CN104386664B - The method of ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate - Google Patents
The method of ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate Download PDFInfo
- Publication number
- CN104386664B CN104386664B CN201410604033.7A CN201410604033A CN104386664B CN 104386664 B CN104386664 B CN 104386664B CN 201410604033 A CN201410604033 A CN 201410604033A CN 104386664 B CN104386664 B CN 104386664B
- Authority
- CN
- China
- Prior art keywords
- filtrate
- ammonium
- dihydrogen phosphate
- potassium dihydrogen
- phosphate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Fertilizers (AREA)
Abstract
The invention discloses a kind of method that ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate, the step of the method is as follows: obtain fertilizer grade ammonium dihydrogen phosphate after being dissolved by fertilizer grade primary ammonium phosphate, fertilizer grade ammonium dihydrogen phosphate and Repone K are carried out replacement(metathesis)reaction, and then centrifugation obtains ammonium potassium dihydrogen phosphate crystal.Present method adopts fertilizer grade primary ammonium phosphate as raw material, and the cost of this raw material is lower than PHOSPHORIC ACID TECH.GRADE ammonium dihydrogen by about 45%, and the finished product production cost is significantly reduced.Present method adopts twice replacement(metathesis)reaction, and make replacement(metathesis)reaction more complete, improve the yield of product, the yield of product reaches more than 90% of theoretical value, effective content>=99% of ammonium potassium dihydrogen phosphate in product, total nutrient (N+P
2o
5+ K
2o)>=75%, reaches the requirement of technical grade completely.Recycling Mother Solution in the present invention uses, and produces, to the less pollution of environment in whole reaction process without waste water.
Description
[technical field]
The present invention relates to a kind of phosphatic production method, be specifically related to a kind of method that ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate.
[background technology]
Ammonium potassium dihydrogen phosphate is the phosphoric acid salt that nitrogen, phosphorus, potassium content are all high, and utilized widely in the industry such as industry, agricultural, health, food, the market requirement is very large.There is the salt index and fertilizer properties that are similar to potassium primary phosphate.Not chloride ion-containing and cupric ion in product, arsenic content is lower than 10ppm.Industrially be mainly used in pharmaceutical sector and fermentation industry, microorganism, mushroom substratum, pH buffer reagent, produce the raw material of potassium pyrophosphate; Main efficient phosphorus potassium complex fertilizer, the high-quality chlorideless potassic fertilizer being used as high density in Agro-industry.Be particluarly suitable for for preparing damping fluid and nutrient solution in fermentation industry, and the high density water-soluble preparation spraying fertilizer entirely.Ammonium potassium dihydrogen phosphate has nutritive ingredient high (nitrogen, phosphorus, potassium effective constituent > 90%), and stable chemical nature is odorless, tasteless, nontoxic, soluble in water, does not lump, is thus applicable to various soil and crop; Ammonium potassium dihydrogen phosphate can improve crops quality and can improve crop and resist saline and alkaline, drought resisting, ability cold-resistant, resistant to lodging; With agricultural chemicals or growth regulator rationally mixed can play apply fertilizer, preventing disease pest control and stimulate the effect of plant growth.Higher with the product cost of traditional technology, the current developments of industry adopts new raw material and novel technique, reduces production cost further, improve the quality of products.The production method of ammonium potassium dihydrogen phosphate mainly contains: in and cocrystallization method, ion exchange method, double decomposition etc.China mainly adopts directly and cocrystallization method, and technique is simple, but need consume expensive potassium hydroxide, and production cost is higher, limits production-scale expansion.The production cost of ion exchange method is lower slightly, but technique is more complicated, to the heavy contamination of environment.
The clear 49-40560 of Japanese Patent Publication (1974) discloses a kind of method of primary ammonium phosphate and Repone K manufacture potassium primary phosphate, the advantage of the method is that production potassium primary phosphate is less demanding to processing condition, product yield is high, but very high to the requirement of raw material, price is relatively high.
Publication number be CN85104779 patent discloses a kind of with mud phosphoric acid for raw material, PH=5 is neutralized with bicarbonate of ammonia, produce the method for ammonium potassium dihydrogen phosphate with Repone K replacement(metathesis)reaction after removing impurity, the advantage of the method is less demanding to raw material, produce that ammonium potassium dihydrogen phosphate technical process is simple, energy consumption is not high in production process, but potassium element utilization ratio is not high, product quality is not high, the main content of phosphoric acid salt only 75%.
