CN104016324A - Production method for tripotassium phosphate - Google Patents
Production method for tripotassium phosphate Download PDFInfo
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- CN104016324A CN104016324A CN201410213425.0A CN201410213425A CN104016324A CN 104016324 A CN104016324 A CN 104016324A CN 201410213425 A CN201410213425 A CN 201410213425A CN 104016324 A CN104016324 A CN 104016324A
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- Prior art keywords
- ureaphil
- tripotassium phosphate
- potassium hydroxide
- temperature
- stirring
- Prior art date
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- LWIHDJKSTIGBAC-UHFFFAOYSA-K tripotassium phosphate Chemical compound [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 title claims abstract description 232
- 229910000404 tripotassium phosphate Inorganic materials 0.000 title claims abstract description 111
- 235000019798 tripotassium phosphate Nutrition 0.000 title claims abstract description 111
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 45
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 207
- 238000003756 stirring Methods 0.000 claims abstract description 84
- 238000006243 chemical reaction Methods 0.000 claims abstract description 60
- VSNHCAURESNICA-UHFFFAOYSA-N Hydroxyurea Chemical compound NC(=O)NO VSNHCAURESNICA-UHFFFAOYSA-N 0.000 claims description 120
- 239000000047 product Substances 0.000 claims description 84
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 54
- 239000000243 solution Substances 0.000 claims description 50
- 239000000706 filtrate Substances 0.000 claims description 30
- 235000015320 potassium carbonate Nutrition 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- 239000012065 filter cake Substances 0.000 claims description 28
- 238000005119 centrifugation Methods 0.000 claims description 27
- 238000002360 preparation method Methods 0.000 claims description 19
- 239000007787 solid Substances 0.000 claims description 19
- 239000013078 crystal Substances 0.000 claims description 18
- 125000003917 carbamoyl group Chemical class [H]N([H])C(*)=O 0.000 claims description 16
- 239000007864 aqueous solution Substances 0.000 claims description 15
- 238000002425 crystallisation Methods 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 12
- 238000010792 warming Methods 0.000 claims description 12
- KDSSEOIBFVTMNM-UHFFFAOYSA-N [K].[K].[K].P(O)(O)(O)=O Chemical compound [K].[K].[K].P(O)(O)(O)=O KDSSEOIBFVTMNM-UHFFFAOYSA-N 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 32
- 239000002994 raw material Substances 0.000 abstract description 14
- 238000005265 energy consumption Methods 0.000 abstract description 10
- DZHMRSPXDUUJER-UHFFFAOYSA-N [amino(hydroxy)methylidene]azanium;dihydrogen phosphate Chemical compound NC(N)=O.OP(O)(O)=O DZHMRSPXDUUJER-UHFFFAOYSA-N 0.000 abstract description 4
- 238000003889 chemical engineering Methods 0.000 abstract 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 34
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 17
- 229910000027 potassium carbonate Inorganic materials 0.000 description 12
- 235000011181 potassium carbonates Nutrition 0.000 description 12
- 239000007795 chemical reaction product Substances 0.000 description 11
- 238000004458 analytical method Methods 0.000 description 10
- 238000005070 sampling Methods 0.000 description 10
- 238000001035 drying Methods 0.000 description 7
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 5
- 238000006386 neutralization reaction Methods 0.000 description 5
- 229940072033 potash Drugs 0.000 description 5
- 239000011591 potassium Substances 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- 235000011009 potassium phosphates Nutrition 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000003337 fertilizer Substances 0.000 description 4
- 229910000160 potassium phosphate Inorganic materials 0.000 description 4
- 229940093916 potassium phosphate Drugs 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 239000004202 carbamide Substances 0.000 description 3
- 230000008025 crystallization Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical compound Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 239000004278 EU approved seasoning Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 240000004808 Saccharomyces cerevisiae Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- MPNNOLHYOHFJKL-UHFFFAOYSA-N peroxyphosphoric acid Chemical compound OOP(O)(O)=O MPNNOLHYOHFJKL-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229940099402 potassium metaphosphate Drugs 0.000 description 1
- OQZCJRJRGMMSGK-UHFFFAOYSA-M potassium metaphosphate Chemical compound [K+].[O-]P(=O)=O OQZCJRJRGMMSGK-UHFFFAOYSA-M 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000003352 sequestering agent Substances 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000012747 synergistic agent Substances 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Landscapes
- Fertilizers (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of chemical engineering, and particularly relates to a production method for tripotassium phosphate. A tripotassium phosphate product is prepared by directly reacting urea phosphate and potassium hydroxide according to a molar ratio of 1: 2.95-3.05 for 30-60 min at a reaction temperature of 40-80 DEG C, with stirring at a stirring speed of 30 r/min. The tripotassium phosphate product is prepared by directly reacting urea phosphate and potassium hydroxide, so that the whole process has no requirements for high energy consumption; raw materials can be obtained relatively easily; a process route is short and simple; and production cost of tripotassium phosphate is reduced. By adjusting the process route and controlling reaction conditions, the produced tripotassium phosphate completely meets a first level standard of industrial tripotassium phosphate.
Description
Technical field
The present invention relates to chemical technology field, especially a kind of production method of Tripotassium phosphate.
