CN103879981A - Method for preparing potassium dihydrogen phosphate by using extraction residual acid of phosphoric acid - Google Patents
Method for preparing potassium dihydrogen phosphate by using extraction residual acid of phosphoric acid Download PDFInfo
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- CN103879981A CN103879981A CN201410103271.XA CN201410103271A CN103879981A CN 103879981 A CN103879981 A CN 103879981A CN 201410103271 A CN201410103271 A CN 201410103271A CN 103879981 A CN103879981 A CN 103879981A
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- Prior art keywords
- phosphoric acid
- acid raffinate
- raffinate
- water
- gac
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 216
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 108
- 238000000034 method Methods 0.000 title claims abstract description 36
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000000605 extraction Methods 0.000 title abstract description 14
- 229910000402 monopotassium phosphate Inorganic materials 0.000 title abstract description 7
- 235000019796 monopotassium phosphate Nutrition 0.000 title abstract description 7
- 239000002253 acid Substances 0.000 title abstract 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000000706 filtrate Substances 0.000 claims abstract description 48
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 42
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 35
- 238000001914 filtration Methods 0.000 claims abstract description 23
- 239000012535 impurity Substances 0.000 claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 21
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 229910019142 PO4 Inorganic materials 0.000 claims description 28
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 28
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 28
- 239000010452 phosphate Substances 0.000 claims description 28
- 229910052700 potassium Inorganic materials 0.000 claims description 28
- 239000011591 potassium Substances 0.000 claims description 28
- 230000001105 regulatory effect Effects 0.000 claims description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 9
- 239000013078 crystal Substances 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000010790 dilution Methods 0.000 claims description 5
- 239000012895 dilution Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 2
- 239000001103 potassium chloride Substances 0.000 abstract 1
- 235000011164 potassium chloride Nutrition 0.000 abstract 1
- 239000012047 saturated solution Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 9
- 230000008569 process Effects 0.000 description 8
- 235000011118 potassium hydroxide Nutrition 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000006386 neutralization reaction Methods 0.000 description 5
- 235000013305 food Nutrition 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 235000015320 potassium carbonate Nutrition 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- -1 without washing Substances 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 102000004160 Phosphoric Monoester Hydrolases Human genes 0.000 description 1
- 108090000608 Phosphoric Monoester Hydrolases Proteins 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 229940072033 potash Drugs 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Abstract
The invention discloses a method for preparing potassium dihydrogen phosphate by using extraction residual acid of phosphoric acid. The method comprises the steps of taking extraction residual acid as a raw material, removing organic impurities by using hydrogen peroxide, activated carbon and water, then adjusting the PH value to be 6.5-7.5 by using triethylamine, adding a proper amount of a potassium chloride saturated solution, filtering, concentrating and drying to obtain potassium dihydrogen phosphate; or, after removing the organic impurities, adjusting the PH value of the extraction residual acid to be 6.5-7.5 by using a potassium hydroxide solution of which the weight content is 45-50%, filtering, then adjusting the PH value of the extraction residual acid to be 8.5-10.5 by using the potassium hydroxide solution of which the weight content is 45-50%, filtering, then adjusting the PH value of the extraction residual acid to be 3.8-4.1 by using a phosphoric acid solution of which the weight content is 80-85%, filtering, concentrating and drying filtrate obtained through filtration to prepare potassium dihydrogen phosphate. According to the method disclosed by the invention, potassium dihydrogen phosphate is prepared by adopting the extraction residual acid of phosphoric acid to ensure that the utilization rate of extraction residual acid of phosphoric acid is more than 85%, so that the utilization rate of extraction residual acid of phosphoric acid is improved; the purity of prepared potassium dihydrogen phosphate is about 98%, so that the beneficial effects are improved.
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 of 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, make the evolution phosphoric acid of technical grade and food grade, in production, phosphoric acid remaining after extraction becomes raffinate, in the process of producing at purifying phosphoric acid, in phosphoric acid by wet process, a large amount of impurity has entered in raffinate, and therefore, phosphoric acid raffinate is except containing P
2o
5outside 40%～50%, also contain 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 below 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 adopts neutralisation more, secondly also has organic extraction, double decomposition, ion exchange method.
