CN102963874A - Method for producing industrial-grade potassium dihydrogen phosphate (KH2PO4) by wet method purified phosphoric acid and potassium sulfate - Google Patents
Method for producing industrial-grade potassium dihydrogen phosphate (KH2PO4) by wet method purified phosphoric acid and potassium sulfate Download PDFInfo
- Publication number
- CN102963874A CN102963874A CN2012104873489A CN201210487348A CN102963874A CN 102963874 A CN102963874 A CN 102963874A CN 2012104873489 A CN2012104873489 A CN 2012104873489A CN 201210487348 A CN201210487348 A CN 201210487348A CN 102963874 A CN102963874 A CN 102963874A
- Authority
- CN
- China
- Prior art keywords
- phosphoric acid
- potassium dihydrogen
- potassium sulfate
- potassium
- market
- 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.)
- Granted
Links
Images
Abstract
The invention discloses a method for producing industrial-grade potassium dihydrogen phosphate (KH2PO4) by wet method purified phosphoric acid and potassium sulfate, belonging to the field of phosphorus chemical industry. The method comprises the following steps: a. adding potassium sulfate in wet method purified phosphoric acid and fully dissolving potassium sulfate, wherein the addition amount of potassium sulfate based on mole ratio is that p:K is 0.6-1.2:1; b, adding calcium carbonate slurry with solid content of 50-90% in the solution obtained from the step a, stirring for reaction, wherein the reaction temperature is controlled to 60-90 DEG C, the addition amount of the calcium carbonate slurry based on mole ratio is that Ca:S is 0.6-1.2; c. filtering a mixed material system which is obtained by the reaction in the step b; and d. adjusting the pH value of the filtrate obtained from the step c to 4-5, and then concentrating and crystallizing, thus obtaining the potassium dihydrogen phosphate product. The method is simple in process, easy to control and industrially apply, low in cost and high in yield; and the yield of P2O5 can be up to over 96% and the yield of K2O can be up to over 98%.
Description
Technical field
The invention belongs to the phosphorous chemical industry field, be specifically related to a kind of method with Wet Phosphoric Acid Market and potassium sulfate production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen.
Background technology
Phosphate industry is a large branch of chemical industry, KH
2P0
4It is the staple product of phosphate industry.The pure phosphoric acid potassium dihydrogen contains potassium oxide (K
2O) 34.6%, Vanadium Pentoxide in FLAKES (P
2O
5) 52.2%.Potassium primary phosphate (KH
2PO
4) be a kind of colourless or white rhomboidal crystal with gloss, can be water-soluble, react acid, be insoluble to alcohol.Because its special character, potassium primary phosphate is a kind of important chemical goods, has a wide range of applications in industries such as agricultural, industry, food, medicine.
1821, potassium primary phosphate was produced out first, and it is by phosphoric acid and solution of potassium carbonate neutralization reaction to occur at first, and then crystallization obtains.Originally, prepare in this way potassium primary phosphate, just as theoretical investigation, be not used for commercial use.Until eighties of last century sixties, countries in the world just begin the theoretical basis of its process and technique are carried out deep research, have proposed several production technique, such as neutralisation, KCl and phosphoric acid high temperature double decomposition, ion exchange method, solvent extration etc.
At present, main method and the quality thereof of production potassium primary phosphate have following:
1, neutralisation: in the enterprise of existing potassium primary phosphate, most of neutralisation technique that adopts, this method technical process is simple, technology maturation, facility investment is few, stable and reliable product quality, but take thermal phosphoric acid and potassium hydroxide as raw material, expensive, production cost is too high, makes its use range be subject to certain limitation.
2, Repone K high temperature double decomposition: owing to be take KCl as raw material, therefore have certain cost advantage, but the production process heat exhaustion is very large, equipment corrosion is serious, also can cause quality product relatively poor because of side reaction.
3, the solvent extration technical process is simple, and scale is changeable, reacts under the low temperature, and equipment corrosion is little, and cost is low, pollutes without " three wastes ", and shortcoming is that organic solvent is expensive, now still has the loss of solvent and the problem of inactivation to fail to be solved well.
4, conversion method: transform Repone K with PHOSPHORIC ACID TECH.GRADE, obtain potassium primary phosphate, by-product hydrochloric acid, this method temperature of reaction is high, and corrosion protection of equipment is difficult to reach a standard.
5, ion exchange method: utilize ion exchange resin respectively to H
2PO
4 -And K
+The absorption and regeneration process generate potassium primary phosphate, the disadvantage of this production method is that the water yield of evaporation is too large, energy consumption is too high.