Publication number be CN92108206.1 patent discloses one raw phosphoric acid Repone K defluorinate silicic acid in a wet process, pH value 3 ~ 5 is neutralized again with ammonia, produce the production method of ammonium potassium dihydrogen phosphate with Repone K replacement(metathesis)reaction after secondary filtration removing impurity, the advantage of the method is less demanding to phosphate raw material, comparatively traditional method reduces costs 20 ~ 30%, but total recovery only 60 ~ 80%, the main content of phosphoric acid salt is not high, cl content 2%, product quality is not high.
Application number is the preparation method that patent discloses a kind of ammonium potassium dihydrogen phosphate of CN200810058885.5, with phosphorus ore, sulfuric acid, Repone K for raw material, neutralization, concentrated, filter and obtain ammonium potassium dihydrogen phosphate, the raw materials cost of the method is lower, but waste gas, waste sludge discharge are more, to the heavy contamination of environment.
[summary of the invention]
[technical problem that will solve]
The object of this invention is to provide that a kind of cost is low, quality is high, be convenient to the production method of the ammonium potassium dihydrogen phosphate of large-scale production, the method adopts cheap fertilizer grade primary ammonium phosphate and Repone K replacement(metathesis)reaction to produce ammonium potassium dihydrogen phosphate and by-product ammonium chloride.
[technical scheme]
The present invention is achieved through the following technical solutions.
The invention provides a kind of method that ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate, the step of the method is as follows:
A, by fertilizer grade primary ammonium phosphate and water by solid-to-liquid ratio 1:2 ~ 1:3 stirring and dissolving at temperature 60 ~ 100 DEG C, then flame filter press collecting by filtration first filtrate is used, in the first filtrate, add 25% ammoniacal liquor regulate pH to 4 ~ 5, then plate and frame filter collecting by filtration second filtrate is used, in the second filtrate, add 25% ammoniacal liquor regulate pH to 7 ~ 8, then use plate and frame filter collecting by filtration the 3rd filtrate;
B, in the 3rd filtrate, add solid potassium chloride and stirring and dissolving, the phosphoric acid adding 85% again regulates material liquid pH to 4.0 ~ 4.5 reaction 2 ~ 4h at temperature >=80 DEG C, treats that feed liquid is cooled to 45 ~ 50 DEG C of centrifugations and obtains the first mother liquor and described ammonium potassium dihydrogen phosphate crystal;
C, continue to add Repone K and stirring and dissolving in the first mother liquor, then the phosphoric acid adding 85% regulates material liquid pH to 3.8 ~ 4.2, continues to be cooled to 18 ~ 25 DEG C of centrifugations and obtains the second mother liquor and described ammonium potassium dihydrogen phosphate crystal;
D, by the second mother liquor and fertilizer grade primary ammonium phosphate and water stirring and dissolving at temperature 60 ~ 100 DEG C, wherein the solid-to-liquid ratio of fertilizer grade primary ammonium phosphate and the second mother liquor and water is 1:2 ~ 1:3, repeats above-mentioned steps A ~ C.
According to another implementation of the invention, the step of the method is as follows:
A, by fertilizer grade primary ammonium phosphate and water by solid-to-liquid ratio 1:2 ~ 1:3 stirring and dissolving at temperature 60 ~ 100 DEG C, then flame filter press collecting by filtration first filtrate is used, in the first filtrate, add 25% ammoniacal liquor regulate pH to 4 ~ 5, then plate and frame filter collecting by filtration second filtrate is used, in the second filtrate, add 25% ammoniacal liquor regulate pH to 7 ~ 8, then use plate and frame filter collecting by filtration the 3rd filtrate;
B, in the 3rd filtrate, add solid potassium chloride and stirring and dissolving, the phosphoric acid adding 85% again regulates material liquid pH to 4.0 ~ 4.5 reaction 2 ~ 4h at temperature >=80 DEG C, treats that feed liquid is cooled to 45 ~ 50 DEG C of centrifugations and obtains the first mother liquor and described ammonium potassium dihydrogen phosphate crystal;
C, continue to add Repone K and stirring and dissolving in the first mother liquor, then the phosphoric acid adding 85% regulates material liquid pH to 3.8 ~ 4.2, continues to be cooled to 18 ~ 25 DEG C of centrifugations and obtains the second mother liquor and described ammonium potassium dihydrogen phosphate crystal;
D, by the second mother liquor and fertilizer grade primary ammonium phosphate and water stirring and dissolving at temperature 60 ~ 100 DEG C, wherein the solid-to-liquid ratio of fertilizer grade primary ammonium phosphate and the second mother liquor and water is 1:2 ~ 1:3, then flame filter press collecting by filtration the 4th filtrate is used, in the 4th filtrate, add 25% ammoniacal liquor regulate pH to 4 ~ 5, then plate and frame filter collecting by filtration the 5th filtrate is used, in the 5th filtrate, add 25% ammoniacal liquor regulate pH to 7 ~ 8, then use plate and frame filter collecting by filtration the 6th filtrate;
E, the 6th filtrate is cooled to 18 ~ 20 DEG C, centrifugation obtains the 7th filtrate and solid by-product ammonium chloride;
F, in the 7th filtrate, add Repone K and stirring and dissolving, repeat above-mentioned step B ~ E.