Background technology
Tripotassium phosphate, another name: potassiumphosphate, potassium orthophosphate, three water potassiumphosphates, anhydrous phosphoric acid potassium; Colourless rhombic system crystallization or white crystalline powder; Tripotassium phosphate is in the industrial boiler water processing that is mainly used in, manufacture liquid soap, high-quality paper, treated gasoline, synthetic rubber, in foodstuffs industry, also can be used as buffer reagent, emulsifying agent, sequestrant, seasonings, yeast food, anti-oxidant synergistic agent, meat binding agent etc., in agricultural, be widely used in the production of high-efficient liquid fertilizer material.At present, for the preparation method of Tripotassium phosphate, mainly contain thermal phosphoric acid method, thermal phosphoric acid method is divided into again neutralisation and salt of wormwood method, neutralisation is to adopt thermal phosphoric acid to react preparing phosphoric acid tripotassium with potassium hydroxide, although this method obtains, product quality is higher, and its production energy consumption is larger, and cost is higher; Another method makes salt of wormwood method, this method is to adopt thermal phosphoric acid first to react with salt of wormwood, generate dipotassium hydrogen phosphate, dipotassium hydrogen phosphate solution continues to use in potassium hydroxide and generates Tripotassium phosphate, centrifugation, be dried to obtain product, this method salt of wormwood consumption is large, and processing condition require strict, and quality product is difficult to guarantee, and energy consumption is larger, cost is higher.
As the patent No. is: the preparation method > > of a < < Potassium tripolyphosphate of 200510048775.7 adopts peroxophosphoric acid and Anhydrous potassium carbonate high temperature solid state reaction one-step synthesis Tripotassium phosphate, through techniques such as neutralization, dry, pulverizing, roasting, pulverizing, obtain product again, visible this technical process is longer, complex process, energy consumption is high, raw materials cost is large, pollute greatly, be unfavorable for environmental protection and do not there is preferably economic benefit.
And for example the patent No. is: the preparation method > > of a < < electronic grade high-purity potassium permanganate of 200910193400.8 mixes potassium hydroxide solution and phosphoric acid solution, be heated to 85-100 ℃, under agitation condition, react, regulate pH value to 8-12, obtain the slip that pulp density is 47-50; Potassium hydroxide in potassium hydroxide solution and the amount of the phosphoric acid in phosphoric acid solution are than being 1:1; By the concentrated rear decoloring of slip high temperature, carrying out separation and purification, separation and purification product is continued to condensing crystal, dry, obtain dipotassium hydrogen phosphate; Dipotassium hydrogen phosphate, under 300-600 ℃ of hot conditions, is reacted, obtain potassiumphosphate product, although this method rate of recovery is higher, contamination-free produces, and repeatedly carries out pyroprocessing in the whole production technique of this method, its energy consumption is larger, and technical process is complicated, and life cycle of the product is long.
The preparation method > > of the < < high viscosity Potassium polymetaphosphate that the patent No. is 201310566409.5 for another example be take potassium primary phosphate as raw material, thermal dehydration polymerization generates, and in control raw material containing potassium raw material and the potassium of phosphorous raw material and the mol ratio of phosphorus, control temperature is the hot environment of 550-600 ℃, obtains final full-bodied potassiumphosphate product; This method has adopted technical process complicated, adopts pyroprocessing in technique, makes the energy consumption in whole production technique larger, and proportioning raw materials condition is harsh, makes raw materials cost larger, causes the cost of potassiumphosphate products production larger.
As can be seen here, in the prior art, the energy consumption that ubiquity in Tripotassium phosphate production process is larger, and raw materials cost is higher, the technical problem that production cost is larger.
Summary of the invention
In order to solve the above-mentioned technical problem existing in prior art, the invention provides a kind of production method of Tripotassium phosphate, this method has the advantages that energy consumption is low, technique is short and simple, with low cost.
Specifically be achieved through the following technical solutions:
A kind of production method of Tripotassium phosphate, that directly to adopt Ureaphil and potassium hydroxide be 1:(2.95-3.05 according to mol ratio), in temperature of reaction, be at 40-80 ℃, with the stirring velocity of 30r/min stirring reaction 30-60min at the uniform velocity, obtain Tripotassium phosphate product.
Specifically comprise the following steps:
(1) preparation of Ureaphil solution: Ureaphil is placed in to dissolving tank, the ratio that is 1:1 according to the mass ratio of Ureaphil and water adds water, and carry out stirring and dissolving according to the stirring velocity of 30-40r/min, and after being warming up to temperature and being 38 ℃, after continuation stirring and dissolving is even, obtain Ureaphil solution, stand-by;
(2) adding potassium hydroxide synthetic: by step 1) the Ureaphil solution that obtains proceeds in synthetic groove, and be 1:(2.95-3.05 according to the mol ratio of the mol ratio of Ureaphil and potassium hydroxide), add potassium hydroxide, and the temperature of controlling in reaction process maintains at 40-80 ℃, with the stirring velocity of 30r/min, at the uniform velocity after stirring reaction 30-90min, obtain Tripotassium phosphate product slip;
(3) crystallisation by cooling centrifugation: Tripotassium phosphate product slip is proceeded to and carries out decrease temperature crystalline processing in crystallizer, reduce temperature after≤35 ℃, after complete crystallize out, proceed to and in separating centrifuge, carry out centrifugation, obtain filtrate and filter cake, filtrate is the aqueous solution of carboxamide, sends to Ureaphil synthetic thread; Filter cake is Tripotassium phosphate crystal product, dry at 90 ℃, obtains Tripotassium phosphate product.