Neutralisation, be to deliver to neutralizer after Pian Zhuan caustic potash flakes or salt of wormwood are made into 30% solution, under agitation, with 50% phosphoric acid solution neutralization, control temperature at 80-100 DEG C, pH is 4-5, neutralized reaction product after filtration, concentrated, crystallisation by cooling, centrifugation, get product after dry.Current, the throughput of national neutralisation potassium primary phosphate accounts for the more than 90% of overall throughput.This method is taking thermal phosphoric acid and potash as raw material, and production cost is high, is difficult to apply in agricultural, 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 be convenient to industrial applications; but; the method needs expensive potassium hydroxide and food grade phosphoric acid; production cost is higher, has limited large-scale production, and Recycling Mother Solution is just abandoned the pollution having increased environment 5 times.
Because high-quality phosphoric acid shortage and existing method are to utilize 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 and improves the utilization ratio of raffinate.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, and a kind of embodiment that utilizes phosphoric acid raffinate to prepare potassium primary phosphate is provided, and the method is prepared potassium primary phosphate using phosphoric acid raffinate as starting material, has improved 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), taking phosphoric acid raffinate as raw material, add any two kinds of organic impuritys removed in phosphoric acid raffinate in hydrogen peroxide, gac and water;
(2) to adding triethylamine in step (1) gained phosphoric acid raffinate, to regulate the PH of phosphoric acid raffinate be 6.5～7.5, filters and obtain filtrate A; Or be 45%～50% potassium hydroxide solution to adding weight content in step (1) gained phosphoric acid raffinate, regulating the PH of phosphoric acid raffinate is 6.5～7.5, filters and obtains liquor B;
(3) in filtrate A, add enough saturated potassium chloride solutions to make to add again enough water that crystal is all dissolved after its crystallize out, filter and obtain liquor C; Or to add in liquor B weight content be 45%～50% potassium hydroxide solution to regulate PH be 8.5～10.5, after filtration again to add in filtrate weight content be 80%～85% phosphoric acid solution to regulate PH be 3.8～4.1, filter and obtain filtrate D;
(4) by concentrated to liquor C or filtrate D, the dry solid phosphoric acid potassium dihydrogen that obtains.
According to one embodiment of present invention: the organic impurity that step (1) is removed in phosphoric acid raffinate is selected 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: after described hydrogen peroxide, gac are added in phosphoric acid raffinate, need to leave standstill 2～3 hours, then filter removal gac and impurity after adding suitable quantity of water dilution.
According to one embodiment of present invention: the organic impurity that step (1) is removed in phosphoric acid raffinate is selected 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: after described hydrogen peroxide, water are added in phosphoric acid raffinate, need heated and stirred, stop 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 is selected 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: after described water, gac are added in phosphoric acid raffinate, need to leave standstill after 2～3 hours and filter and 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%, the utilization ratio that has greatly improved phosphoric acid raffinate, this is simple for process, without great amount of investment, technical process is short, productive expense is low, without contaminated wastewater, without washing, water loss is few, can realize cleaner production, the potassium primary phosphate purity making, in 98% left and right, has improved its economic benefit greatly.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, 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, is not intended to limit the present invention.
The present invention can regulate pH value to 6.5～7.5 by phosphoric acid raffinate being added to different materials and phosphatase reaction, and described different material comprises the potassium hydroxide solution that triethylamine and weight content are 45%～50%.According to the difference of the material adding in this step, the processing mode of its gained filtrate is also different.