According to an embodiment of the invention, the saturated ammonium potassium dihydrogen phosphate solution washing at least twice of described ammonium potassium dihydrogen phosphate crystal, then dry at temperature 80 ~ 100 DEG C after centrifuge dehydration, after washing, the fertilizer grade primary ammonium phosphate of mother liquor and steps A and water mix.
According to an embodiment of the invention, in described step B, the mol ratio of solid potassium chloride and fertilizer grade primary ammonium phosphate is 0.5 ~ 0.8:1.
According to an embodiment of the invention, in described step C, in Repone K and step B, solid potassium chloride mass ratio is 1 ~ 2:10.
The present invention is further illustrated below.
The invention provides a kind of method that ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate, the step of the method is as follows:
A, by fertilizer grade primary ammonium phosphate and water by solid-to-liquid ratio 1:2 ~ 1:3 stirring and dissolving at temperature 60 ~ 100 DEG C, then flame filter press collecting by filtration first filtrate is used, in the first filtrate, add 25% ammoniacal liquor regulate pH to 4 ~ 5, then plate and frame filter collecting by filtration second filtrate is used, in the second filtrate, add 25% ammoniacal liquor regulate pH to 7 ~ 8, then use plate and frame filter collecting by filtration the 3rd filtrate;
In above-mentioned step, add 25% ammoniacal liquor and regulate the effect of pH to 4 ~ 5 to be that this part impurity precipitated under making mild acid conditions is separated out in the first filtrate, if pH is less than 4 or be greater than 5, this part impurity can be dissolved in filtrate.In the second filtrate, add 25% ammoniacal liquor regulates the effect of pH to 7 ~ 8 to be that the impurity precipitated under making neutrallty condition is separated out, if pH is less than 7 or be greater than 8, partial impurities can be dissolved in filtrate.
In above-mentioned step, 25% ammoniacal liquor is the ammoniacal liquor of massfraction 25%, i.e. in the ammonia soln of total mass 100g, and the NH containing 25g
3.
B, in the 3rd filtrate, add solid potassium chloride and stirring and dissolving, the phosphoric acid adding 85% again regulates material liquid pH to 4.0 ~ 4.5 reaction 2 ~ 4h at temperature >=80 DEG C, treats that feed liquid is cooled to 45 ~ 50 DEG C of centrifugations and obtains the first mother liquor and described ammonium potassium dihydrogen phosphate crystal;
In above-mentioned step, there is following reaction in the solid potassium chloride added and ammonium dihydrogen phosphate: NH
4h
2pO
4+ KCl → KH
2pO
4+ NH
4cl.This reaction is reacted at temperature >=80 DEG C in pH to 4.0 ~ 4.5, and as temperature of reaction < 80 DEG C, then speed of response significantly reduces.
In above-mentioned step, add 85% phosphoric acid regulate material liquid pH to 4.0 ~ 4.5, if pH be less than 4.0 or be greater than 4.5 time, then affect the purity of the finished product.
According to the preferred embodiment of the present invention, the phosphoric acid adding 85% regulates material liquid pH to 4.0 ~ 4.5 to react 2 ~ 4h at temperature 80 ~ 120 DEG C; Preferred embodiment is, at temperature 80 ~ 100 DEG C, react 2 ~ 4h; Preferred embodiment is, at temperature 80 DEG C, react 2 ~ 4h.
In above-mentioned step, feed liquid is cooled to 45 ~ 50 DEG C of centrifugations and obtains the first mother liquor and described ammonium potassium dihydrogen phosphate crystal at temperature 45 ~ 50 DEG C, why carry out centrifugation be because product is easy to separate out at this temperature.
