acid raffinate as starting material, improves the utilization ratio of phosphoric acid raffinate.
For solving above-mentioned technical problem, one embodiment of the present invention by the following technical solutions:
Utilize phosphoric acid raffinate to prepare a method for potassium primary phosphate, comprise the steps:
(1) with phosphoric acid raffinate for raw material, add any two kinds of organic impuritys removed in phosphoric acid raffinates in hydrogen peroxide, gac and water;
(2) in step (1) gained phosphoric acid raffinate, add triethylamine regulates the PH of phosphoric acid raffinate to be 6.5 ~ 7.5, filters and obtains filtrate A; Or the potassium hydroxide solution that weight content is 45% ~ 50% is added in step (1) gained phosphoric acid raffinate, the PH regulating phosphoric acid raffinate is 6.5 ~ 7.5, filters and obtains liquor B;
(3) add in filtrate A and add enough water again after enough saturated potassium chloride solutions make its crystallize out crystal is all dissolved, filter and obtain liquor C; Or add in liquor B weight content be 45% ~ 50% potassium hydroxide solution regulate PH be 8.5 ~ 10.5, add in filtrate again after filtration weight content be 80% ~ 85% phosphoric acid solution regulate PH be 3.8 ~ 4.1, filter obtain filtrate D;
(4) liquor C or filtrate D is concentrated, drying obtains solid phosphoric acid potassium dihydrogen.
According to one embodiment of present invention: the organic impurity that step (1) is removed in phosphoric acid raffinate selects hydrogen peroxide and gac, and the ratio of the weight of phosphoric acid raffinate, hydrogen peroxide, gac is 100:(5 ~ 10): (1 ~ 5).
Further technical scheme is: by described hydrogen peroxide, gac adds to after in phosphoric acid raffinate needs standing 2 ~ 3 hours, then filters after adding suitable quantity of water dilution and remove gac and impurity.
According to one embodiment of present invention: the organic impurity that step (1) is removed in phosphoric acid raffinate selects hydrogen peroxide and water, and the ratio of the weight of phosphoric acid raffinate, hydrogen peroxide, water is 100:(5 ~ 10): (30 ~ 50).
Further technical scheme is: by described hydrogen peroxide, water adds to after in phosphoric acid raffinate needs heated and stirred, stops heating after making phosphoric acid raffinate temperature rise to 60 ~ 90 DEG C.
According to one embodiment of present invention: the organic impurity that step (1) is removed in phosphoric acid raffinate selects gac and water, and the ratio of the weight of phosphoric acid raffinate, gac, water is 100:(1 ~ 5): (30 ~ 50).
Further technical scheme is: described water, gac added to after in phosphoric acid raffinate and need to filter after standing 2 ~ 3 hours to remove gac and impurity.
Compared with prior art, one of beneficial effect of the present invention is: the present invention adopts phosphoric acid raffinate preparing potassium dihydrogen phosphate, makes the utilization ratio of phosphoric acid raffinate more than 85%, substantially increase the utilization ratio of phosphoric acid raffinate, this is simple for process, without the need to great amount of investment, technical process is short, productive expense is low, without contaminated wastewater, without the need to washing, water loss is few, can realize cleaner production, obtained potassium primary phosphate purity, about 98%, substantially increases its economic benefit.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The present invention can by adding different materials to phosphoric acid raffinate and phosphatase reaction regulates pH value to 6.5 ~ 7.5, and described different material comprises triethylamine and weight content is the potassium hydroxide solution of 45% ~ 50%.According to the difference of the material added in this step, the processing mode of its gained filtrate is also different.
Mode one, interpolation triethylamine regulate phosphoric acid raffinate PH to be that 6.5 ~ 7.5 rear filtrations obtain filtrate, then in filtrate, add enough saturated potassium chloride solutions make its crystallize out, and then add enough water crystal is all dissolved, filtration obtains filtrate, and filtrate concentrate drying is obtained solid phosphoric acid potassium dihydrogen;
The potassium hydroxide solution of mode two, interpolation 45% ~ 50% regulates the PH of phosphoric acid raffinate to be that 6.5 ~ 7.5 rear filtrations obtain filtrate, and then regulate the PH of phosphoric acid raffinate to be 8.5 ~ 10.5 with the potassium hydroxide solution of 45% ~ 50%, PH is regulated to be 3.8 ~ 4.1 with the phosphoric acid solution that weight content is 80% ~ 85% again after filtration, filtration obtains filtrate, and filtrate concentrate drying is obtained solid phosphoric acid potassium dihydrogen.Adopting two sections of potassium hydroxide solutions to regulate PH once to filter because with the addition of between its two sections in the manner, is that impurity-eliminating effect is better.