It is that 6.5～7.5 rear filtrations obtain filtrate that mode one, interpolation triethylamine regulate phosphoric acid raffinate PH, then in filtrate, add enough saturated potassium chloride solutions to make its crystallize out, and then add enough water that crystal is all dissolved, filtration obtains filtrate, and filtrate concentrate drying is obtained to solid phosphoric acid potassium dihydrogen;
It is that 6.5～7.5 rear filtrations obtain filtrate that the potassium hydroxide solution of mode two, interpolation 45%～50% regulates the PH of phosphoric acid raffinate, and then to regulate the PH of phosphoric acid raffinate with 45%～50% potassium hydroxide solution be 8.5～10.5, it is 3.8～4.1 that the phosphoric acid solution that is 80%～85% with weight content again after filtration regulates PH, filtration obtains filtrate, and filtrate concentrate drying is obtained to solid phosphoric acid potassium dihydrogen.In the manner, adopting two sections of potassium hydroxide solutions to regulate PH to be because added once filtration between its two sections, 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
Taking 500kg phosphoric acid raffinate as raw material, add 45kg hydrogen peroxide and 220kg water to it, heated and stirred, make temperature rise to 90 DEG C, stop heating, starting slowly to add 306kg triethylamine to regulate the PH of phosphoric acid raffinate is 7, filters and obtains filter residue and filtrate, and hydrogen peroxide can be removed the organic impurity in phosphoric acid raffinate.In filter residue, add the recyclable triethylamine of potassium hydroxide, the rate of recovery of triethylamine reaches 92%, in filtrate, add 156kg saturated potassium chloride solution, make filtrate crystallize out, and then add 150kg water that the crystal of separating out is dissolved completely to it, then filter, by concentrated filtrate, the dry finished product potassium primary phosphate 331.5kg that obtains, 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 using 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, too much interpolation saturated potassium chloride solution only can make filtrate reaction residual solution later increase Repone K, crystal is separated out and be there is no useful effect, add very few saturated potassium chloride solution, can not make crystal all separate out, therefore, add enough saturated potassium chloride solutions that in filtrate, crystal is all separated out that makes.
Embodiment 2
Taking 500kg phosphoric acid raffinate as raw material, add 35kg hydrogen peroxide and 15kg gac to it, leave standstill 2 hours, after adding the dilution of 200kg water, filter, to dripping 350kg triethylamine in filtrate, to regulate the PH of phosphoric acid raffinate be 7.5, filtration obtains filter residue and filtrate, and hydrogen peroxide can be removed the organic impurity in phosphoric acid raffinate.In filter residue, add the recyclable triethylamine of potassium hydroxide, the rate of recovery of triethylamine reaches 92%, in filtrate, add 175kg saturated potassium chloride solution, make filtrate crystallize out, and then add 150kg water that the crystal of separating out is dissolved completely to it, and then filter, by concentrated filtrate, the dry finished product potassium primary phosphate 339kg that obtains, its productive rate is 88.9%, and the content of potassium primary phosphate is 98.8%.
Embodiment 3
Taking 500kg phosphoric acid raffinate as raw material, add 50kg hydrogen peroxide and 250kg water to it, heated and stirred, make temperature rise to 60 DEG C, stop heating, starting slowly to add 310kg triethylamine to regulate the PH of phosphoric acid raffinate is 6.5, filters and obtains filter residue and filtrate, and hydrogen peroxide can be removed the organic impurity in phosphoric acid raffinate.In filter residue, add the recyclable triethylamine of potassium hydroxide, the rate of recovery of triethylamine reaches 91%, in filtrate, add 160kg saturated potassium chloride solution, make filtrate crystallize out, and then add 150kg water that the crystal of separating out is dissolved completely to it, and then filter, by concentrated filtrate, the dry finished product potassium primary phosphate 330kg that obtains, its productive rate is 87%, and the content of potassium primary phosphate is 97.7%.
Embodiment 4
Taking 500kg phosphoric acid raffinate as raw material, add wherein 5kg gac and 150kg water, leave standstill 3 hours, to filter, subsequent operations step is identical with embodiment 2.