C, continue to add Repone K and stirring and dissolving in the first mother liquor, then the phosphoric acid adding 85% regulates material liquid pH to 3.8 ~ 4.2, continues to be cooled to 18 ~ 25 DEG C of centrifugations and obtains the second mother liquor and described ammonium potassium dihydrogen phosphate crystal;
Above-mentioned step C is that solid potassium chloride and ammonium dihydrogen phosphate further replacement(metathesis)reaction occur, the object of this step be make the phosphate radical in mother liquor and potassium ion excessive.
The temperature of reaction of above-mentioned steps is 45 ~ 50 DEG C (temperature of the first mother liquor that step B obtains is 45 ~ 50 DEG C).In above-mentioned step, obtaining the second mother liquor and described ammonium potassium dihydrogen phosphate crystal in 18 ~ 25 DEG C of centrifugations, at temperature 18 ~ 25 DEG C, why carry out centrifugation object be separate out more ammonium potassium dihydrogen phosphate crystal.
D, by the second mother liquor and fertilizer grade primary ammonium phosphate and water stirring and dissolving at temperature 60 ~ 100 DEG C, wherein the solid-to-liquid ratio of fertilizer grade primary ammonium phosphate and the second mother liquor and water is 1:2 ~ 1:3, repeats above-mentioned steps A ~ C.
According to another implementation of the invention, the step of the method is as follows:
A, by fertilizer grade primary ammonium phosphate and water by solid-to-liquid ratio 1:2 ~ 1:3 stirring and dissolving at temperature 60 ~ 100 DEG C, then flame filter press collecting by filtration first filtrate is used, in the first filtrate, add 25% ammoniacal liquor regulate pH to 4 ~ 5, then plate and frame filter collecting by filtration second filtrate is used, in the second filtrate, add 25% ammoniacal liquor regulate pH to 7 ~ 8, then use plate and frame filter collecting by filtration the 3rd filtrate;
B, in the 3rd filtrate, add solid potassium chloride and stirring and dissolving, the phosphoric acid adding 85% again regulates material liquid pH to 4.0 ~ 4.5 reaction 2 ~ 4h at temperature >=80 DEG C, treats that feed liquid is cooled to 45 ~ 50 DEG C of centrifugations and obtains the first mother liquor and described ammonium potassium dihydrogen phosphate crystal;
C, continue to add Repone K and stirring and dissolving in the first mother liquor, then the phosphoric acid adding 85% regulates material liquid pH to 3.8 ~ 4.2, continues to be cooled to 18 ~ 25 DEG C of centrifugations and obtains the second mother liquor and described ammonium potassium dihydrogen phosphate crystal;
D, by the second mother liquor and fertilizer grade primary ammonium phosphate and water stirring and dissolving at temperature 60 ~ 100 DEG C, wherein the solid-to-liquid ratio of fertilizer grade primary ammonium phosphate and the second mother liquor and water is 1:2 ~ 1:3, then flame filter press collecting by filtration the 4th filtrate is used, in the 4th filtrate, add 25% ammoniacal liquor regulate pH to 4 ~ 5, then plate and frame filter collecting by filtration the 5th filtrate is used, in the 5th filtrate, add 25% ammoniacal liquor regulate pH to 7 ~ 8, then use plate and frame filter collecting by filtration the 6th filtrate;
E, the 6th filtrate is cooled to 18 ~ 20 DEG C, centrifugation obtains the 7th filtrate and solid by-product ammonium chloride;
F, in the 7th filtrate, add Repone K and stirring and dissolving, repeat above-mentioned step B ~ E.
According to an embodiment of the invention, the technical process of this production method has two kinds of modes: first kind of way, and process flow steps comprises above-mentioned steps A ~ F, includes the obtaining step of by-product ammonium chloride in which; The second way, process flow steps comprises steps A ~ D and F, circulate above-mentioned step, the 6th filtrate of collecting in step D in which add Repone K and stirring and dissolving obtain described in ammonium potassium dihydrogen phosphate crystal, do not comprise the obtaining step of by-product ammonium chloride.According in a specific embodiment of the present invention, the second way often circulates after 3 ~ 5 times and carries out 1 ~ 2 first kind of way, crystallization when building up to a certain amount of to make by-product ammonium chloride.
According to an embodiment of the invention, the saturated ammonium potassium dihydrogen phosphate solution washing at least twice of described ammonium potassium dihydrogen phosphate crystal, then dry at temperature 80 ~ 100 DEG C after centrifuge dehydration, after washing, the fertilizer grade primary ammonium phosphate of mother liquor and steps A and water mix.
According to an embodiment of the invention, solid potassium chloride in described step B: the mol ratio of primary ammonium phosphate is 0.5 ~ 0.8:1.