Embodiment 1 ~ 4 is the embodiment of mode one, and embodiment 5 ~ 10 is the embodiment of mode two.
Embodiment 1
With 500kg phosphoric acid raffinate for raw material, 45kg hydrogen peroxide and 220kg water is added to it, heated and stirred, temperature is made to rise to 90 DEG C, stop heating, starting slowly to add 306kg triethylamine regulates the PH of phosphoric acid raffinate to be 7, and filter and obtain filter residue and filtrate, hydrogen peroxide can remove the organic impurity in phosphoric acid raffinate.The recyclable triethylamine of potassium hydroxide is added in filter residue, the rate of recovery of triethylamine reaches 92%, 156kg saturated potassium chloride solution is added in filtrate, make filtrate crystallize out, and then add 150kg water to it crystal of precipitation is dissolved completely, then filter, filtrate is concentrated, drying obtains finished product potassium primary phosphate 331.5kg, its productive rate is 87%, and the content of potassium primary phosphate is 98.7%.There is chemical reaction in the saturated potassium chloride solution used in the present embodiment and filtrate, the amount of saturated potassium chloride solution can make filtrate crystallize out as much as possible, the 156kg saturated potassium chloride solution that the present embodiment uses enough makes filtrate crystallize out, residual solution after too much interpolation saturated potassium chloride solution only can make filtrate reacted increases Repone K, crystal is separated out and there is no useful effect, add very few saturated potassium chloride solution, crystal can not be made all to separate out, therefore, enough saturated potassium chloride solutions that crystal in filtrate is all separated out are added.
Embodiment 2
With 500kg phosphoric acid raffinate for raw material, 35kg hydrogen peroxide and 15kg gac is added to it, leave standstill 2 hours, filter after adding the dilution of 200kg water, in filtrate, drip 350kg triethylamine regulates the PH of phosphoric acid raffinate to be 7.5, filtration obtains filter residue and filtrate, and hydrogen peroxide can remove the organic impurity in phosphoric acid raffinate.The recyclable triethylamine of potassium hydroxide is added in filter residue, the rate of recovery of triethylamine reaches 92%, 175kg saturated potassium chloride solution is added in filtrate, make filtrate crystallize out, and then add 150kg water to it crystal of precipitation is dissolved completely, and then filter, filtrate is concentrated, drying obtains finished product potassium primary phosphate 339kg, its productive rate is 88.9%, and the content of potassium primary phosphate is 98.8%.
Embodiment 3
With 500kg phosphoric acid raffinate for raw material, 50kg hydrogen peroxide and 250kg water is added to it, heated and stirred, temperature is made to rise to 60 DEG C, stop heating, starting slowly to add 310kg triethylamine regulates the PH of phosphoric acid raffinate to be 6.5, and filter and obtain filter residue and filtrate, hydrogen peroxide can remove the organic impurity in phosphoric acid raffinate.The recyclable triethylamine of potassium hydroxide is added in filter residue, the rate of recovery of triethylamine reaches 91%, 160kg saturated potassium chloride solution is added in filtrate, make filtrate crystallize out, and then add 150kg water to it crystal of precipitation is dissolved completely, and then filter, filtrate is concentrated, drying obtains finished product potassium primary phosphate 330kg, its productive rate is 87%, and the content of potassium primary phosphate is 97.7%.
Embodiment 4
With 500kg phosphoric acid raffinate for raw material, add 5kg gac and 150kg water wherein, leave standstill 3 hours, filter, subsequent process steps is identical with embodiment 2.