6, direct method: directly using ground phosphate rock, sulfuric acid and KCl production potassium primary phosphate, is that early seventies is carried on by Irish Ge Erding company and Yi Er company of this family of the U.S..The greatest problem of this method is that the ground phosphate rock fluorine content is high, generates the potassium silicofluoride of indissoluble in the reaction process, adds to generate a part of syngenite, and the loss of potassium reaches more than 20%, can't reach a standard economically.Also because ground phosphate rock impurity is many, cause potassium primary phosphate of poor quality.
Because aforesaid method drawback separately, up to the present, also there is not fairly large production line, cause on the market potassium primary phosphate source of goods in short supply, product price is always high.The applicant is according to practical situation, developed that (Wet Phosphoric Acid Market is with strong acid and phosphorus ore direct reaction with Wet Phosphoric Acid Market, because its foreign matter content is high, so also through decolouring, extraction treatment, make behind the impurity reduction content) be raw material, the potassium hydroxide that adopts vitriolate of tartar to substitute high price carries out the production technique of potassium primary phosphate.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method with Wet Phosphoric Acid Market and potassium sulfate production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen, and the method production cost is low, yield is high, be easy to industrial applications.
The technical solution adopted for the present invention to solve the technical problems is: the method with Wet Phosphoric Acid Market and potassium sulfate production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen is characterized in that comprising the steps:
A, add vitriolate of tartar in the Wet Phosphoric Acid Market it is dissolved fully, the add-on of vitriolate of tartar is counted in molar ratio: P ︰ K=0.6～1.2 ︰ 1;
B, be that 50～90% calcium carbonate slip joins stirring reaction in the solution of step a gained with solid content, the control temperature of reaction is 60～90 ℃, and the add-on of calcium carbonate slip is counted in molar ratio: Ca ︰ S=0.6～1.2 ︰ 1;
C, the mixture system that obtains after the step b reaction is filtered, obtain filtrate and filter cake; Filter cake is the byproduct phosphogypsum through washing;
D, the filtrate of step c gained is regulated pH value to 4～5 with potassium hydroxide aqueous solution or Wet Phosphoric Acid Market, then condensing crystal makes potassium dihydrogen phosphate product.
Wherein, among the aforesaid method step a, the temperature of dissolving when adding vitriolate of tartar in the Wet Phosphoric Acid Market is 70～80 ℃, is incubated 5～10 minutes after the dissolving again.
Wherein, among the aforesaid method step a, the add-on of vitriolate of tartar is counted in molar ratio: P ︰ K=1.05～1.15 ︰ 1.
Wherein, among the aforesaid method step b, the calcium carbonate slip is joined the temperature of reacting in the solution of step a gained be controlled at 70～80 ℃.
Wherein, among the aforesaid method step b, the add-on of calcium carbonate slip is counted in molar ratio: Ca ︰ S=0.8～1.1 ︰ 1.
Wherein, gained filtrate is also processed through sedimentation among the aforesaid method step c, makes not filter thoroughly close grain sedimentation in the filtrate and remove.
Further, the settling time is 12～24 hours.
Wherein, in the aforesaid method steps d, step c gained filtrate is regulated pH value to 4.2～4.7.
Wherein, in the aforesaid method steps d, the concrete steps of condensing crystal are: will regulate filtrate after the pH value and send into vacuum vaporation system and concentrate, control slip proportion is 1.40～1.45, then be cooled to 30～40 ℃ and separate out potassium dihydrogen phosphate crystal, make potassium dihydrogen phosphate product through centrifugation, oven dry again.
The invention has the beneficial effects as follows: the present invention is take Wet Phosphoric Acid Market and cheap vitriolate of tartar as raw material, and the Wet Phosphoric Acid Market foreign matter content is low, can reduce the loss of phosphorus in the production process, and vitriolate of tartar instead of hydrogen potassium oxide reduces cost as raw material.Simultaneously, the present invention allows first vitriolate of tartar be dissolved in fully in the phosphoric acid, and it is existed with ionic condition, participate in again reaction after the calcium carbonate slurrying, can so that reaction is more thorough, avoid wrapping up phenomenon, and the calcium carbonate meeting is preferential and the sulfate radical reaction, generates the calcium sulfate of indissoluble, has suppressed CaHPO
42H
2The generation of O has further reduced the loss of phosphorus.And the present invention strictly controls processing parameter, can obtain the dihydrate gypsum that particle is thick, be easy to separate, and also can improve the yield of Vanadium Pentoxide in FLAKES.Therefore, production process of the present invention simple, be easy to control and industrial applications, with low cost, yield is high, P
2O
5Yield can reach more than 96%, K
2The O yield can reach more than 98%.
Description of drawings
Fig. 1 is the process flow diagram of the specific embodiment of the invention, and KDP is potassium primary phosphate.