According to an embodiment of the invention, in described step C, Repone K is 10 ~ 20% of potassium chloride dosage in step B.Only needing in this step C to add a small amount of Repone K is to make potassium ion in mother liquor excessive.
[beneficial effect]
Present method adopts fertilizer grade primary ammonium phosphate as raw material, and the cost of this raw material is lower by about 45% than using PHOSPHORIC ACID TECH.GRADE ammonium dihydrogen, and the cost of the finished product is significantly reduced.
Present method adopts twice replacement(metathesis)reaction, and make replacement(metathesis)reaction more complete, improve the yield of product, the yield of product reaches more than 90% of theoretical value, effective content>=99% of ammonium potassium dihydrogen phosphate in product, total nutrient (N+P
2o
5+ K
2o)>=75%, reaches the requirement of technical grade completely.
Recycling Mother Solution in the present invention uses, and produces, to the less pollution of environment in whole reaction process without waste water.
[accompanying drawing explanation]
Fig. 1 is the process flow sheet that one embodiment of the present invention produces ammonium potassium dihydrogen phosphate;
Fig. 2 is the process flow sheet that another embodiment of the present invention produces ammonium potassium dihydrogen phosphate.
[embodiment]
The present invention can be understood better by following embodiment.
Embodiment 1:
The step that ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate is as follows:
A, by 1000kg fertilizer grade primary ammonium phosphate and 3000kg water under temperature 60 C in dissolving tank stirring and dissolving, dissolved stirring time is 0.5h, then flame filter press collecting by filtration first filtrate is used, first filtrate is placed in settling bath, in the first filtrate, add 25% ammoniacal liquor 200 ~ 300kg regulate pH to 4 ~ 5, then plate and frame filter collecting by filtration second filtrate is used, second filtrate is placed in settling bath, in the second filtrate, add 25% ammoniacal liquor regulate pH to 7 ~ 8, then use plate and frame filter collecting by filtration the 3rd filtrate;
B, the 3rd filtrate is put into crystallizer, solid potassium chloride 500kg is added and stirring and dissolving in the 3rd filtrate, industrial phosphoric acid 700 ~ the 750kg adding 85% again regulates material liquid pH to 4.0 ~ 4.5 to react 2h at temperature 80 DEG C, treats that feed liquid is cooled to 50 DEG C of centrifugations and obtains the first mother liquor and described ammonium potassium dihydrogen phosphate crystal 680kg;
C, the first mother liquor is put into crystallizer, continue to add Repone K 100kg and stirring and dissolving in the first mother liquor, the industrial phosphoric acid 150kg adding 85% again regulates material liquid pH to 3.8 ~ 4.2 in temperature 50 C reaction 1 ~ 2h, continues to be cooled to 20 DEG C of centrifugations and obtains the second mother liquor and described ammonium potassium dihydrogen phosphate crystal 1120kg;
D, by the second mother liquor and fertilizer grade primary ammonium phosphate and water stirring and dissolving under temperature 60 C, wherein the solid-to-liquid ratio of fertilizer grade primary ammonium phosphate and the second mother liquor and water is 1:3, repeats above-mentioned steps A ~ C.
By the saturated ammonium potassium dihydrogen phosphate solution washing at least twice of ammonium potassium dihydrogen phosphate crystal obtained, then after centrifuge dehydration, at temperature 80 ~ 100 DEG C, drying obtains ammonium potassium dihydrogen phosphate product, and wherein in product, the effective content of ammonium potassium dihydrogen phosphate is 99.1%.After washing, the fertilizer grade primary ammonium phosphate of mother liquor and steps A and water mix.