Described Ureaphil reacts with potassium hydroxide in preparing phosphoric acid tripotassium, is Ureaphil solution and potassium hydroxide solid reaction.
Described Ureaphil reacts with potassium hydroxide in preparing phosphoric acid tripotassium, is Ureaphil solution and potassium hydroxide solution reaction.
Described Ureaphil reacts with potassium hydroxide in preparing phosphoric acid tripotassium, is Ureaphil solid and potassium hydroxide solution reaction.
The mol ratio of described Ureaphil and the mol ratio of potassium hydroxide are 1:(2.95-3);
Described temperature of reaction is 50-70 ℃;
The described stirring reaction time is 50-70min.
The mol ratio of described Ureaphil and the mol ratio of potassium hydroxide are 1:(3-3.05);
Described temperature of reaction is 60 ℃;
The described stirring reaction time is 60min.
Described decrease temperature crystalline is processed, and reduces temperature to≤30 ℃.
Described filtrate is the aqueous solution of carboxamide, can also send to the synthetic production line of Ureaphil.
Described potassium hydroxide can also first adopt salt of wormwood to replace, and the mol ratio of salt of wormwood and Ureaphil is 1:(0.95-1.05); Adopt potassium hydroxide to react with its mixing solutions, the mol ratio of potassium hydroxide and its mixing solutions is 1:1 again.
Compared with prior art, technique effect of the present invention is embodied in:
1 is reacted and prepares Tripotassium phosphate product with potassium hydroxide by direct employing Ureaphil, makes whole process without high energy consumption demand, and raw material obtains comparatively simple, and operational path is short and simple, has reduced the production cost of Tripotassium phosphate.
2 by recycling the by product producing, and makes it that recycle occur, and avoids the discharge of waste gas and waste liquid and waste residue, has the significant value of environmental protection.
3 by the adjustment of operational path and the control of reaction conditions, and the Tripotassium phosphate that makes to produce meets the acceptable end product standard of industrial Tripotassium phosphate completely.
Accompanying drawing explanation
Fig. 1 is the equipment flowsheet that Ureaphil of the present invention reacts with potassium hydroxide.
Fig. 2 is the equipment flowsheet that Ureaphil of the present invention reacts with salt of wormwood.
1-dissolving tank 2-synthesizes groove 3-crystallizer 4-separating centrifuge 5-pre-synthesis groove.
Embodiment
Below in conjunction with accompanying drawing and concrete embodiment, technical scheme of the present invention is done to further restriction, but claimed scope is not only confined to done description.
Noun explanation:
Ureaphil (Ureaphosphate, UP), is for No. CAS 4861-19-2, and molecular formula is CH
7n
2o
5p, can be expressed as CO (NH
2)
2h
3pO
4:
It is a kind of fine chemical product that is widely used in the fields such as livestock industry, industry, agricultural, its solid is white crystals or crystalline powder, and soluble in water and alcohol is insoluble to ethers, toluene and tetracol phenixin, it is acid that the aqueous solution is, and starts to decompose to emit carbonic acid gas and ammonia during melting.
Principle explanation:
The present invention adopts highly purified Ureaphil to react with potassium hydroxide to prepare Tripotassium phosphate product, and the chemical equation of its reaction is:
CO(NH
2)
2·H
3PO
4+3KOH＝K
3PO
4+CO(NH
2)
2+3H
2O
By controlling the mol ratio of Ureaphil and potassium hydroxide, temperature of reaction, reaction times and adjustment endpoint pH, the final generation of controlling Tripotassium phosphate product, by drying machine, be dried again, can obtain product, this process does not have the discharge of the three wastes, whole technical process is simple, there is no the consumption of high energy consumption, and by product is urea soln, utilization be can be recovered and Ureaphil and crystallization generation chemical fertilizer regenerated, improved the comprehensive utilization of raw material in Tripotassium phosphate preparation process, reduced production cost, constant product quality.
Meanwhile, the present invention also first adopts Ureaphil to react with salt of wormwood to prepare dipotassium hydrogen phosphate product, then adds potassium hydroxide in dipotassium hydrogen phosphate slip, and the principle equation of its reaction is:
CO(NH
2)
2·H
3PO
4+K
2CO
3＝K
2HPO
4+CO(NH
2)
2+H
2O+CO
2K
2HPO
4+KOH＝K
3PO
4+H
2O
This law is on the basis of first method, reduce the degree-of-difficulty factor in starting material source, the preparation process that is Tripotassium phosphate by salt of wormwood provides part potassium element, reduce the waste of potassium hydroxide raw material, simultaneously, in whole production process, by product is urea slip, there is not removal of impurities process, reduced the degree-of-difficulty factor of technical process, simplified Tripotassium phosphate preparation technology, and urea slip can be recovered and utilize cyclic production Ureaphil or as the raw material of chemical fertilizer production line, crystallization generates chemical fertilizer, improved the raw material availability in Tripotassium phosphate process of producing product, strengthened the stability of quality product.