Embodiment
The present invention selects the Wet Phosphoric Acid Market operational path, be conceived to use the raw material of relative low price, adopt relatively gentle reaction conditions also to make every effort to higher yield, provide a kind of practical, can be mass-produced, the production method of economic potassium primary phosphate again.Production process mainly contain moltenly join, slurrying desulfurization, filtration and the washing of slag, the steps such as condensing crystal of the stillness of night.
1, molten joining
Wet Phosphoric Acid Market is added in the reactor with heating unit, start agitator and be warming up to 70～80 ℃; This temperature is for vitriolate of tartar can better be dissolved, and temperature is excessively low, and vitriolate of tartar can not dissolve fully.
Vitriolate of tartar is the mol ratio adding reactor (preferred P ︰ K=1.05～1.15 ︰ 1) of 0.6～1.2 ︰ 1 by P ︰ K, and vitriolate of tartar dissolved rear insulation reaction 5～10 minutes fully, obtained one and contained K
+, PO
4 3-, SO
4 2+Isoionic mixing solutions.And the insulation after the vitriolate of tartar dissolving is all to exist with ionic condition in order to ensure each component in the slip, reduces parcel and entrainment loss in the follow-up pulping process.
H
3PO
4+K
2SO
4=2K
++PO
4 3-+SO
4 2++3H
+
2, slurrying desulfurization
(1) at first the high-quality calcium carbonate powders being added water, to make solid content be 50%～90% slip, and required moisture comes from the slag washing water of subsequent handling;
(2) slip is slowly added in the 1 resulting clear solution, constantly stir slip, guarantee that removal of bubbles is thorough.The add-on of calcium carbonate.
The add-on of calcium carbonate is pressed the SO in Ca ion and the slip
4 2-Radiometer, i.e. the ratio of Ca and S, experiment shows, when the calcium carbonate that adds bring into Ca and the molar ratio of S when being 0.6～1.2, sweetening effectiveness is good, most preferably 0.8～1.1.If this place's calcium carbonate add-on deficiency can cause SO in the slip
4 2-Content is higher, affects product master content; And calcium carbonate adds too much, then unnecessary Ca will with the phosphoric acid combination, form calcium phosphate salt, separate out with the form of precipitation, affect P
2O
5Yield.
(3) the Controlling System temperature of reaction is 60～90 ℃, and preferred 70～80 ℃, guarantee that gypsum produces two water crystallization things, particle is thick; 30 minutes reaction times was advisable.
Principal reaction has:
CaCO
3+SO
4 2++H
+=CaSO
4↓+CO
2↑+H
2O
Process also can be followed certain side reaction simultaneously, and along with the gradually adding of calcium carbonate, pH constantly rises, the Fe of trace in the purifying phosphoric acid
3+, A1
3+, Mg
2+, F
-, S0
4 2-Can be with CaS0 Deng impurity
42H
20, CaF
2, A1P0
4, FeP0
4Form Deng salt is precipitated out.In this process, be difficult to avoid having the phosphorus of part with Ca (H
2PO
4)
2Form separate out, cause P
2O
5Loss.
3, the washing of filtration and slag
(1) slip after reaction is finished pumps into filter equipment and filters.This filter plant can be the band filter, also can be plate-and-frame filter press;
(2) the gained clear liquid enters subsider, can slowly stir in the subsider, makes in the stillness of night to filter thoroughly thin brilliant again crystallization and precipitate with the form of postprecipitation salt.Settling time is 12～24 hours, and the clear liquid foreign matter content after the sedimentation can be down to below 1%;
(3) contain a certain amount of P in the filter residue
2O
5And K
2The useful components such as O need to guarantee P wherein through secondary washing
2O
5Content is down to below 0.5%.The gypsum tailings of high-quality can be used as building materials, mould etc. and directly uses.
The residue washing water water yield: a wash water add-on: be preferably 1 times of the quantity of slag.
Two wash water add-ons: be preferably 0.5 times of the quantity of slag.
4, the accurate adjustment of clear liquid and condensing crystal
The sedimentation clear liquid of above-mentioned (2) gained is adjusted to 4～5 with its pH value, preferred 4.2～4.7 with potassium hydroxide aqueous solution or Wet Phosphoric Acid Market; It is concentrated to pump into vacuum vaporation system again, and control slip proportion is 1.40～1.45.Slip pH value is low herein can cause part P
2O
5Still the form with phosphoric acid exists, can't crystallization, and then affect P
2O
5Yield; Slip pH value height can cause having the part dipotassium hydrogen phosphate to generate, thereby causes product master content defective.
Be cooled to 30～40 ℃ and separate out the potassium primary phosphate crystallization, selecting this temperature is because if excess Temperature, then can't so that the potassium dihydrogen product enough separate out, and temperature crosses that although low single crystallization yield has improved but industrially to drop to lower temperature and need long time, force in addition the required energy consumption of cooling also better, the waste energy consumption; Through centrifugation, oven dry, make potassium dihydrogen phosphate product again.
