CN102951623A - Production process for monopotassium phosphate - Google Patents
Production process for monopotassium phosphate Download PDFInfo
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- CN102951623A CN102951623A CN2012104582267A CN201210458226A CN102951623A CN 102951623 A CN102951623 A CN 102951623A CN 2012104582267 A CN2012104582267 A CN 2012104582267A CN 201210458226 A CN201210458226 A CN 201210458226A CN 102951623 A CN102951623 A CN 102951623A
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- primary phosphate
- phosphoric acid
- potassium primary
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 24
- 229910000402 monopotassium phosphate Inorganic materials 0.000 title claims abstract description 15
- 235000019796 monopotassium phosphate Nutrition 0.000 title claims abstract description 15
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 title abstract 3
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 title abstract 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 47
- 230000008929 regeneration Effects 0.000 claims abstract description 31
- 238000011069 regeneration method Methods 0.000 claims abstract description 31
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 26
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- 239000013078 crystal Substances 0.000 claims abstract description 24
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000000047 product Substances 0.000 claims abstract description 18
- 239000007791 liquid phase Substances 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 11
- 238000000605 extraction Methods 0.000 claims description 58
- 239000003795 chemical substances by application Substances 0.000 claims description 54
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 49
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 46
- 239000011591 potassium Substances 0.000 claims description 46
- 229910052700 potassium Inorganic materials 0.000 claims description 46
- 229910019142 PO4 Inorganic materials 0.000 claims description 42
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 42
- 239000010452 phosphate Substances 0.000 claims description 42
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 18
- 229910021529 ammonia Inorganic materials 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 239000007788 liquid Substances 0.000 claims description 13
- 238000005119 centrifugation Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 230000035484 reaction time Effects 0.000 claims description 11
- 150000003839 salts Chemical class 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 10
- 238000003860 storage Methods 0.000 claims description 10
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 6
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 claims description 6
- 238000012856 packing Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 4
- 150000003512 tertiary amines Chemical class 0.000 claims description 4
- 239000012467 final product Substances 0.000 claims description 3
- 238000005191 phase separation Methods 0.000 claims description 3
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 claims description 3
- 239000001103 potassium chloride Substances 0.000 abstract description 19
- 239000006227 byproduct Substances 0.000 abstract description 8
- 238000011084 recovery Methods 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000005260 corrosion Methods 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 26
- 235000011164 potassium chloride Nutrition 0.000 description 18
- 239000012452 mother liquor Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-L Phosphate ion(2-) Chemical compound OP([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-L 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000007795 chemical reaction product Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 239000012047 saturated solution Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- XTEGARKTQYYJKE-UHFFFAOYSA-M Chlorate Chemical compound [O-]Cl(=O)=O XTEGARKTQYYJKE-UHFFFAOYSA-M 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000001172 regenerating effect Effects 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 206010011409 Cross infection Diseases 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 206010029803 Nosocomial infection Diseases 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012267 brine Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 238000005649 metathesis reaction Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- OOHAUGDGCWURIT-UHFFFAOYSA-N n,n-dipentylpentan-1-amine Chemical compound CCCCCN(CCCCC)CCCCC OOHAUGDGCWURIT-UHFFFAOYSA-N 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
The invention discloses a production process for monopotassium phosphate, which mainly includes the following steps: (1) KCl solution is prepared and added with high-purity phosphoric acid, so that monopotassium phosphate is synthesized; (2) extractant is added, so that crystals are separated out; (3) after centrifugal separation, clean water is added for washing, and the crystals are then dried and packaged; (4) liquid ammonia is filled into the liquid phase, so that extractant regeneration reaction takes place; (5) the extractant is stored, and NH4Cl is concentrated to be crystallized. The process route is short, the investment cost is low, the production process is easy to operate, the product yield is high, the quality is good and stable, moreover, no hydrochloric acid is produced in the process of production, so that the corrosion of production equipment is less, the extractant recovery rate is high, and high-quality ammonium chloride byproduct can be produced as well.
Description
Technical field
The present invention relates to a kind of production technique of potassium primary phosphate, belong to chemical technology field.