Be illustrated in figure 1 the equipment flowsheet that Ureaphil of the present invention reacts with potassium hydroxide.Ureaphil being added in dissolving tank 1 to water is mixed with after Ureaphil solution, in be transported to synthetic groove 2 by transferpump, and according in the certain situation of the mol ratio of Ureaphil and potassium hydroxide, in synthetic groove 2, add potassium hydroxide solution, make it that neutralization reaction occur, and by controlling reaction times and temperature of reaction, adjust endpoint pH, make it generate Tripotassium phosphate slip; By Tripotassium phosphate slip being proceeded to crystallizer 3, be cooled under certain temperature, after Tripotassium phosphate crystal is separated out, again Tripotassium phosphate crystal is proceeded to and in separating centrifuge 4, carry out centrifugation, obtain filtrate and filter cake, the slip that filtrate being contained carboxamide, sent to the synthetic production line of Ureaphil, carried out recycle; Filter cake is Tripotassium phosphate product, sends in drying machine and adopts certain drying temperature to carry out drying treatment, obtains Tripotassium phosphate product, meets an industrial grade Tripotassium phosphate product standard completely.
Be illustrated in figure 2 the equipment flowsheet that Ureaphil of the present invention reacts with salt of wormwood.Ureaphil being added in dissolving tank 1 to water is mixed with after Ureaphil solution, by transferpump, be transported in pre-synthesis groove 5 again, and add salt of wormwood according to Ureaphil and the certain mol ratio of salt of wormwood, after question response acquires a certain degree, then by slurry pipeline transport in synthetic groove 2, then add the potassium hydroxide solution with salt of wormwood equimolar ratio, make it that neutralization reaction occur, and control the temperature of whole reaction process, reaction times and endpoint pH, make it generate Tripotassium phosphate slip; Again Tripotassium phosphate slurry pipeline transport is separated out after Tripotassium phosphate crystal to lowering the temperature in crystallizer 3, again Tripotassium phosphate crystal is proceeded in separating centrifuge 4 and carry out centrifugation, obtain filtrate and filter cake, the slip that filtrate being contained carboxamide, sent to the synthetic production line of Ureaphil, carried out recycle; Filter cake is Tripotassium phosphate product, sends in drying machine and adopts certain drying temperature to carry out drying treatment, obtains Tripotassium phosphate product, meets an industrial grade Tripotassium phosphate product standard completely.
Embodiment 1
A production method for Tripotassium phosphate, specifically comprises the following steps:
(1) preparation of Ureaphil solution: Ureaphil is placed in to dissolving tank, the ratio that is 1:1 according to the mass ratio of Ureaphil and water adds water, and carry out stirring and dissolving according to the stirring velocity of 30r/min, and after being warming up to temperature and being 38 ℃, after continuation stirring and dissolving is even, obtain Ureaphil solution, stand-by;
(2) adding potassium hydroxide synthetic: by step 1) the Ureaphil solution that obtains proceeds in synthetic groove, and be 1:2.95 according to the mol ratio of the mol ratio of Ureaphil and potassium hydroxide, add potassium hydroxide solid, and the temperature of controlling in reaction process maintains at 40 ℃, with the stirring velocity of 30r/min, at the uniform velocity after stirring reaction 30min, obtain Tripotassium phosphate product slip;
(3) crystallisation by cooling centrifugation: Tripotassium phosphate product slip is proceeded to and carries out decrease temperature crystalline processing in crystallizer, reduce after temperature to 35 ℃, after complete crystallize out, proceed to and in separating centrifuge, carry out centrifugation, obtain filtrate and filter cake, filtrate is the aqueous solution of carboxamide, sends to Ureaphil synthetic thread; Filter cake is Tripotassium phosphate crystal product, dry at 90 ℃, obtains Tripotassium phosphate product.
Sampling analysis, quality product reaches PHOSPHORIC ACID TECH.GRADE tripotassium acceptable end product standard completely.
Embodiment 2
A production method for Tripotassium phosphate, specifically comprises the following steps:
(1) preparation of Ureaphil solution: Ureaphil is placed in to dissolving tank, the ratio that is 1:1 according to the mass ratio of Ureaphil and water adds water, and carry out stirring and dissolving according to the stirring velocity of 31r/min, and after being warming up to temperature and being 38 ℃, after continuation stirring and dissolving is even, obtain Ureaphil solution, stand-by;
(2) adding potassium hydroxide synthetic: by step 1) the Ureaphil solution that obtains proceeds in synthetic groove, and be 1:2.96 according to the mol ratio of the mol ratio of Ureaphil and potassium hydroxide, add potassium hydroxide solution, and the temperature of controlling in reaction process maintains at 44 ℃, with the stirring velocity of 30r/min, at the uniform velocity after stirring reaction 36min, obtain Tripotassium phosphate product slip;
(3) crystallisation by cooling centrifugation: Tripotassium phosphate product slip is proceeded to and carries out decrease temperature crystalline processing in crystallizer, reduce after temperature to 34 ℃, after complete crystallize out, proceed to and in separating centrifuge, carry out centrifugation, obtain filtrate and filter cake, filtrate is the aqueous solution of carboxamide, sends to Ureaphil synthetic thread; Filter cake is Tripotassium phosphate crystal product, dry at 90 ℃, obtains Tripotassium phosphate product.
Sampling analysis, quality product reaches PHOSPHORIC ACID TECH.GRADE tripotassium acceptable end product standard completely.