Below by embodiment the specific embodiment of the present invention is further described, but therefore protection scope of the present invention is not limited among the embodiment.
Embodiment one
This example P ︰ K mol ratio=0.6 ︰ 1, Ca ︰ SO
4Mol ratio=0.8 ︰ 1, each component concentration is as shown in table 1 in the used Wet Phosphoric Acid Market:
Table 1 Wet Phosphoric Acid Market indices
| Project | P 2O 5 | Fe | As | Mg | F | SO 4 |
| Index/% | 20.12 | 0.0097 | 0.0014 | 0.03 | 0.0054 | 0.19 |
Test used vitriolate of tartar, potassium hydroxide, calcium carbonate and be analytical pure, main content is more than 98;
(1) molten joining
Taking by weighing the 1000g Wet Phosphoric Acid Market adds in the reactor with heating unit, start agitator and be warming up to 70～80 ℃, take by weighing again vitriolate of tartar 420g and add dissolving, be incubated after the entry to be completely 5～10 minutes, guarantee to dissolve fully, and each component all exists with ionic species;
(2) slurrying desulfurization
Take by weighing high-quality calcium carbonate powders 192.8g, add the slurrying of 128.5g water, be configured to solid content and be about 60% calcium carbonate slip;
Slip is slowly added in the 1 resulting clear solution, constantly stir slip, guarantee that removal of bubbles is thorough.
70～80 ℃ of Controlling System temperature of reaction guarantee that gypsum produces two water crystallization things, and particle is thick; Reaction times is 30 minutes;
Obtain slip 1525.1g.
(3) washing of filtration and slag
Slip after reaction is finished carries out suction filtration, obtains filtrate 1164g, filter residue 361g;
The gained clear liquid is placed clarification in the place, cool place, and clear liquid pH value is 5.3;
Filter cake is plasm scouring more all, and the bath water amount is 361g, behind the suction filtration filter residue 342g filtrate 380g;
The whole secondaries of filter cake are plasm scouring again, and the bath water amount is 171g, the filter residue 324g of suction filtration, filtrate 189g;
Washings returns pulping system, contains P in the slag
2O
5Be that 0.9%, K2O is 0.4%.
(4) accurate adjustment of clear liquid and condensing crystal
Get (3) gained clear liquor, add secondary wet process purifying phosphoric acid 666.76g; Recording KDP slip pH value is 4.32, to its condensing crystal, gets concentrated solution 825.1g, slip proportion 1.40.Get KDP crystallization 550g through the cooling down Crystallization Separation, crystalline mother solution 226g, sample presentation analysed preparation quality sees Table 2 after the oven dry.The P of system as calculated
2O
5Transformation efficiency (being yield) be 96.4%; System K
2The transformation efficiency of O (being yield) is 98.03%.
Embodiment two
This example P ︰ K mol ratio=1.1 ︰ 1, Ca ︰ SO4 mol ratio=0.9 ︰ 1, Wet Phosphoric Acid Market indices such as table 1.
(1) molten joining
Taking by weighing the 1000g Wet Phosphoric Acid Market adds in the reactor with heating unit, start agitator and be warming up to 70～80 ℃, take by weighing again vitriolate of tartar 229g and add dissolving, be incubated after the entry to be completely 5～10 minutes, guarantee to dissolve fully, and each component all exists with ionic species;
(2) slurrying desulfurization
Take by weighing high-quality calcium carbonate powders 118.31g, add the slurrying of 78.87g water, be configured to solid content and be about 60% calcium carbonate slip;
Slip is slowly added in the 1 resulting clear solution, constantly stir slip, guarantee that removal of bubbles is thorough.
70～80 ℃ of Controlling System temperature of reaction guarantee that gypsum produces two water crystallization things, and particle is thick; Reaction times is 30 minutes;
Obtain slip 1290g.
(3) washing of filtration and slag
Slip after reaction is finished carries out suction filtration, obtains filtrate 1068g, filter residue 222g.
The gained clear liquid is placed clarification in the place, cool place, and clear liquid pH value is 3.51;
Filter cake is plasm scouring more all, and the bath water amount is 222g, behind the suction filtration filter residue 210g filtrate 234g;
The whole secondaries of filter cake are plasm scouring again, and the bath water amount is 105g, the filter residue 199g of suction filtration, filtrate 116g;
Washings returns pulping system, contains P in the slag
2O
5Be that 0.7%, K2O is 0.4%.