Background technology
Potassium primary phosphate is a kind of broad-spectrum water-soluble phosphorous, high-efficiency compound fertilizer of potassium and the important source material of industry and pharmaceutical industries.Because potassium primary phosphate is of many uses, demand strengthens day by day, and production method is also varied, but still there are different shortcomings in each production method.Although the neutralisation operational path is short, reduced investment, its raw material is potassium hydroxide, and is expensive, production cost is higher.Ion exchange method has been used ion exchange resin, and price is high, and the one-time investment cost is large, and potassium dihydrogen phosphate concentration is low aborning, needs a large amount of energy consumptions during evaporation concentration, and economy is bad.The raw material of phosphoric acid salt double decomposition substantially all adopts KCl, and production cost is relatively low, but operational path is long, and the chlorate separating difficulty of the potassium primary phosphate of producing and reaction generation is large, causes quality product not high, and yield is low.The technique of solvent extration production potassium primary phosphate also has multiple, and because the solvent price is high, the rate of recovery is low eventually, or because the selection of solvent is unreasonable, and cause poor product quality, react the hydrochloric acid of generation to the seriously corroded of equipment, thereby can't be promoted.
CN102602905A discloses a kind of Methods For The Manufacture of Potassium Dihydrogen Phosphate, and it comprises: 1. with Repone K and the water-soluble product mother liquid that is made into of phosphoric acid, with ammonia and the water-soluble byproduct mother liquor that is made into of ammonium chloride; 2. in micro mixer, use extraction agent extracted products mother liquor, after this separate obtaining load extraction agent and extraction liquid; 3. potassium dihydrogen phosphate crystal is separated out in the raffinate cooling, through being separated, solid is product again, and liquid is the product mother liquid reuse; 4. in another micro mixer, with the byproduct mother liquor load extraction agent is carried out back extraction, obtain again regenerating extracting agent and strip liquor through being separated; 5. gained regenerating extracting agent reuse, strip liquor are separated out ammonia chloride crystal through cooling, and again through solid-liquid separation, solid is byproduct, and liquid is the reuse of byproduct mother liquor.This scheme can avoid product mother liquid and byproduct mother liquor to cause cross infection because carrying secretly with selective problems by technology controlling and process, avoids microlite to produce extraction process and crystallisation process decoupling zero by equipment intensification, can produce high-quality potassium primary phosphate.But, the quality that the Repone K that this scheme is used and phosphoric acid can not guarantee potassium primary phosphate and ammonium chloride; And the reaction times of each step is also indefinite, also is unfavorable for guaranteeing the quality of potassium primary phosphate and the reclaim recovery efficiency of extraction agent; Basic temperature maintains 20 ℃～50 ℃ in the technological process, temperature is on the low side, speed for each stage chemical does not play prograding, needs cooling to process in the product potassium primary phosphate precipitation process, when having increased facility investment so that operational path lengthen.
Summary of the invention
The object of the present invention is to provide a kind of production technique of potassium primary phosphate, solve the problem in the existing potassium primary phosphate production technology.
A kind of production technique of potassium primary phosphate mainly may further comprise the steps:
(1) preparation KCl solution adds high-purity phosphoric acid, synthetic potassium primary phosphate: under 55 ℃～75 ℃, salt bath is water-soluble with KCl changing, and is mixed with massfraction and is 20%～35% KCl solution; Send into 75%～85% high-purity phosphoric acid with pump in synthetic groove, add KCl solution in synthetic groove, Repone K and phosphoric acid molar ratios are 1:0.9, and temperature of reaction is 55 ℃～75 ℃, and the reaction times is 20～35min;
(2) add extraction agent, crystallize out: with the mixing solutions of completely reacted potassium primary phosphate and hydrochloric acid with being pumped in the groove of saltouing, starting simultaneously the extraction liquid pump sends into extraction agent in the groove of saltouing, stir, mix, reaction times is 20min～40min, and potassium dihydrogen phosphate crystal is separated out from mixing solutions; Described extraction agent refers to tri-n-butylamine, tri-n-amyl amine;
(3) centrifugation adds the clear water washing, again dried crystals, packing: the slip of phosphoric acid potassium dihydrogen crystal is sent into centrifugation in the whizzer, rotating speed is 800～1200r/min, and the time is 10～20min, and the liquid phase part of centrifugation is put the extractant regeneration groove into and done manipulation of regeneration; After liquid phase separation is finished, in whizzer, add the clear water washing, the potassium primary phosphate after washing is put into the drying machine inner drying, and temperature is 80～110 ℃, and the time is 30min, gets potassium dihydrogen phosphate product, and packing gets final product at last;
(4) pass into liquefied ammonia to liquid phase, generation extractant regeneration reaction: in the extractant regeneration groove, pass into concentration and be 10%～30% ammoniacal liquor, make the liquid phase of liquefied ammonia and centrifugation that the extractant regeneration reaction occur under the condition that stirs, reaction times is 15min～40min, afterwards with the extraction agent of regeneration with contain NH
4The solution of Cl is sent into the extraction agent separator tank;
(5) store extraction agent, NH
4Cl condensing crystal: with extraction agent and NH
4The mixing solutions of Cl enters standing demix behind the extraction agent separator tank, and the extraction agent on upper strata is sent into the extraction agent storage tank after the layering, in order to using next time; The NH of lower floor
4Cl solution is produced NH with being pumped into ammonium chloride condensing crystal groove
4The Cl product;
The purity of KCl in the described step (1) is more than 95%.