Embodiment 3
A production method for Tripotassium phosphate, specifically comprises the following steps:
(1) preparation of potassium hydroxide solution: potassium hydroxide solid is placed in to dissolving tank, the ratio that is 1:1 according to the mass ratio of potassium hydroxide and water adds water, and carry out stirring and dissolving according to the stirring velocity of 32r/min, and after being warming up to temperature and being 38 ℃, after continuation stirring and dissolving is even, obtain potassium hydroxide solution, stand-by;
(2) adding Ureaphil solid synthetic: by step 1) potassium hydroxide solution that obtains proceeds in synthetic groove, and be 1:3.05 according to the mol ratio of the mol ratio of Ureaphil and potassium hydroxide, add Ureaphil solid, and the temperature of controlling in reaction process maintains at 48 ℃, with the stirring velocity of 30r/min, at the uniform velocity after stirring reaction 42min, obtain Tripotassium phosphate product slip;
(3) crystallisation by cooling centrifugation: Tripotassium phosphate product slip is proceeded to and carries out decrease temperature crystalline processing in crystallizer, reduce after temperature to 33 ℃, after complete crystallize out, proceed to and in separating centrifuge, carry out centrifugation, obtain filtrate and filter cake, filtrate is the aqueous solution of carboxamide, sends to Ureaphil synthetic thread; Filter cake is Tripotassium phosphate crystal product, dry at 90 ℃, obtains Tripotassium phosphate product.
Sampling analysis, quality product reaches PHOSPHORIC ACID TECH.GRADE tripotassium acceptable end product standard completely.
Embodiment 4
A production method for Tripotassium phosphate, specifically comprises the following steps:
(1) preparation of Ureaphil solution: Ureaphil is placed in to dissolving tank, the ratio that is 1:1 according to the mass ratio of Ureaphil and water adds water, and carry out stirring and dissolving according to the stirring velocity of 33r/min, and after being warming up to temperature and being 38 ℃, after continuation stirring and dissolving is even, obtain Ureaphil solution, stand-by;
(2) adding potassium hydroxide synthetic: by step 1) the Ureaphil solution that obtains proceeds in synthetic groove, and according to the mol ratio of the mol ratio of Ureaphil and salt of wormwood, be first 1:0.95, add potash solid, and the temperature of controlling in reaction process maintains at 52 ℃, with the stirring velocity of 30r/min at the uniform velocity after stirring reaction 48min; The ratio that is 1:1 according to the mol ratio of Ureaphil and potassium hydroxide again adds potassium hydroxide solid, and the temperature of controlling in reaction process maintains at 52 ℃, with the stirring velocity of 30r/min at the uniform velocity after stirring reaction 30min; Obtain Tripotassium phosphate product slip;
(3) crystallisation by cooling centrifugation: Tripotassium phosphate product slip is proceeded to and carries out decrease temperature crystalline processing in crystallizer, reduce after temperature to 32 ℃, after complete crystallize out, proceed to and in separating centrifuge, carry out centrifugation, obtain filtrate and filter cake, filtrate is the aqueous solution of carboxamide, sends to Ureaphil synthetic thread; Filter cake is Tripotassium phosphate crystal product, dry at 90 ℃, obtains Tripotassium phosphate product.
Sampling analysis, quality product reaches PHOSPHORIC ACID TECH.GRADE tripotassium acceptable end product standard completely.
Embodiment 5
A production method for Tripotassium phosphate, specifically comprises the following steps:
(1) preparation of Ureaphil solution: Ureaphil is placed in to dissolving tank, the ratio that is 1:1 according to the mass ratio of Ureaphil and water adds water, and carry out stirring and dissolving according to the stirring velocity of 35r/min, and after being warming up to temperature and being 38 ℃, after continuation stirring and dissolving is even, obtain Ureaphil solution, stand-by;
(2) adding potassium hydroxide synthetic: by step 1) the Ureaphil solution that obtains proceeds in synthetic groove, and according to the mol ratio of the mol ratio of Ureaphil and salt of wormwood, be first 1:1.05, add solution of potassium carbonate, and the temperature of controlling in reaction process maintains at 56 ℃, with the stirring velocity of 30r/min at the uniform velocity after stirring reaction 42min; The ratio that is 1:1 according to the mol ratio of Ureaphil and potassium hydroxide again adds potassium hydroxide solution, and the temperature of controlling in reaction process maintains at 56 ℃, with the stirring velocity of 30r/min at the uniform velocity after stirring reaction 48min; Obtain Tripotassium phosphate product slip;
(3) crystallisation by cooling centrifugation: Tripotassium phosphate product slip is proceeded to and carries out decrease temperature crystalline processing in crystallizer, reduce after temperature to 31 ℃, after complete crystallize out, proceed to and in separating centrifuge, carry out centrifugation, obtain filtrate and filter cake, filtrate is the aqueous solution of carboxamide, sends to Ureaphil synthetic thread; Filter cake is Tripotassium phosphate crystal product, dry at 90 ℃, obtains Tripotassium phosphate product.
Sampling analysis, quality product reaches PHOSPHORIC ACID TECH.GRADE tripotassium acceptable end product standard completely.