(4) accurate adjustment of clear liquid and condensing crystal
Get (3) gained clear liquor, add potassium hydroxide 11.61g; Recording KDP slip pH value is 4.29, to its condensing crystal, gets concentrated solution 720g, slip proportion 1.40.Get KDP crystallization 251g through the cooling down Crystallization Separation, crystalline mother solution 461g, sample presentation analysed preparation quality sees Table 2 after the oven dry.The P of system as calculated
2O
5Transformation efficiency be 99.1%, system K
2The transformation efficiency of O is 98.7%.
Embodiment three
This example P ︰ K mol ratio=1.2 ︰ 1, Ca ︰ SO4 mol ratio=1.1 ︰ 1, Wet Phosphoric Acid Market indices such as table 1.
(1) molten joining
Taking by weighing the 1000g Wet Phosphoric Acid Market adds in the reactor with heating unit, start agitator and be warming up to 70～80 ℃, take by weighing again vitriolate of tartar 210g and add dissolving, be incubated after the entry to be completely 5～10 minutes, guarantee to dissolve fully, and each component all exists with ionic species;
(2) slurrying desulfurization
Take by weighing high-quality calcium carbonate powders 132.6g, add the slurrying of 88.3g water, be configured to solid content and be about 60% calcium carbonate slip;
Slip is slowly added in the 1 resulting clear solution, constantly stir slip, guarantee that removal of bubbles is thorough.
70～80 ℃ of Controlling System temperature of reaction guarantee that gypsum produces two water crystallization things, and particle is thick; Reaction times is 30 minutes;
Obtain slip 1280g.
(3) washing of filtration and slag
Slip after reaction is finished carries out suction filtration, obtains filtrate 1032g, filter residue 248g.
The gained clear liquid is placed clarification in the place, cool place, and clear liquid pH value is 3.02;
Filter cake is plasm scouring more all, and the bath water amount is 248g, behind the suction filtration filter residue 235g filtrate 261g;
The whole secondaries of filter cake are plasm scouring again, and the bath water amount is 118g, the filter residue 224g of suction filtration, filtrate 129g;
Washings returns pulping system, contains P in the slag
2O
5Be that 0.8%, K2O is 0.4%.
(4) accurate adjustment of clear liquid and condensing crystal
Get (3) gained clear liquor, add potassium hydroxide 21.29g; Recording KDP slip pH value is 4.40, to its condensing crystal, gets concentrated solution 688g, slip proportion 1.41.Get KDP crystallization 256g through the cooling down Crystallization Separation, crystalline mother solution 275.1g, sample presentation analysed preparation quality sees Table 2 after the oven dry.The P of system as calculated
2O
5Transformation efficiency be 99.1%, system K
2The transformation efficiency of O is 99.8%.
Each embodiment product index of table 2
P in the byproduct phosphogypsum among the embodiment one, two and three
2O
5Content be respectively 0.9%, 0.7%, 0.7%; K
2The content of O is respectively 0.4%, 0.3%, 0.5%; Because phosphoric acid by wet process has passed through the primary purification processing, does not detect other foreign ions, CaSO
4Main content reaches more than 90%, and quality is more excellent.
By embodiment as can be known, the present invention is by reasonable disposition principle, control technological process and parameter, so that P
2O
5Yield can reach more than 96%, K
2The O yield can reach more than 98%, and product potassium primary phosphate and phosphogypsum foreign matter content are few, and quality is high, and technological process is simple, is easy to industrial applications.
Claims (9)
1. with the method for Wet Phosphoric Acid Market and potassium sulfate production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen, it is characterized in that comprising the steps:
A, add vitriolate of tartar in the Wet Phosphoric Acid Market it is dissolved fully, the add-on of vitriolate of tartar is counted in molar ratio: P ︰ K=0.6～1.2 ︰ 1;
B, be that 50～90% calcium carbonate slip joins stirring reaction in the solution of step a gained with solid content, the control temperature of reaction is 60～90 ℃, and the add-on of calcium carbonate slip is counted in molar ratio: Ca ︰ S=0.6～1.2 ︰ 1;
C, the mixture system that obtains after the step b reaction is filtered, obtain filtrate and filter cake; Filter cake is the byproduct phosphogypsum through washing;
D, the filtrate of step c gained is regulated pH value to 4～5 with potassium hydroxide aqueous solution or Wet Phosphoric Acid Market, then condensing crystal makes potassium dihydrogen phosphate product.
2. the method with Wet Phosphoric Acid Market and potassium sulfate production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen according to claim 1, it is characterized in that: among the step a, the temperature of dissolving when adding vitriolate of tartar in the Wet Phosphoric Acid Market is 70～80 ℃, is incubated 5～10 minutes after the dissolving again.
3. the method with Wet Phosphoric Acid Market and potassium sulfate production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen according to claim 1, it is characterized in that: among the step a, the add-on of vitriolate of tartar is counted in molar ratio: P ︰ K=1.05～1.15 ︰ 1.