Except above-described embodiment, when the organic impurity removed in phosphoric acid raffinate selects hydrogen peroxide and gac, as long as the ratio of the weight of phosphoric acid raffinate, hydrogen peroxide, gac meets 100:(5 ~ 10): (1 ~ 5), time of repose can be 2 ~ 3 hours; The organic impurity removed in phosphoric acid raffinate selects hydrogen peroxide and water, as long as the ratio of the weight of phosphoric acid raffinate, hydrogen peroxide, water meets 100:(5 ~ 10): (30 ~ 50), can make temperature rise to 60 ~ 90 DEG C during heating; The organic impurity removed in phosphoric acid raffinate selects gac and water, as long as the ratio of the weight of phosphoric acid raffinate, gac, water meets 100:(1 ~ 5): (30 ~ 50); Time of repose can be 2 ~ 3 hours.
Embodiment 5
With 500kg phosphoric acid raffinate for raw material, add 45kg hydrogen peroxide and 5kg gac wherein, leave standstill 2 hours, filter after adding the dilution of 150kg water, hydrogen peroxide and gac can remove the organic impurity in phosphoric acid raffinate, after dilute with water, are more convenient for filtering, the amount of diluting the water used, without strict demand, only needs to add appropriate water and phosphoric acid raffinate is filtered more easily.The potassium hydroxide solution that 697kg weight content is 48% is added in filtrate, PH is regulated to be 10 rear filtrations, the phosphoric acid that 292kg weight content is 85% is added in filtrate, PH is regulated to be 3.8, then solid phosphoric acid potassium dihydrogen 671.7kg is obtained through concentrated, drying, its productive rate is 86%, and the content of potassium primary phosphate is 97.6%.
Embodiment 6
With 500kg phosphoric acid raffinate for raw material, add 5kg gac and 150kg water wherein, leave standstill 2.5 hours, filter, the potassium hydroxide solution that 391kg weight content is 48% is added in filtrate, PH is regulated to be 7, in filtrate, the potassium hydroxide solution that 205kg weight content is 48% is added again after filtration, PH is regulated to be 10 rear filtrations, in filtrate, add the phosphoric acid that 205kg weight content is 85%, regulate PH to be 3.8, then obtain solid phosphoric acid potassium dihydrogen 575.4kg through concentrated, drying, its productive rate is 89.9%, and the content of potassium primary phosphate is 98.4%.
Embodiment 7
With 500kg phosphoric acid raffinate for raw material, add 25kg hydrogen peroxide and 25kg gac wherein, leave standstill 3 hours, filter, the potassium hydroxide solution that 385kg weight content is 50% is added in filtrate, PH is regulated to be 7.5, in filtrate, the potassium hydroxide solution that 200kg weight content is 50% is added again after filtration, PH is regulated to be 10.5 rear filtrations, in filtrate, add the phosphoric acid that 201kg weight content is 85%, regulate PH to be 4.1, then obtain solid phosphoric acid potassium dihydrogen 569.8kg through concentrated, drying, its productive rate is 89.1%, and the content of potassium primary phosphate is 98.45%.
Embodiment 8
With 500kg phosphoric acid raffinate for raw material, add 50kg hydrogen peroxide and 250kg water wherein, heated and stirred, temperature is made to rise to 60 DEG C, stop heating, the potassium hydroxide solution that 405kg weight content is 45% is added in filtrate, PH is regulated to be 6.5, in filtrate, the potassium hydroxide solution that 200kg weight content is 45% is added again after filtration, PH is regulated to be 8.5 rear filtrations, the phosphoric acid that 220kg weight content is 80% is added in filtrate, PH is regulated to be 4.1, then through concentrated, drying obtains solid phosphoric acid potassium dihydrogen 550kg, its productive rate is 88.1%, the content of potassium primary phosphate is 97.84%.
Embodiment 9
With 500kg phosphoric acid raffinate for raw material, add 25kg hydrogen peroxide and 150kg water wherein, heated and stirred, make temperature rise to 90 DEG C, stop heating, subsequent process steps is identical with embodiment 8.
Embodiment 10
With 500kg phosphoric acid raffinate for raw material, add 25kg gac and 250kg water wherein, leave standstill 3 hours, filter, subsequent step is identical with embodiment 6.
Mode two uses hydrogen peroxide, gac identical with consumption with the method for mode one with consumption with any two kinds of methods removing the organic impurity in phosphoric acid raffinate in water, therefore, the method for the organic impurity in any two kinds of removal phosphoric acid raffinates in hydrogen peroxide, gac and water and consumption is used all can to apply in the embodiment of mode one in mode two.