Embodiment 6
A production method for Tripotassium phosphate, specifically comprises the following steps:
(1) preparation of Ureaphil solution: Ureaphil is placed in to dissolving tank, the ratio that is 1:1 according to the mass ratio of Ureaphil and water adds water, and carry out stirring and dissolving according to the stirring velocity of 37r/min, and after being warming up to temperature and being 38 ℃, after continuation stirring and dissolving is even, obtain Ureaphil solution, stand-by;
(2) adding potassium hydroxide synthetic: by step 1) the Ureaphil solution that obtains proceeds in synthetic groove, and according to the mol ratio of the mol ratio of Ureaphil and salt of wormwood, be first 1:1, add potash solid, and the temperature of controlling in reaction process maintains at 60 ℃, with the stirring velocity of 30r/min at the uniform velocity after stirring reaction 50min; The ratio that is 1:1 according to the mol ratio of Ureaphil and potassium hydroxide again adds potassium hydroxide solution, and the temperature of controlling in reaction process maintains at 60 ℃, with the stirring velocity of 30r/min at the uniform velocity after stirring reaction 32min; Obtain Tripotassium phosphate product slip;
(3) crystallisation by cooling centrifugation: Tripotassium phosphate product slip is proceeded to and carries out decrease temperature crystalline processing in crystallizer, reduce after temperature to 30 ℃, after complete crystallize out, proceed to and in separating centrifuge, carry out centrifugation, obtain filtrate and filter cake, filtrate is the aqueous solution of carboxamide, sends to Ureaphil synthetic thread; Filter cake is Tripotassium phosphate crystal product, dry at 90 ℃, obtains Tripotassium phosphate product.
Sampling analysis, quality product reaches PHOSPHORIC ACID TECH.GRADE tripotassium acceptable end product standard completely.
Embodiment 7
A production method for Tripotassium phosphate, specifically comprises the following steps:
(1) preparation of Ureaphil solution: Ureaphil is placed in to dissolving tank, the ratio that is 1:1 according to the mass ratio of Ureaphil and water adds water, and carry out stirring and dissolving according to the stirring velocity of 39r/min, and after being warming up to temperature and being 38 ℃, after continuation stirring and dissolving is even, obtain Ureaphil solution, stand-by;
(2) adding potassium hydroxide synthetic: by step 1) the Ureaphil solution that obtains proceeds in synthetic groove, and according to the mol ratio of the mol ratio of Ureaphil and salt of wormwood, be first 1:1.04, add solution of potassium carbonate, and the temperature of controlling in reaction process maintains at 70 ℃, with the stirring velocity of 30r/min at the uniform velocity after stirring reaction 55min; The ratio that is 1:1 according to the mol ratio of Ureaphil and potassium hydroxide again adds potassium hydroxide solid, and the temperature of controlling in reaction process maintains at 70 ℃, with the stirring velocity of 30r/min at the uniform velocity after stirring reaction 35min; Obtain Tripotassium phosphate product slip;
(3) crystallisation by cooling centrifugation: Tripotassium phosphate product slip is proceeded to and carries out decrease temperature crystalline processing in crystallizer, reduce after temperature to 25 ℃, after complete crystallize out, proceed to and in separating centrifuge, carry out centrifugation, obtain filtrate and filter cake, filtrate is the aqueous solution of carboxamide, sends to Ureaphil synthetic thread; Filter cake is Tripotassium phosphate crystal product, dry at 90 ℃, obtains Tripotassium phosphate product.
Sampling analysis, quality product reaches PHOSPHORIC ACID TECH.GRADE tripotassium acceptable end product standard completely.
Embodiment 8
A production method for Tripotassium phosphate, specifically comprises the following steps:
(1) preparation of solution of potassium carbonate: potash solid is placed in to dissolving tank, the ratio that is 1:1 according to the mass ratio of salt of wormwood and water adds water, and carry out stirring and dissolving according to the stirring velocity of 40r/min, and after being warming up to temperature and being 38 ℃, after continuation stirring and dissolving is even, obtain solution of potassium carbonate, stand-by;
(2) adding Ureaphil synthetic: by step 1) solution of potassium carbonate that obtains proceeds in synthetic groove, and be 1:1.02 according to the mol ratio of the mol ratio of Ureaphil and salt of wormwood, add Ureaphil solution, and the temperature of controlling in reaction process maintains at 80 ℃, with the stirring velocity of 30r/min at the uniform velocity after stirring reaction 70min, the ratio that is 1:1 according to the mol ratio of Ureaphil and potassium hydroxide again adds potassium hydroxide solution, and the temperature of controlling in reaction process maintains at 80 ℃, with the stirring velocity of 30r/min at the uniform velocity after stirring reaction 20min, obtain Tripotassium phosphate product slip,
(3) crystallisation by cooling centrifugation: Tripotassium phosphate product slip is proceeded to and carries out decrease temperature crystalline processing in crystallizer, reduce after temperature to 29 ℃, after complete crystallize out, proceed to and in separating centrifuge, carry out centrifugation, obtain filtrate and filter cake, filtrate is the aqueous solution of carboxamide, sends to Ureaphil synthetic thread; Filter cake is Tripotassium phosphate crystal product, dry at 90 ℃, obtains Tripotassium phosphate product.
Sampling analysis, quality product reaches PHOSPHORIC ACID TECH.GRADE tripotassium acceptable end product standard completely.