Change salt bath temperature in the described step (1) and KCl solution temperature are not higher than the temperature of synthetic groove.
Extraction agent in the described step (2) is alkyl carbon atoms at 4～8 tertiary amine.
Technical solution of the present invention is to utilize KCl and high-purity phosphoric acid generation replacement(metathesis)reaction to generate the principle preparing potassium dihydrogen phosphate of potassium primary phosphate and hydrochloric acid, and its chemical equation is:
H
3PO
4+KCl=KH
2PO
4+HCl
Generate the miscible fluid of potassium primary phosphate and hydrochloric acid after the reaction, add alkyl carbon atoms in the mixing solutions at 4～8 tertiary amine extraction hydrochloric acid wherein again, produce simultaneously salting-out effect, potassium dihydrogen phosphate crystal is separated out from mixing solutions, reaction equation is:
S+H
3PO
4+ KCl=KH
2PO
4+ SHCl(S represents extraction agent)
Pass into liquefied ammonia in the SHCl solution that occurs in the solvent extraction process again, make extractant regeneration, the extraction agent after the regeneration recycles, and the ammonium chloride that produces in the extractant regeneration process is done production marketing through aftertreatment.
S·HCl+NH
3→S+NH
4Cl
The present invention uses 75%～85% high-purity phosphoric acid and purity at the Repone K more than 95%, has guaranteed the quality of potassium primary phosphate and ammonium chloride.In step (1), changing salt bath and KCl solution temperature is 55 ℃～70 ℃, and brine temp must not be higher than synthetic groove temperature, not only avoided saturated potassium chloride solution Yin Wendu in building-up reactions to reduce and supersaturation causes solid potassium chloride to be separated out affecting reaction effect, also reduced the energy consumption when the byproduct ammonium chloride solution is concentrated; Repone K and phosphoric acid are 20～35min in the reaction times of synthetic groove, have guaranteed that building-up reactions generates the effect of potassium primary phosphate; The synthesis temperature of synthetic groove remains on 55 ℃～70 ℃, the speed of response that can accelerate to synthesize and minimizing reaction times.In step (2), extraction agent is the alkyl carbon atoms number at 4～8 tertiary amine, plays with the hydrochloric acid that reacts generation and is combined, and reduces the solubleness of potassium primary phosphate in water, promotes the effect of potassium primary phosphate crystallization; Extraction agent and the reaction times in the groove of saltouing are 20min～40min, have guaranteed the eduction rate of potassium primary phosphate.In step (4), the material stirring reaction times in the extractant regeneration groove has been improved the reclaim recovery efficiency of extraction agent at 15min～40min.
Beneficial effect of the present invention: operational path is short, and cost of investment is low, and is simple to operate, product yield is high, quality better, steady quality, and not having in process of production hydrochloric acid generates, corrosion to production unit is little, and the extraction agent rate of recovery is high, can also produce the ammonium chloride byproduct of quality better.
Reference numeral
Fig. 1 is process flow sheet of the present invention;
Fig. 2 is equipment flowsheet corresponding to Fig. 1.