Embodiment 2:
The step that ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate is as follows:
A, by 1000kg fertilizer grade primary ammonium phosphate and 3000kg water at temperature 100 DEG C in dissolving tank stirring and dissolving, dissolving the time of stirring is 0.5h, then flame filter press collecting by filtration first filtrate is used, first filtrate is placed in settling bath, in the first filtrate, add 25% ammoniacal liquor regulate pH to 4 ~ 5, then plate and frame filter collecting by filtration second filtrate is used, second filtrate is placed in settling bath, in the second filtrate, add 25% ammoniacal liquor regulate pH to 7 ~ 8, then use plate and frame filter collecting by filtration the 3rd filtrate;
B, the 3rd filtrate is placed in crystallizer, solid potassium chloride 480kg is added and stirring and dissolving in the 3rd filtrate, industrial phosphoric acid 700 ~ the 750kg adding 85% again regulates material liquid pH to 4.0 ~ 4.5 to react 2 ~ 4h at temperature 80 DEG C, treats that feed liquid is cooled to 45 ~ 50 DEG C of centrifugations and obtains the first mother liquor and described ammonium potassium dihydrogen phosphate crystal 675kg;
C, the first mother liquor is placed in crystallizer, continue to add Repone K 100kg and stirring and dissolving in the first mother liquor, the phosphoric acid adding 85% again regulates material liquid pH to 3.8 ~ 4.2 in temperature 45 C reaction 1 ~ 2h, continues to be cooled to 20 DEG C of centrifugations and obtains the second mother liquor and described ammonium potassium dihydrogen phosphate crystal 1155kg;
D, the second mother liquor to be back in dissolving tank the stirring and dissolving at temperature 100 DEG C with 1000kg fertilizer grade primary ammonium phosphate and water, wherein the total mass of the second mother liquor and water is 3000kg, then flame filter press collecting by filtration the 4th filtrate is used, 4th filtrate is placed in settling bath, in the 4th filtrate, add 25% ammoniacal liquor regulate pH to 4 ~ 5, then plate and frame filter collecting by filtration the 5th filtrate is used, in the 5th filtrate, add 25% ammoniacal liquor regulate pH to 7 ~ 8, then use plate and frame filter collecting by filtration the 6th filtrate;
E, the 6th filtrate is cooled to 18 ~ 20 DEG C, centrifugation obtains the 7th filtrate and solid by-product ammonium chloride 190kg;
F, in the 7th filtrate, add Repone K and stirring and dissolving, repeat above-mentioned step B ~ E.
By the saturated ammonium potassium dihydrogen phosphate solution washing at least twice of ammonium potassium dihydrogen phosphate crystal obtained, then after centrifuge dehydration, at temperature 80 ~ 100 DEG C, drying obtains ammonium potassium dihydrogen phosphate product, and wherein in product, the effective content of ammonium potassium dihydrogen phosphate is 99.2%.After washing, the fertilizer grade primary ammonium phosphate of mother liquor and steps A and water mix.
Claims (5)
1. a method for ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate, it is characterized in that the step of the method is as follows:
A, by fertilizer grade primary ammonium phosphate and water by solid-to-liquid ratio 1:2 ~ 1:3 stirring and dissolving at temperature 60 ~ 100 DEG C, then flame filter press collecting by filtration first filtrate is used, in the first filtrate, add 25% ammoniacal liquor regulate pH to 4 ~ 5, then plate and frame filter collecting by filtration second filtrate is used, in the second filtrate, add 25% ammoniacal liquor regulate pH to 7 ~ 8, then use plate and frame filter collecting by filtration the 3rd filtrate;
B, in the 3rd filtrate, add solid potassium chloride and stirring and dissolving, the phosphoric acid adding 85% again regulates material liquid pH to 4.0 ~ 4.5 reaction 2 ~ 4h at temperature >=80 DEG C, treats that feed liquid is cooled to 45 ~ 50 DEG C of centrifugations and obtains the first mother liquor and described ammonium potassium dihydrogen phosphate crystal;
C, continue to add Repone K and stirring and dissolving in the first mother liquor, then the phosphoric acid adding 85% regulates material liquid pH to 3.8 ~ 4.2, continue to be cooled to 18 ~ 25 DEG C, centrifugation obtains the second mother liquor and described ammonium potassium dihydrogen phosphate crystal;
D, by the second mother liquor and fertilizer grade primary ammonium phosphate and water stirring and dissolving at temperature 60 ~ 100 DEG C, wherein the solid-to-liquid ratio of fertilizer grade primary ammonium phosphate and the second mother liquor and water is 1:2 ~ 1:3, repeats above-mentioned steps A ~ C.