4. the method with Wet Phosphoric Acid Market and potassium sulfate production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen according to claim 1 is characterized in that: among the step b, the calcium carbonate slip is joined the temperature of reacting in the solution of step a gained be controlled at 70～80 ℃.
5. the method with Wet Phosphoric Acid Market and potassium sulfate production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen according to claim 1, it is characterized in that: among the step b, the add-on of calcium carbonate slip is counted in molar ratio: Ca ︰ S=0.8～1.1 ︰ 1.
6. each described method with Wet Phosphoric Acid Market and potassium sulfate production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen in 5 according to claim 1, it is characterized in that: gained filtrate is also processed through sedimentation among the step c, makes not filter thoroughly close grain sedimentation in the filtrate and remove.
7. the method with Wet Phosphoric Acid Market and potassium sulfate production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen according to claim 6, it is characterized in that: the settling time is 12～24 hours.
8. each described method with Wet Phosphoric Acid Market and potassium sulfate production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen in 5 according to claim 1 is characterized in that: in the steps d, step c gained filtrate is regulated pH value to 4.2～4.7.
9. each described method with Wet Phosphoric Acid Market and potassium sulfate production PHOSPHORIC ACID TECH.GRADE potassium dihydrogen in 5 according to claim 1, it is characterized in that: in the steps d, the concrete steps of condensing crystal are: will regulate filtrate after the pH value and send into vacuum vaporation system and concentrate, control slip proportion is 1.40～1.45, then be cooled to 30～40 ℃ and separate out potassium dihydrogen phosphate crystal, make potassium dihydrogen phosphate product through centrifugation, oven dry again.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210487348.9A CN102963874B (en) | 2012-11-26 | 2012-11-26 | Method for producing industrial-grade potassium dihydrogen phosphate (KH2PO4) by wet method purified phosphoric acid and potassium sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210487348.9A CN102963874B (en) | 2012-11-26 | 2012-11-26 | Method for producing industrial-grade potassium dihydrogen phosphate (KH2PO4) by wet method purified phosphoric acid and potassium sulfate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102963874A true CN102963874A (en) | 2013-03-13 |
| CN102963874B CN102963874B (en) | 2015-04-15 |
Family
ID=47794355
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210487348.9A Active CN102963874B (en) | 2012-11-26 | 2012-11-26 | Method for producing industrial-grade potassium dihydrogen phosphate (KH2PO4) by wet method purified phosphoric acid and potassium sulfate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102963874B (en) |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104944397A (en) * | 2015-05-27 | 2015-09-30 | 陈锂 | Low-cost technique for preparing potassium dihydrogen phosphate from purification wet-process phosphoric acid |
| CN105174237A (en) * | 2015-09-22 | 2015-12-23 | 贵州开磷集团股份有限公司 | Method for preparing sodium dihydrogen phosphate by means of phosphoric acid obtained by wet process |
| CN105174239A (en) * | 2015-09-22 | 2015-12-23 | 贵州开磷集团股份有限公司 | Method for preparing disodium hydrogen phosphate by means of phosphoric acid obtained by wet process |
| CN105174238A (en) * | 2015-09-22 | 2015-12-23 | 贵州开磷集团股份有限公司 | Method for preparing dipotassium phosphate by means of phosphoric acid obtained by wet process |
| CN108117054A (en) * | 2017-12-18 | 2018-06-05 | 湖北三宁化工股份有限公司 | A kind of method for preparing potassium dihydrogen phosphate coproduction ammonium potassium dihydrogen phosphate |
| CN109231179A (en) * | 2018-11-28 | 2019-01-18 | 杨新艳 | A kind of potassium dihydrogen phosphate preparation method |
| RU2712689C1 (en) * | 2018-11-29 | 2020-01-30 | Федеральное Государственное Унитарное Предприятие "Институт Химических Реактивов И Особо Чистых Химических Веществ Национального Исследовательского Центра "Курчатовский Институт" (Ниц "Курчатовский Институт" - Иреа) | Method of producing high-purity potassium dihydrophosphate |
| CN110745803A (en) * | 2019-11-25 | 2020-02-04 | 湖北三宁碳磷基新材料产业技术研究院有限公司 | Method for preparing potassium dihydrogen phosphate from wet-process phosphoric acid |