Wherein: the 1-ization salt bath, the 2-phosphoric acid storage tank, 3-synthesizes groove, the 4-groove of saltouing, 5-extraction agent storage tank, the 6-whizzer, 7-extractant regeneration groove, 8-washing water storage tank, 9-drying machine, the 10-wrapping machine, 11-extraction agent separator tank, 12-extraction agent storage tank, 13-ammonium chloride condensing crystal groove.
Embodiment
In order to deepen the understanding of the present invention, the present invention is described in further detail below in conjunction with drawings and Examples, and this embodiment only is used for explaining the present invention, does not consist of the restriction to protection domain of the present invention.
Fig. 1 is process flow sheet of the present invention, as shown in Figure 1, technical process of the present invention is mainly: preparation KCl solution, add high-purity phosphoric acid, and make both that building-up reactions occur and generate potassium primary phosphate, then in the reactant that obtains, add extraction agent, crystallize out (potassium primary phosphate) carries out centrifugation again, adds the clear water washing and separates the crystal that obtains, and after dried crystals, pack, can obtain the potassium primary phosphate finished product; The liquid phase that separation obtains then by carrying out the extractant regeneration reaction to wherein passing into liquefied ammonia, is extracted agent and contains NH
4The solution of Cl, last, store extraction agent, and with NH
4The Cl condensing crystal obtains NH
4The Cl product.
Fig. 2 is equipment flowsheet corresponding to Fig. 1, and as shown in Figure 2, technical process of the present invention may further comprise the steps:
(1) preparation KCl solution adds high-purity phosphoric acid, synthetic potassium primary phosphate: add KCl and water to changing in the salt bath 1, be mixed with massfraction and be 20%～35% KCl solution; In synthetic groove 3, send into 75%～85% high-purity phosphoric acid from phosphoric acid storage tank 2 with pump, after reaching certain liquid level, synthetic groove 3 starts stirring rake, restart for salt pump, to synthetic groove 3 interior adding KCl solution, both mol ratios are 1:0.9, make KCl and phosphoric acid generate potassium primary phosphate at synthetic groove 3 internal reactions.
(2) add extraction agent, crystallize out: with the mixing solutions of completely reacted potassium primary phosphate and hydrochloric acid with being pumped in the groove 4 of saltouing, starting simultaneously the extraction liquid pump sends into extraction agent in the groove 4 of saltouing from extraction agent storage tank 5, extraction agent and hydrochloric potassium dihydrogen phosphate are fully mixed in situation about stirring, potassium dihydrogen phosphate crystal is separated out from mixing solutions.
(3) centrifugation, add the clear water washing, dried crystals is packed: after potassium primary phosphate is separated out fully again, the slip of phosphoric acid potassium dihydrogen crystal is sent into whizzer 6 interior centrifugations, and the liquid phase part of centrifugation is put extractant regeneration groove 7 into and is done manipulation of regeneration; After liquid phase separation was finished, to an amount of clear water washing of whizzer 6 interior addings, the potassium primary phosphate after washing was put into drying machine 9 inner dryings and is got potassium dihydrogen phosphate product by washing water storage tank 8 when centrifugal, sent at last wrapping machine 10 packings and got final product.
(4) pass into liquefied ammonia to liquid phase, the extractant regeneration reaction occur: in extractant regeneration groove 7, pass into the liquefied ammonia of metering, liquefied ammonia and SHCl reacted under the condition that stirs, extractant regeneration out, after extractant regeneration is finished, with extraction agent with contain NH
4The solution of Cl is sent into extraction agent separator tank 10.
(5) store extraction agent, NH
4Cl condensing crystal: extraction agent and NH
4The mixing solutions of Cl enters extraction agent separator tank 11 rear standing demix, and the extraction agent on upper strata is sent into extraction agent storage tank 12 after the layering, in order to using next time; The NH of lower floor
4Cl solution is produced NH with being pumped into ammonium chloride condensing crystal groove 13
4The Cl product.