2. the method for ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate according to claim 1, it is characterized in that the step of the method is as follows:
A, by fertilizer grade primary ammonium phosphate and water by solid-to-liquid ratio 1:2 ~ 1:3 stirring and dissolving at temperature 60 ~ 100 DEG C, then flame filter press collecting by filtration first filtrate is used, in the first filtrate, add 25% ammoniacal liquor regulate pH to 4 ~ 5, then plate and frame filter collecting by filtration second filtrate is used, in the second filtrate, add 25% ammoniacal liquor regulate pH to 7 ~ 8, then use plate and frame filter collecting by filtration the 3rd filtrate;
B, in the 3rd filtrate, add solid potassium chloride and stirring and dissolving, the phosphoric acid adding 85% again regulates material liquid pH to 4.0 ~ 4.5 reaction 2 ~ 4h at temperature >=80 DEG C, treats that feed liquid is cooled to 45 ~ 50 DEG C of centrifugations and obtains the first mother liquor and described ammonium potassium dihydrogen phosphate crystal;
C, continue to add Repone K and stirring and dissolving in the first mother liquor, then the phosphoric acid adding 85% regulates material liquid pH to 3.8 ~ 4.2, continues to be cooled to 18 ~ 25 DEG C of centrifugations and obtains the second mother liquor and described ammonium potassium dihydrogen phosphate crystal;
D, by the second mother liquor and fertilizer grade primary ammonium phosphate and water stirring and dissolving at temperature 60 ~ 100 DEG C, wherein the solid-to-liquid ratio of fertilizer grade primary ammonium phosphate and the second mother liquor and water is 1:2 ~ 1:3, then flame filter press collecting by filtration the 4th filtrate is used, in the 4th filtrate, add 25% ammoniacal liquor regulate pH to 4 ~ 5, then plate and frame filter collecting by filtration the 5th filtrate is used, in the 5th filtrate, add 25% ammoniacal liquor regulate pH to 7 ~ 8, then use plate and frame filter collecting by filtration the 6th filtrate;
E, the 6th filtrate is cooled to 18 ~ 20 DEG C, centrifugation obtains the 7th filtrate and solid by-product ammonium chloride;
F, in the 7th filtrate, add Repone K and stirring and dissolving, repeat above-mentioned step B ~ E.
3. the method for ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate according to claim 1 and 2, it is characterized in that the saturated ammonium potassium dihydrogen phosphate solution washing at least twice of described ammonium potassium dihydrogen phosphate crystal, then dry at temperature 80 ~ 100 DEG C after centrifuge dehydration, after washing, the fertilizer grade primary ammonium phosphate of mother liquor and steps A and water mix.
4. the method for ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate according to claim 1 and 2, it is characterized in that the mol ratio of solid potassium chloride and fertilizer grade primary ammonium phosphate in described step B is 0.5 ~ 0.8:1.
5. the method for ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate according to claim 1 and 2, it is characterized in that in described step C, in Repone K and step B, solid potassium chloride mass ratio is 1 ~ 2:10.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410604033.7A CN104386664B (en) | 2014-10-30 | 2014-10-30 | The method of ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410604033.7A CN104386664B (en) | 2014-10-30 | 2014-10-30 | The method of ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104386664A CN104386664A (en) | 2015-03-04 |
| CN104386664B true CN104386664B (en) | 2016-02-17 |
Family
ID=52604646
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410604033.7A Active CN104386664B (en) | 2014-10-30 | 2014-10-30 | The method of ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104386664B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107720713B (en) * | 2017-10-29 | 2020-11-20 | 贵阳开磷化肥有限公司 | Method for preparing ammonium dihydrogen phosphate and co-producing potassium dihydrogen phosphate by wet-process phosphoric acid |
| CN113024284B (en) * | 2020-12-03 | 2022-10-11 | 天津大学 | Method for preparing nitrogen-phosphorus-potassium compound fertilizer by fertilizer-grade phosphoric acid eutectic |
| CN112607718A (en) * | 2021-01-25 | 2021-04-06 | 瓮福（集团）有限责任公司 | Production method of fertilizer-grade potassium dihydrogen phosphate |
| CN115490541B (en) * | 2022-11-22 | 2023-06-23 | 云南缁磷工业技术有限公司 | Method for continuously producing ammonium potassium phosphate |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1070901A (en) * | 1992-09-26 | 1993-04-14 | 简阳县农业生产资料公司 | A kind of production technique of potassium-ammonium phosphate |
| CN1083034A (en) * | 1992-07-13 | 1994-03-02 | 成都科技大学 | The production method of ammonium potassium dihydrogen phosphate |
| RU2103348C1 (en) * | 1994-10-10 | 1998-01-27 | Акционерное общество открытого типа "Невинномысский Азот" | Method of potassium-ammonium-phosphate solution producing |