Embodiment 9
A production method for Tripotassium phosphate, specifically comprises the following steps:
(1) preparation of solution of potassium carbonate: potash solid is placed in to dissolving tank, the ratio that is 1:1 according to the mass ratio of salt of wormwood and water adds water, and carry out stirring and dissolving according to the stirring velocity of 39r/min, and after being warming up to temperature and being 38 ℃, after continuation stirring and dissolving is even, obtain solution of potassium carbonate, stand-by;
(2) adding Ureaphil synthetic: by step 1) solution of potassium carbonate that obtains proceeds in synthetic groove, and be 1:1.01 according to the mol ratio of the mol ratio of Ureaphil and salt of wormwood, add Ureaphil solid, and the temperature of controlling in reaction process maintains at 75 ℃, with the stirring velocity of 30r/min at the uniform velocity after stirring reaction 75min, the ratio that is 1:1 according to the mol ratio of Ureaphil and potassium hydroxide again adds potassium hydroxide solid, and the temperature of controlling in reaction process maintains at 75 ℃, with the stirring velocity of 30r/min at the uniform velocity after stirring reaction 15min, obtain Tripotassium phosphate product slip,
(3) crystallisation by cooling centrifugation: Tripotassium phosphate product slip is proceeded to and carries out decrease temperature crystalline processing in crystallizer, reduce after temperature to 27 ℃, after complete crystallize out, proceed to and in separating centrifuge, carry out centrifugation, obtain filtrate and filter cake, filtrate is the aqueous solution of carboxamide, sends to Ureaphil synthetic thread; Filter cake is Tripotassium phosphate crystal product, dry at 90 ℃, obtains Tripotassium phosphate product.
Sampling analysis, quality product reaches PHOSPHORIC ACID TECH.GRADE tripotassium acceptable end product standard completely.
Embodiment 10
A production method for Tripotassium phosphate, specifically comprises the following steps:
(1) preparation of solution of potassium carbonate: potash solid is placed in to dissolving tank, the ratio that is 1:1 according to the mass ratio of salt of wormwood and water adds water, and carry out stirring and dissolving according to the stirring velocity of 36r/min, and after being warming up to temperature and being 38 ℃, after continuation stirring and dissolving is even, obtain solution of potassium carbonate, stand-by;
(2) adding Ureaphil synthetic: by step 1) solution of potassium carbonate that obtains proceeds in synthetic groove, and be 1:0.99 according to the mol ratio of the mol ratio of Ureaphil and salt of wormwood, add Ureaphil solid, and the temperature of controlling in reaction process maintains at 65 ℃, with the stirring velocity of 30r/min at the uniform velocity after stirring reaction 45min, the ratio that is 1:1 according to the mol ratio of Ureaphil and potassium hydroxide again adds potassium hydroxide solution, and the temperature of controlling in reaction process maintains at 65 ℃, with the stirring velocity of 30r/min at the uniform velocity after stirring reaction 45min, obtain Tripotassium phosphate product slip,
(3) crystallisation by cooling centrifugation: Tripotassium phosphate product slip is proceeded to and carries out decrease temperature crystalline processing in crystallizer, reduce after temperature to 28 ℃, after complete crystallize out, proceed to and in separating centrifuge, carry out centrifugation, obtain filtrate and filter cake, filtrate is the aqueous solution of carboxamide, sends to Ureaphil synthetic thread; Filter cake is Tripotassium phosphate crystal product, dry at 90 ℃, obtains Tripotassium phosphate product.
Sampling analysis, quality product reaches PHOSPHORIC ACID TECH.GRADE tripotassium acceptable end product standard completely.
At this, it is important to point out: above embodiment only limits to understand technical scheme of the present invention is further elaborated; and can not be interpreted as technical scheme of the present invention is done to further restriction; those skilled in the art is in the scope of above-described embodiment and technical scheme of the present invention; that makes does not have outstanding substantive distinguishing features and significant progressive improvement with the present invention, still belongs to protection category of the present invention.
Claims (10)
1. the production method of a Tripotassium phosphate, it is characterized in that: be that directly to adopt Ureaphil and potassium hydroxide be 1:(2.95-3.05 according to mol ratio), in temperature of reaction, be at 40-80 ℃, with the stirring velocity of 30r/min stirring reaction 30-60min at the uniform velocity, obtain Tripotassium phosphate product.
2. the production method of Tripotassium phosphate as claimed in claim 1, is characterized in that: comprise the following steps:
(1) preparation of Ureaphil solution: Ureaphil is placed in to dissolving tank, the ratio that is 1:1 according to the mass ratio of Ureaphil and water adds water, and carry out stirring and dissolving according to the stirring velocity of 30-40r/min, and after being warming up to temperature and being 38 ℃, after continuation stirring and dissolving is even, obtain Ureaphil solution, stand-by;
(2) adding potassium hydroxide synthetic: by step 1) the Ureaphil solution that obtains proceeds in synthetic groove, and be 1:(2.95-3.05 according to the mol ratio of the mol ratio of Ureaphil and potassium hydroxide), add potassium hydroxide, and the temperature of controlling in reaction process maintains at 40-80 ℃, with the stirring velocity of 30r/min, at the uniform velocity after stirring reaction 30-90min, obtain Tripotassium phosphate product slip;
(3) crystallisation by cooling centrifugation: Tripotassium phosphate product slip is proceeded to and carries out decrease temperature crystalline processing in crystallizer, reduce temperature after≤35 ℃, after complete crystallize out, proceed to and in separating centrifuge, carry out centrifugation, obtain filtrate and filter cake, filtrate is the aqueous solution of carboxamide, sends to the synthetic production line of Ureaphil; Filter cake is Tripotassium phosphate crystal product, dry at 90 ℃, obtains Tripotassium phosphate product.
3. the production method of Tripotassium phosphate as claimed in claim 1 or 2, is characterized in that: described Ureaphil reacts with potassium hydroxide in preparing phosphoric acid tripotassium, is Ureaphil solution and potassium hydroxide solid reaction.
4. the production method of Tripotassium phosphate as claimed in claim 1 or 2, is characterized in that: described Ureaphil reacts with potassium hydroxide in preparing phosphoric acid tripotassium, is Ureaphil solution and potassium hydroxide solution reaction.