| CN110862074A (en) * | 2019-12-18 | 2020-03-06 | 瓮福（集团）有限责任公司 | Preparation method for producing calcium dihydrogen phosphate slurry by wet-process phosphoric acid slurry method |
| CN112758906A (en) * | 2020-12-31 | 2021-05-07 | 谢坪 | Process for producing potassium dihydrogen phosphate |
| CN113072047A (en) * | 2021-05-25 | 2021-07-06 | 贵州川恒化工股份有限公司 | Production process for continuously preparing monopotassium phosphate |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106430132A (en) * | 2016-11-04 | 2017-02-22 | 湖北三宁化工股份有限公司 | Method for preparing monopotassium phosphate and co-product ammonium sulfate by circulation method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4008307A (en) * | 1975-06-02 | 1977-02-15 | Southwire Company | Production of monobasic potassium phosphate by ion exchange |
| CN85102898A (en) * | 1985-04-01 | 1987-01-17 | 贵州省化工研究所 | The coming of new method of potassium primary phosphate |
| US4885148A (en) * | 1988-09-06 | 1989-12-05 | Phosphate Engineering & Construction Co., Inc. | Production of monobasic potassium phosphate with low chloride content from potassium chloride and phosphoric acid produced from the commercial wet process |
| CN102424374A (en) * | 2011-09-07 | 2012-04-25 | 湖北三宁化工股份有限公司 | Production method of potassium dihydrogen phosphate |
-
2012
- 2012-11-26 CN CN201210487348.9A patent/CN102963874B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4008307A (en) * | 1975-06-02 | 1977-02-15 | Southwire Company | Production of monobasic potassium phosphate by ion exchange |
| CN85102898A (en) * | 1985-04-01 | 1987-01-17 | 贵州省化工研究所 | The coming of new method of potassium primary phosphate |
| US4885148A (en) * | 1988-09-06 | 1989-12-05 | Phosphate Engineering & Construction Co., Inc. | Production of monobasic potassium phosphate with low chloride content from potassium chloride and phosphoric acid produced from the commercial wet process |
| CN102424374A (en) * | 2011-09-07 | 2012-04-25 | 湖北三宁化工股份有限公司 | Production method of potassium dihydrogen phosphate |
Non-Patent Citations (2)
| Title |
|---|
| 左文成: "磷酸二氢钾生产新工艺试验探索", 《湖北化工》 * |
| 雷武: "以湿法磷酸生产磷酸二氢钾", 《无机盐工业》 * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104944397B (en) * | 2015-05-27 | 2019-05-07 | 陈锂 | A kind of technique that potassium dihydrogen phosphate is prepared by purification of wet process phosphoric acid low cost |
| CN104944397A (en) * | 2015-05-27 | 2015-09-30 | 陈锂 | Low-cost technique for preparing potassium dihydrogen phosphate from purification wet-process phosphoric acid |
| CN105174237A (en) * | 2015-09-22 | 2015-12-23 | 贵州开磷集团股份有限公司 | Method for preparing sodium dihydrogen phosphate by means of phosphoric acid obtained by wet process |
| CN105174239A (en) * | 2015-09-22 | 2015-12-23 | 贵州开磷集团股份有限公司 | Method for preparing disodium hydrogen phosphate by means of phosphoric acid obtained by wet process |
| CN105174238A (en) * | 2015-09-22 | 2015-12-23 | 贵州开磷集团股份有限公司 | Method for preparing dipotassium phosphate by means of phosphoric acid obtained by wet process |
| CN105174239B (en) * | 2015-09-22 | 2018-03-13 | 贵州开磷集团股份有限公司 | A kind of phosphoric acid by wet process prepares disodium hydrogen phosphate method |
| CN108117054A (en) * | 2017-12-18 | 2018-06-05 | 湖北三宁化工股份有限公司 | A kind of method for preparing potassium dihydrogen phosphate coproduction ammonium potassium dihydrogen phosphate |
| CN109231179A (en) * | 2018-11-28 | 2019-01-18 | 杨新艳 | A kind of potassium dihydrogen phosphate preparation method |
| RU2712689C1 (en) * | 2018-11-29 | 2020-01-30 | Федеральное Государственное Унитарное Предприятие "Институт Химических Реактивов И Особо Чистых Химических Веществ Национального Исследовательского Центра "Курчатовский Институт" (Ниц "Курчатовский Институт" - Иреа) | Method of producing high-purity potassium dihydrophosphate |
| CN110745803A (en) * | 2019-11-25 | 2020-02-04 | 湖北三宁碳磷基新材料产业技术研究院有限公司 | Method for preparing potassium dihydrogen phosphate from wet-process phosphoric acid |
| CN110862074A (en) * | 2019-12-18 | 2020-03-06 | 瓮福（集团）有限责任公司 | Preparation method for producing calcium dihydrogen phosphate slurry by wet-process phosphoric acid slurry method |
| CN112758906A (en) * | 2020-12-31 | 2021-05-07 | 谢坪 | Process for producing potassium dihydrogen phosphate |
| CN113072047A (en) * | 2021-05-25 | 2021-07-06 | 贵州川恒化工股份有限公司 | Production process for continuously preparing monopotassium phosphate |