| CN103011122A (en) * | 2012-12-28 | 2013-04-03 | 山东金正大生态工程股份有限公司 | Method for producing water-soluble potassium ammonium phosphate from wet-process phosphoric acid |
-
2014
- 2014-10-30 CN CN201410604033.7A patent/CN104386664B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1083034A (en) * | 1992-07-13 | 1994-03-02 | 成都科技大学 | The production method of ammonium potassium dihydrogen phosphate |
| CN1070901A (en) * | 1992-09-26 | 1993-04-14 | 简阳县农业生产资料公司 | A kind of production technique of potassium-ammonium phosphate |
| RU2103348C1 (en) * | 1994-10-10 | 1998-01-27 | Акционерное общество открытого типа "Невинномысский Азот" | Method of potassium-ammonium-phosphate solution producing |
| CN103011122A (en) * | 2012-12-28 | 2013-04-03 | 山东金正大生态工程股份有限公司 | Method for producing water-soluble potassium ammonium phosphate from wet-process phosphoric acid |
Non-Patent Citations (1)
| Title |
|---|
| 磷酸二氢钾铵无氯复肥的研制;林治华;《渝州大学学报（自然科学版）》;19921231(第4期);第21-26页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104386664A (en) | 2015-03-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105036852B (en) | Utilize the method for industrial grade monoammonium phosphate mother liquor production a great number of elements water-soluble fertilizer | |
| CN104326771B (en) | A kind of method utilizing phosphorus mine tailing to prepare calcium nitrate fertiliser containing magnesium | |
| CN104355326B (en) | Thermal circulation technology of utilizing sodium sulfate solution or carrier to cogenerate sodium carbonate and ammonium sulfate | |
| CN103803518A (en) | Method for preparing monopotassium phosphate by using wet-process phosphoric acid | |
| CN104386664B (en) | The method of ammonium potassium dihydrogen phosphate produced by fertilizer grade primary ammonium phosphate | |
| CN102701868A (en) | Modified glutamic acid fertilizer synergist and production method and application thereof | |
| CN105600763B (en) | A kind of method that fluoride salt method of purification produces industrial monoammonium phosphate | |
| CN102633382B (en) | 4,6-dichloropyrimidine waste water treatment and resource recovery method | |
| CN103011122B (en) | Method for producing water-soluble potassium ammonium phosphate from wet-process phosphoric acid | |
| CN104477943A (en) | Method for preparing potassium sulfate | |
| CN104744175A (en) | Method for producing nitrogen-phosphorus-potassium mixed fertilizer by utilizing phosphorus-potassium associated ore | |
| CN102126742A (en) | Method for producing chloride-based compound fertilizer and co-producing gypsum through decomposing phosphorite with hydrochloric acid | |
| CN105712388B (en) | Nitro-compound fertilizer and industrial potassium nitrate coproduction method | |
| CN104230448A (en) | Method for preparing N-P-K (Nitrogen-Phosphorus-Potassium) compound fertilizer by using hydrochloric acid to decompose phosphorite acidified solution | |
| CN103159195A (en) | Method for preparing potassium dihydrogen phosphate from low-concentration wet-process phosphoric acid | |
| CN107746045B (en) | A method of PHOSPHORIC ACID TECH.GRADE potassium dihydrogen is produced using agricultural monoammonium phosphate | |
| CN100441502C (en) | Method of classification utilizing wet-process phosphoric acid | |
| CN105000539A (en) | Method for producing potassium dihydrogen phosphate and potassium-ammonium dihydrogen phosphate through wet process phosphoric acid | |
| CN105480959A (en) | Method for producing monopotassium phosphate by fluoride salt purification process | |
| CN101380062B (en) | Method for producing feedstuff calcium hydrogen phosphate by decomposition of medium-low grade phosphate ore using hydrochloric acid | |
| CN106430132A (en) | Method for preparing monopotassium phosphate and co-product ammonium sulfate by circulation method | |
| CN104261374B (en) | A kind of production method preparing primary ammonium phosphate by-product Radix Astragali special fertilizer | |
| CN102766157A (en) | Method for producing technical-grade fosetyl-aluminum | |
| CN102442655B (en) | Method for preparing potassium dihydrogen phosphate with phosphorus recovery product in sewage | |
| CN104944397B (en) | A kind of technique that potassium dihydrogen phosphate is prepared by purification of wet process phosphoric acid low cost |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20161027 Address after: 200120 Shanghai city Pudong New Area Lvke Road No. 90 Patentee after: Shanghai Ding Ding Industrial Technology Co., Ltd. Address before: 610000 B District, Xinjin Industrial Park, Xinjin County, Chengdu, Sichuan Patentee before: Chengdu Chemical Co., Ltd. |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20161228 Address after: 200120 Shanghai city Pudong New Area Lvke Road No. 90 Patentee after: Shanghai new tripod Data Technology Co., Ltd. Address before: 200120 Shanghai city Pudong New Area Lvke Road No. 90 Patentee before: Shanghai Ding Ding Industrial Technology Co., Ltd. |