Although with reference to multiple explanatory embodiment of the present invention, invention has been described here, but, should be appreciated that, those skilled in the art can design a lot of other amendment and embodiment, these amendments and embodiment will drop within spirit disclosed in the present application and spirit.More particularly, in the scope of and claim open in the application, multiple modification and improvement can be carried out to the building block of subject combination layout and/or layout.Except the modification of carrying out building block and/or layout is with except improvement, to those skilled in the art, other purposes also will be obvious.
Claims (4)
1. utilize phosphoric acid raffinate to prepare a method for potassium primary phosphate, it is characterized in that, comprise the steps:
(1) with phosphoric acid raffinate for raw material, add any two kinds of organic impuritys removed in phosphoric acid raffinates in hydrogen peroxide, gac and water; When selecting hydrogen peroxide and gac to remove the organic impurity in phosphoric acid raffinate, the ratio of the weight of phosphoric acid raffinate, hydrogen peroxide, gac is 100:(5 ~ 10): (1 ~ 5); When selecting hydrogen peroxide and water to remove the organic impurity in phosphoric acid raffinate, the ratio of the weight of phosphoric acid raffinate, hydrogen peroxide, water is 100:(5 ~ 10): (30 ~ 50); When selecting gac and water to remove the organic impurity in phosphoric acid raffinate, the ratio of the weight of phosphoric acid raffinate, gac, water is 100:(1 ~ 5): (30 ~ 50);
(2) in step (1) gained phosphoric acid raffinate, add triethylamine regulates the pH of phosphoric acid raffinate to be 6.5 ~ 7.5, filters and obtains filtrate A;
(3) add in filtrate A and add enough water again after enough saturated potassium chloride solutions make its crystallize out crystal is all dissolved, filter and obtain liquor C;
(4) liquor C is concentrated, drying obtains solid phosphoric acid potassium dihydrogen.
2. the method utilizing phosphoric acid raffinate to prepare potassium primary phosphate according to claim 1, it is characterized in that: by described hydrogen peroxide, gac adds to after in phosphoric acid raffinate needs standing 2 ~ 3 hours, then filter after adding suitable quantity of water dilution and remove gac and impurity.
3. the method utilizing phosphoric acid raffinate to prepare potassium primary phosphate according to claim 1, is characterized in that: by described hydrogen peroxide, water adds to after in phosphoric acid raffinate needs heated and stirred, stops heating after making phosphoric acid raffinate temperature rise to 60 ~ 90 DEG C.
4. the method utilizing phosphoric acid raffinate to prepare potassium primary phosphate according to claim 1, is characterized in that: described water, gac added to after in phosphoric acid raffinate and need to filter after standing 2 ~ 3 hours to remove gac and impurity.
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| CN105967417A (en) * | 2016-05-19 | 2016-09-28 | 浙江永泉化学有限公司 | Treatment method of phosphorus-containing wastewater |
| CN106082153B (en) * | 2016-08-23 | 2018-04-20 | 湖北中孚化工集团有限公司 | Utilize the method and device for extracting tail washings synthesis potassium dihydrogen phosphate |
| CN106586990B (en) * | 2016-11-09 | 2019-03-19 | 长江师范学院 | With the method for Wet-process Phosphoric Acid Production potassium dihydrogen phosphate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1324760A (en) * | 2001-02-28 | 2001-12-05 | 四川龙蟒集团有限责任公司 | Production process of potassium dihydrogen phosphate |
| CN102285649A (en) * | 2011-06-15 | 2011-12-21 | 安徽恒星制药有限公司 | Method for preparing monopotassium phosphate |
| CN102602904A (en) * | 2012-04-16 | 2012-07-25 | 瓮福（集团）有限责任公司 | Method for producing monoammonium phosphate from raffinate acid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1324760A (en) * | 2001-02-28 | 2001-12-05 | 四川龙蟒集团有限责任公司 | Production process of potassium dihydrogen phosphate |
| CN102285649A (en) * | 2011-06-15 | 2011-12-21 | 安徽恒星制药有限公司 | Method for preparing monopotassium phosphate |
| CN102602904A (en) * | 2012-04-16 | 2012-07-25 | 瓮福（集团）有限责任公司 | Method for producing monoammonium phosphate from raffinate acid |
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