| CN113072047B (en) * | 2021-05-25 | 2023-03-10 | 贵州川恒化工股份有限公司 | Production process for continuously preparing monopotassium phosphate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102963874B (en) | 2015-04-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102963874B (en) | Method for producing industrial-grade potassium dihydrogen phosphate (KH2PO4) by wet method purified phosphoric acid and potassium sulfate | |
| CN103496685B (en) | The method of continuous seepage calcium hydrophosphate fodder | |
| CN103787293A (en) | Method for preparing sodium dihydrogen phosphate by utilizing phosphoric acid by wet process | |
| CN105600763B (en) | A kind of method that fluoride salt method of purification produces industrial monoammonium phosphate | |
| CN101337657A (en) | Process for disassembling phosphate ore by mixed acid and coproducing potassium dihydrogen phosphate, hydrogen phosphate and combined fertilizer | |
| CN103011122B (en) | Method for producing water-soluble potassium ammonium phosphate from wet-process phosphoric acid | |
| CN102126738A (en) | Method for producing nitrophosphate fertilizer and co-producing gypsum through decomposing phosphorite with nitric acid | |
| CN100503440C (en) | Process of preparing potassium sulfate with potassium containing bittern of magnesium sulfate subtype | |
| CN102126737A (en) | Method for producing nitrate-and-sulfur-based compound fertilizer and co-producing gypsum by utilizing potassium hydrogen sulfate | |
| CN101348244A (en) | Preparation of ammonium potassium dihydrogen phosphate | |
| CN103073041A (en) | Method for producing water-soluble calcium nitrate dihydrate and phosphoric acid by decomposing phosphorite through nitric acid | |
| CN104016324A (en) | Production method for tripotassium phosphate | |
| CN110395704A (en) | The method of phosphoric acid by wet process coproduction PHOSPHORIC ACID TECH.GRADE potassium dihydrogen and calcium hydrophosphate fodder | |
| CN106744764B (en) | A method of producing potassium dihydrogen phosphate | |
| CN111086977A (en) | Method for preparing MCP and MDCP (Madin-Darby Canine phosphate) by using raffinate acid | |
| CN100441502C (en) | Method of classification utilizing wet-process phosphoric acid | |
| CN1174812A (en) | Industrial monoammonium phosphate and productive method for industrial monoammunium phosphate and calcium hydrogen phosphate fodder | |
| CN100402418C (en) | Hydrochloric acid process of producing feed level calcium diphosphate and gypsum coproduct | |
| CN105293459A (en) | Method for producing fully water-soluble monoammonium phosphate and co-producing ammonium magnesium phosphate by wet process phosphoric acid | |
| CN106430132A (en) | Method for preparing monopotassium phosphate and co-product ammonium sulfate by circulation method | |
| CN103466583A (en) | Method of preparing iron phosphate by using phosphor-iron oxidizing slag | |
| CN108117054A (en) | A kind of method for preparing potassium dihydrogen phosphate coproduction ammonium potassium dihydrogen phosphate | |
| CN111517832B (en) | Separation method of P, Ca in medium-low grade phosphate ore and method for producing fertilizer | |
| CN114314540A (en) | Method for producing magnesium hydrogen phosphate by using phosphate tailings | |
| CN111689875B (en) | Method for producing feed-grade urea phosphate by using wet-process phosphoric acid residues |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| ASS | Succession or assignment of patent right |
Owner name: GUIZHOU CHUANHENG CHEMICAL CO., LTD. Free format text: FORMER OWNER: SICHUAN CHUANHENG CHEMICAL CORPORATION Effective date: 20150217 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 618400 DEYANG, SICHUAN PROVINCE TO: 550500 QIANNAN BUYEI AND MIAO AUTONOMOUS PREFECTURE, GUIZHOU PROVINCE |
|
| TA01 | Transfer of patent application right |
Effective date of registration: 20150217 Address after: 550500 Guizhou Province, Qiannan Buyei and Miao Autonomous Prefecture Fuquan City Longchang town Applicant after: Guizhou Chuanheng Chemical Co., Ltd. Address before: 618400, No. 399 east station, Shifang, Sichuan, Deyang Applicant before: Sichuan Chuanheng Chemical Industry Co., Ltd. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: GUIZHOU CHANHEN CHEMICAL CO., LTD. Free format text: FORMER NAME: GUIZHOU CHUANHENG CHEMICAL CO., LTD. |
|
| CP01 | Change in the name or title of a patent holder |
Address after: 550500 Guizhou Province, Qiannan Buyei and Miao Autonomous Prefecture Fuquan City Longchang town Patentee after: GUIZHOU CHANHEN CHEMICAL CO., LTD. Address before: 550500 Guizhou Province, Qiannan Buyei and Miao Autonomous Prefecture Fuquan City Longchang town Patentee before: Guizhou Chuanheng Chemical Co., Ltd. |