Except above-described embodiment, when organic impurity in removal phosphoric acid raffinate is selected 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 of removing in phosphoric acid raffinate is selected 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 when heating; The organic impurity of removing in phosphoric acid raffinate is selected 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
Taking 500kg phosphoric acid raffinate as raw material, add wherein 45kg hydrogen peroxide and 5kg gac, leave standstill 2 hours, after adding the dilution of 150kg water, filter, hydrogen peroxide and gac can be removed the organic impurity in phosphoric acid raffinate, after dilute with water, are more convenient for filtering, the amount of the water that dilution is used, without strict demand, only need to be added appropriate water phosphoric acid raffinate is filtered more easily.Be 48% potassium hydroxide solution to adding 697kg weight content in filtrate, regulating PH is 10 rear filtrations, be 85% phosphoric acid to adding 292kg weight content in filtrate, regulating PH is 3.8, then through concentrated, the dry solid phosphoric acid potassium dihydrogen 671.7kg that obtains, its productive rate is 86%, and the content of potassium primary phosphate is 97.6%.
Embodiment 6
Taking 500kg phosphoric acid raffinate as raw material, add wherein 5kg gac and 150kg water, leave standstill 2.5 hours, filter, be 48% potassium hydroxide solution to adding 391kg weight content in filtrate, regulating PH is 7, after filtration, be 48% potassium hydroxide solution to adding 205kg weight content in filtrate again, regulating PH is 10 rear filtrations, be 85% phosphoric acid to adding 205kg weight content in filtrate, regulating PH is 3.8, then through concentrated, the dry solid phosphoric acid potassium dihydrogen 575.4kg that obtains, its productive rate is 89.9%, and the content of potassium primary phosphate is 98.4%.
Embodiment 7
Taking 500kg phosphoric acid raffinate as raw material, add wherein 25kg hydrogen peroxide and 25kg gac, leave standstill 3 hours, filter, be 50% potassium hydroxide solution to adding 385kg weight content in filtrate, regulating PH is 7.5, after filtration, be 50% potassium hydroxide solution to adding 200kg weight content in filtrate again, regulating PH is 10.5 rear filtrations, be 85% phosphoric acid to adding 201kg weight content in filtrate, regulating PH is 4.1, then through concentrated, the dry solid phosphoric acid potassium dihydrogen 569.8kg that obtains, its productive rate is 89.1%, and the content of potassium primary phosphate is 98.45%.
Embodiment 8
Taking 500kg phosphoric acid raffinate as raw material, add wherein 50kg hydrogen peroxide and 250kg water, heated and stirred, make temperature rise to 60 DEG C, stop heating, be 45% potassium hydroxide solution to adding 405kg weight content in filtrate, regulating PH is 6.5, after filtration, be 45% potassium hydroxide solution to adding 200kg weight content in filtrate again, regulating PH is 8.5 rear filtrations, be 80% phosphoric acid to adding 220kg weight content in filtrate, regulating PH is 4.1, then through concentrated, the dry solid phosphoric acid potassium dihydrogen 550kg that obtains, its productive rate is 88.1%, the content of potassium primary phosphate is 97.84%.
Embodiment 9
Taking 500kg phosphoric acid raffinate as raw material, add wherein 25kg hydrogen peroxide and 150kg water, heated and stirred, makes temperature rise to 90 DEG C, stops heating, and subsequent operations step is identical with embodiment 8.
Embodiment 10
Taking 500kg phosphoric acid raffinate as raw material, add wherein 25kg gac and 250kg water, leave standstill 3 hours, filter, subsequent step is identical with embodiment 6.
Mode two is used any two kinds of methods of removing the organic impurity in phosphoric acid raffinate in hydrogen peroxide, gac and water identical with method and the consumption of mode one with consumption, therefore, in mode two, use any two kinds of method and the consumptions of removing the organic impurity in phosphoric acid raffinate in hydrogen peroxide, gac and water all can apply in the embodiment of mode one.
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 embodiments, within these amendments and embodiment will drop on the disclosed principle scope and spirit of the application.More particularly, in the scope of and claim open in the application, can carry out multiple modification and improvement to the building block of subject combination layout and/or layout.Except modification that building block and/or layout are carried out with improving, to those skilled in the art, other purposes will be also obvious.