Be 85% thermal phosphoric acid with being pumped into 1000Kg acid dense in the synthetic groove, in situation about stirring with sour temperature rise to 60 ℃, after be that 60 ℃ the saturated solution that contains 650KgKCl is with the synthetic groove of pumping with the salt liquid temp, keeping the temperature of synthetic groove is 60 ℃, reaction 30min, the mixed solution of synthetic phosphoric acid potassium dihydrogen is put to the groove of saltouing, the tri-n-butylamine that adds 1600Kg in the groove of saltouing is made extraction agent and is stirred 20min, through centrifugal, washing, get potassium primary phosphate 1130Kg after the drying, the biphosphate potassium content is more than 98% by analysis, and other indexs all reach the acceptable end product requirement.Mother liquor after centrifugal enters the mother liquor regeneration groove, and with entering liquefied ammonia 150Kg stirring reaction 30min, weighing gets tri-n-butylamine 1590Kg behind the standing demix to regeneration tank.
Adding 1500Kg acid dense with pump in the synthetic groove is 70% the phosphorus mud made phosphoric acid that burns, in situation about stirring with sour temperature rise to 70 ℃, after be that 70 ℃ the saturated solution that contains 810KgKCl is with the synthetic groove of pumping with the salt liquid temp, keeping the temperature of synthetic groove is 70 ℃, reaction 35min, the mixed solution of synthetic phosphoric acid potassium dihydrogen is put to the groove of saltouing, the tri-n-butylamine that adds 2020Kg in the groove of saltouing is made extraction agent and is stirred 30min, through centrifugal, washing, get potassium primary phosphate 1380Kg after the drying, the biphosphate potassium content is 98.5% by analysis, and other indexs all reach the acceptable end product requirement.Liquid phase after centrifugal enters the extractant regeneration groove, sends into liquefied ammonia 180Kg stirring reaction 35min to the extractant regeneration groove, and weighing gets tri-n-butylamine 2175Kg behind the standing demix.
Adding 1500Kg acid dense with pump in the synthetic groove is 70% the phosphorus mud made phosphoric acid that burns, in situation about stirring with sour temperature rise to 70 ℃, after be that 70 ℃ the saturated solution that contains 810KgKCl is with the synthetic groove of pumping with the salt liquid temp, keeping the temperature of synthetic groove is 70 ℃, reaction 35min, the mixed solution of synthetic phosphoric acid potassium dihydrogen is put to the groove of saltouing, the Tri-n-Propylamine that adds 2020Kg in the groove of saltouing is made extraction agent and is stirred 30min, through centrifugal, washing, get potassium primary phosphate 1380Kg after the drying, the biphosphate potassium content is 98.5% by analysis, and other indexs all reach the acceptable end product requirement.Liquid phase after centrifugal enters the liquid phase regeneration tank, sends into liquefied ammonia 180Kg stirring reaction 35min to the extractant regeneration groove, and weighing gets Tri-n-Propylamine 2175Kg behind the standing demix.
Claims (5)
1. the production technique of a potassium primary phosphate is characterized in that: mainly may further comprise the steps:
(1) preparation KCl solution adds high-purity phosphoric acid, synthetic potassium primary phosphate: under 55 ℃～75 ℃, salt bath is water-soluble with KCl changing, and is mixed with massfraction and is 20%～35% KCl solution; Send into 75%～85% high-purity phosphoric acid with pump in synthetic groove, add KCl solution in synthetic groove, Repone K and phosphoric acid molar ratios are 1:0.9, and temperature of reaction is 55 ℃～75 ℃, and the reaction times is 20～35min;
(2) add extraction agent, crystallize out: with the mixing solutions of completely reacted potassium primary phosphate and hydrochloric acid with being pumped in the groove of saltouing, starting simultaneously the extraction liquid pump sends into extraction agent in the groove of saltouing, stir, mix, reaction times is 20min～40min, and potassium dihydrogen phosphate crystal is separated out from mixing solutions; Described extraction agent refers to tri-n-butylamine, Tri-n-Propylamine;
(3) centrifugation adds the clear water washing, again dried crystals, packing: the slip of phosphoric acid potassium dihydrogen crystal is sent into centrifugation in the whizzer, rotating speed is 800～1200r/min, and the time is 10～20min, and the liquid phase part of centrifugation is put the extractant regeneration groove into and done manipulation of regeneration; After liquid phase separation is finished, in whizzer, add the clear water washing, the potassium primary phosphate after washing is put into the drying machine inner drying, and temperature is 80～110 ℃, and the time is 30min, gets potassium dihydrogen phosphate product, and packing gets final product at last;
(4) pass into liquefied ammonia to liquid phase, generation extractant regeneration reaction: in the extractant regeneration groove, pass into concentration and be about 10%～30% liquefied ammonia, make the liquid phase of liquefied ammonia and centrifugation that the extractant regeneration reaction occur under the condition that stirs, reaction times is 15min～40min, afterwards with the extraction agent of regeneration with contain NH
4The solution of Cl is sent into the extraction agent separator tank;
(5) store extraction agent, NH
4Cl condensing crystal: with extraction agent and NH
4The mixing solutions of Cl enters standing demix behind the extraction agent separator tank, and the extraction agent on upper strata is sent into the extraction agent storage tank after the layering, in order to using next time; The NH of lower floor
4Cl solution is produced NH with being pumped into ammonium chloride condensing crystal groove
4The Cl product.