5. the production method of Tripotassium phosphate as claimed in claim 1 or 2, is characterized in that: described Ureaphil reacts with potassium hydroxide in preparing phosphoric acid tripotassium, is Ureaphil solid and potassium hydroxide solution reaction.
6. the production method of Tripotassium phosphate as claimed in claim 1 or 2, is characterized in that: the mol ratio of described Ureaphil and the mol ratio of potassium hydroxide are 1:(2.95-3); Described temperature of reaction is 50-70 ℃; The described stirring reaction time is 50-70min.
7. the production method of Tripotassium phosphate as claimed in claim 1 or 2, is characterized in that: the mol ratio of described Ureaphil and the mol ratio of potassium hydroxide are 1:(3-3.05); Described temperature of reaction is 60 ℃; The described stirring reaction time is 60min.
8. the production method of Tripotassium phosphate as claimed in claim 2, is characterized in that: described decrease temperature crystalline is processed, and reduces temperature to≤30 ℃.
9. the production method of Tripotassium phosphate as claimed in claim 2, is characterized in that: the aqueous solution that described filtrate is carboxamide, can also send to the synthetic production line of Ureaphil.
10. the production method of Tripotassium phosphate as claimed in claim 1 or 2, is characterized in that: described potassium hydroxide can also first adopt salt of wormwood to replace, and the mol ratio of salt of wormwood and Ureaphil is 1:(0.95-1.05); Adopt potassium hydroxide to react with its mixing solutions, the mol ratio of potassium hydroxide and its mixing solutions is 1:1 again.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104276557A (en) * | 2014-09-19 | 2015-01-14 | 贵阳中化开磷化肥有限公司 | Production method for preparing tripotassium phosphate and byproduct special fertilizer for sunflowers |
| CN104276556A (en) * | 2014-09-19 | 2015-01-14 | 贵阳中化开磷化肥有限公司 | Production method of monopotassium phosphate with byproduct fertilizer specially used for towel gourd |
| CN104291904A (en) * | 2014-09-19 | 2015-01-21 | 贵州大学 | Preparation method of special fertilizer for mung bean |
| CN104291294A (en) * | 2014-09-19 | 2015-01-21 | 贵阳中化开磷化肥有限公司 | Production method for preparing tripotassium phosphate and by-producing special fertilizer for litchi |
| CN104291302A (en) * | 2014-09-19 | 2015-01-21 | 贵阳中化开磷化肥有限公司 | Production method for preparing tripotassium phosphate and co-producing fertilizer special for kiwi fruits |
| CN104310349A (en) * | 2014-09-19 | 2015-01-28 | 贵阳中化开磷化肥有限公司 | Method for preparing tripotassium phosphate and preparing special fertilizer for flax as byproduct |
| CN111747776A (en) * | 2020-06-04 | 2020-10-09 | 普罗丰禾(武汉)科技有限公司 | Polymeric full-water-soluble fertilizer, preparation method and application thereof, and preparation method of boron potassium polyphosphate compound |
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| GB1191635A (en) * | 1966-07-27 | 1970-05-13 | Marchon Products Ltd | Improvements in the manufacture of Orthophosphates |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| GB1191635A (en) * | 1966-07-27 | 1970-05-13 | Marchon Products Ltd | Improvements in the manufacture of Orthophosphates |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104276557A (en) * | 2014-09-19 | 2015-01-14 | 贵阳中化开磷化肥有限公司 | Production method for preparing tripotassium phosphate and byproduct special fertilizer for sunflowers |
| CN104276556A (en) * | 2014-09-19 | 2015-01-14 | 贵阳中化开磷化肥有限公司 | Production method of monopotassium phosphate with byproduct fertilizer specially used for towel gourd |
| CN104291904A (en) * | 2014-09-19 | 2015-01-21 | 贵州大学 | Preparation method of special fertilizer for mung bean |
| CN104291294A (en) * | 2014-09-19 | 2015-01-21 | 贵阳中化开磷化肥有限公司 | Production method for preparing tripotassium phosphate and by-producing special fertilizer for litchi |
| CN104291302A (en) * | 2014-09-19 | 2015-01-21 | 贵阳中化开磷化肥有限公司 | Production method for preparing tripotassium phosphate and co-producing fertilizer special for kiwi fruits |
| CN104310349A (en) * | 2014-09-19 | 2015-01-28 | 贵阳中化开磷化肥有限公司 | Method for preparing tripotassium phosphate and preparing special fertilizer for flax as byproduct |
| CN104291302B (en) * | 2014-09-19 | 2016-07-06 | 贵州开磷集团股份有限公司 | A kind of production method preparing tripotassium phosphate by-product special fertilizer for Chinese goosebeery |
| CN104291294B (en) * | 2014-09-19 | 2016-08-10 | 贵州开磷集团股份有限公司 | A kind of production method of preparing litchi special fertilizer by-product of tripotassium phosphate |
| CN104310349B (en) * | 2014-09-19 | 2016-08-17 | 贵州开磷集团股份有限公司 | A kind of production method preparing tripotassium phosphate by-product Caulis et Folium Lini special fertilizer |
| CN111747776A (en) * | 2020-06-04 | 2020-10-09 | 普罗丰禾(武汉)科技有限公司 | Polymeric full-water-soluble fertilizer, preparation method and application thereof, and preparation method of boron potassium polyphosphate compound |
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