Claims (7)
1. utilize phosphoric acid raffinate to prepare a method for potassium primary phosphate, it is characterized in that, comprise the steps:
(1), taking phosphoric acid raffinate as raw material, add any two kinds of organic impuritys removed in phosphoric acid raffinate in hydrogen peroxide, gac and water;
(2) to adding triethylamine in step (1) gained phosphoric acid raffinate, to regulate the PH of phosphoric acid raffinate be 6.5～7.5, filters and obtain filtrate A; Or be 45%～50% potassium hydroxide solution to adding weight content in step (1) gained phosphoric acid raffinate, regulating the PH of phosphoric acid raffinate is 6.5～7.5, filters and obtains liquor B;
(3) in filtrate A, add enough saturated potassium chloride solutions to make to add again enough water that crystal is all dissolved after its crystallize out, filter and obtain liquor C; Or to add in liquor B weight content be 45%～50% potassium hydroxide solution to regulate PH be 8.5～10.5, after filtration again to add in filtrate weight content be 80%～85% phosphoric acid solution to regulate PH be 3.8～4.1, filter and obtain filtrate D;
(4) by concentrated to liquor C or filtrate D, the dry solid phosphoric acid potassium dihydrogen that obtains.
2. the method for utilizing phosphoric acid raffinate to prepare potassium primary phosphate according to claim 1, it is characterized in that: the organic impurity that step (1) is removed in phosphoric acid raffinate is selected hydrogen peroxide and gac, and the ratio of the weight of phosphoric acid raffinate, hydrogen peroxide, gac is 100:(5～10): (1～5).
3. the method for utilizing phosphoric acid raffinate to prepare potassium primary phosphate according to claim 2, it is characterized in that: after described hydrogen peroxide, gac are added in phosphoric acid raffinate, need to leave standstill 2～3 hours, then filter removal gac and impurity after adding suitable quantity of water dilution.
4. the method for utilizing phosphoric acid raffinate to prepare potassium primary phosphate according to claim 1, it is characterized in that: the organic impurity that step (1) is removed in phosphoric acid raffinate is selected hydrogen peroxide and water, and the ratio of the weight of phosphoric acid raffinate, hydrogen peroxide, water is 100:(5～10): (30～50).
5. the method for utilizing phosphoric acid raffinate to prepare potassium primary phosphate according to claim 4, is characterized in that: after described hydrogen peroxide, water are added in phosphoric acid raffinate, need heated and stirred, stop heating after making phosphoric acid raffinate temperature rise to 60～90 DEG C.
6. the method for utilizing phosphoric acid raffinate to prepare potassium primary phosphate according to claim 1, it is characterized in that: the organic impurity that step (1) is removed in phosphoric acid raffinate is selected gac and water, and the ratio of the weight of phosphoric acid raffinate, gac, water is 100:(1～5): (30～50).
7. the method for utilizing phosphoric acid raffinate to prepare potassium primary phosphate according to claim 6, is characterized in that: after described water, gac are added in phosphoric acid raffinate, need to leave standstill after 2～3 hours and filter and remove gac and impurity.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN106082153A (en) * | 2016-08-23 | 2016-11-09 | 湖北中孚化工集团有限公司 | Utilize the method and device of extraction tail washings synthesis potassium dihydrogen phosphate |
| CN106586990A (en) * | 2016-11-09 | 2017-04-26 | 中化重庆涪陵化工有限公司 | Method of using phosphoric acid by wet process to produce monopotassium phosphate |
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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 |
| CN101857216A (en) * | 2010-06-29 | 2010-10-13 | 贵州川恒化工有限责任公司 | Method for extracting and purifying wet-process phosphorous acid to produce industrial-grade phosphorous acid |
| 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 |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
| CN106082153A (en) * | 2016-08-23 | 2016-11-09 | 湖北中孚化工集团有限公司 | Utilize the method and device of extraction tail washings synthesis potassium dihydrogen phosphate |
| 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 |
| CN106586990A (en) * | 2016-11-09 | 2017-04-26 | 中化重庆涪陵化工有限公司 | Method of using phosphoric acid by wet process to produce monopotassium 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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