2. the production technique of a kind of potassium primary phosphate according to claim 1, it is characterized in that: the purity of the KCl in the described step (1) is more than 95%.
3. the production technique of a kind of potassium primary phosphate according to claim 1, it is characterized in that: the high-purity phosphoric acid in the described step (1) is thermal phosphoric acid or Wet Phosphoric Acid Market.
4. the production technique of a kind of potassium primary phosphate according to claim 1 is characterized in that: the change salt bath temperature in the described step (1) and KCl solution temperature are not higher than the temperature of synthetic groove.
5. the production technique of a kind of potassium primary phosphate according to claim 1, it is characterized in that: the extraction agent in the described step (2) is the tertiary amine of alkyl carbon atoms number between 4～8.
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261377A (en) * | 2014-09-19 | 2015-01-07 | 贵阳中化开磷化肥有限公司 | Production method for preparing monopotassium phosphate and coproducing special fertilizer for capsella bursa-pastoris |
| CN105271153A (en) * | 2015-09-25 | 2016-01-27 | 贵州开磷集团股份有限公司 | Method for preparing potassium dihydrogen phosphate from wet phosphoric acid |
| CN107739026A (en) * | 2017-11-13 | 2018-02-27 | 贵阳开磷化肥有限公司 | A kind of method of the micro- reaction production PHOSPHORIC ACID TECH.GRADE ammonium dihydrogen of phosphoric acid by wet process |
| CN107758637A (en) * | 2017-11-13 | 2018-03-06 | 贵阳开磷化肥有限公司 | A kind of method of the micro- reaction production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen of phosphoric acid by wet process |
| CN110395707A (en) * | 2019-08-13 | 2019-11-01 | 广州怡和生物科技有限公司 | A kind of preparation method of potassium dihydrogen phosphate |
| CN114191847A (en) * | 2021-12-12 | 2022-03-18 | 四川鑫瑞源科技发展有限公司 | Extracting agent for producing potassium dihydrogen phosphate by solvent extraction method and preparation method and application thereof |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261377A (en) * | 2014-09-19 | 2015-01-07 | 贵阳中化开磷化肥有限公司 | Production method for preparing monopotassium phosphate and coproducing special fertilizer for capsella bursa-pastoris |
| CN105271153A (en) * | 2015-09-25 | 2016-01-27 | 贵州开磷集团股份有限公司 | Method for preparing potassium dihydrogen phosphate from wet phosphoric acid |
| CN107739026A (en) * | 2017-11-13 | 2018-02-27 | 贵阳开磷化肥有限公司 | A kind of method of the micro- reaction production PHOSPHORIC ACID TECH.GRADE ammonium dihydrogen of phosphoric acid by wet process |
| CN107758637A (en) * | 2017-11-13 | 2018-03-06 | 贵阳开磷化肥有限公司 | A kind of method of the micro- reaction production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen of phosphoric acid by wet process |
| CN107758637B (en) * | 2017-11-13 | 2020-12-18 | 贵阳开磷化肥有限公司 | Method for producing industrial-grade potassium dihydrogen phosphate by wet-process phosphoric acid micro-reaction |
| CN110395707A (en) * | 2019-08-13 | 2019-11-01 | 广州怡和生物科技有限公司 | A kind of preparation method of potassium dihydrogen phosphate |
| CN114191847A (en) * | 2021-12-12 | 2022-03-18 | 四川鑫瑞源科技发展有限公司 | Extracting agent for producing potassium dihydrogen phosphate by solvent extraction method and preparation method and application thereof |
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| CN102951623B (en) | 2014-11-26 |
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