CN104445126A - Coproduction method of anhydrous tripotassium phosphate, crystallographic tripotassium phosphate and calcium phosphate - Google Patents
Coproduction method of anhydrous tripotassium phosphate, crystallographic tripotassium phosphate and calcium phosphate Download PDFInfo
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- CN104445126A CN104445126A CN201410680185.5A CN201410680185A CN104445126A CN 104445126 A CN104445126 A CN 104445126A CN 201410680185 A CN201410680185 A CN 201410680185A CN 104445126 A CN104445126 A CN 104445126A
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Abstract
The invention relates to a coproduction method of anhydrous tripotassium phosphate, crystallographic tripotassium phosphate and calcium phosphate. The method comprises the following steps: (1) preparing a solution with 40-50wt% of potassium hydroxide, and adding a phosphoric acid to the solution to be reacted; (2) thermally filtering the mixture of the solution and the phosphoric acid which are reacted, collecting mother liquid to perform concentration, concentrating the collected mother liquid until a large number of crystallographic films are generated, stopping heating, cooling the concentrated mother liquid, separating out crystallization when the temperature is 50-60 DEG C, performing filtration so as to collect the crystallization and filtrate respectively, spin-drying the crystallization while the crystallization is hot, washing the spin-dried crystallization with a little hot water, and spin-drying the washed crystallization again so as to obtain trihydrate crystallographic tripotassium phosphate; (3) recycling the surplus mother liquid and precipitating the recycled mother liquid with calcium chloride so as to obtain the calcium phosphate. The method disclosed by the invention utilizes same raw materials by a conventional method to produce the anhydrous tripotassium phosphate and the crystallographic tripotassium phosphate, and in other to protect environment, the mother liquid which generates the tripotassium phosphate is recycled as dicalcium phosphate, so that the method not only is environment friendly but also reduces the cost; the anhydrous tripotassium phosphate, the crystallographic tripotassium phosphate and the calcium phosphate are coproduced, so that the cost is saved, and the work efficiency and the economic benefits are improved.
Description
Technical field
The invention belongs to field, especially a kind of anhydrous phosphoric acid tripotassium and crystalline tripotassium, the calcium phosphate co-productions such as chemical industry preparation, chemical reagent field, foodstuff additive.
Technical background
Tripotassium phosphate generally has two kinds of structures, namely containing three crystal water and anhydrous phosphoric acid tripotassium.Crystalline tripotassium is crystalline powder, there is deliquescence, be widely used in analytical reagent, the preparation of buffer reagent, water-softening chemicals, washing composition and the refining of gasoline, anhydrous phosphoric acid tripotassium is mainly used in foodstuff additive, emulsifying agent, seasonings, antioxidant, is pharmaceutically used as the reinforcer of potassium.
The synthetic method of current Tripotassium phosphate, multiplex phosphoric acid and potassium hydroxide react, and generate crystalline tripotassium, then obtain anhydrous phosphoric acid tripotassium with desiccating method or distillation method removing crystal water.Desiccating method needs high temperature dehydration, complex process, and difficulty is very large, and cost is very high.Distillation method, needs specific installation, and discharging difficulty, and the way finding a fast dewatering is very important.
The solubleness of phosphoric acid is very large, causes the mother liquid concentration after discharging very high, repeatedly concentrated discharging, and quality product declines, and directly discharges, pollutes, so the recovery of producing potassiumphosphate mother liquor is very important.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art part, provide that a kind of cost is low, working efficiency is high, the anhydrous phosphoric acid tripotassium of environmental protection and crystalline tripotassium, calcium phosphate co-production.
The object of the invention is to be achieved through the following technical solutions:
A kind of anhydrous phosphoric acid tripotassium and crystalline tripotassium, calcium phosphate co-production, step is as follows:
(1) potassium hydroxide is made into the solution of 40-50 % by weight, slowly joins in strong phosphoric acid, potassium hydroxide: the mol ratio of strong phosphoric acid is 3:1;
(2) after completion of the reaction, heat filtering, filtrate concentrates, and being concentrated to density is 1.4-1.8g/cm
3time, be cooled to 40-60 DEG C, have crystallization, take out crystallization, namely obtain the Tripotassium phosphate containing a water, dry, wash with water once, in drying plant, be dried to constant weight, obtain anhydrous phosphoric acid tripotassium;
(3) mother liquor continues to be concentrated to and again occurs crystalline film, is cooled to 20-30 DEG C, leaches crystallization, dries, washes with water, dries nature and dries, obtain crystalline tripotassium;
(4) remain in mother liquor and add solid calcium chloride, can calcium phosphate precipitation be generated.
And through filtering reconcentration after described step disposing mother liquor (2), same to aforesaid operations, can reclaim a part of three water crystallization Tripotassium phosphates again.
And the residue Repone K of described step (3) in waste liquid can be concentrated near dry, uses after cooling as chemical fertilizer.
Advantage of the present invention and positively effect:
1, the present invention utilizes same raw material, anhydrous phosphoric acid tripotassium, crystalline tripotassium is once produced by ordinary method, in order to environmental protection, be secondary calcium phosphate the disposing mother liquor of output Tripotassium phosphate, both environmental protection again reduced cost, three kinds of product coproduction, have saved cost, increase work efficiency and economic benefit.
2, the present invention changes over synthesis temperature and the drop temperature of Tripotassium phosphate, and first crystallization goes out a water Tripotassium phosphate, is dried to constant weight after drying, anhydrous phosphoric acid tripotassium, decrease the operation that high temperature sloughs three crystal water.
3, after remaining mother liquor continuation concentrates by the present invention, be cooled to 0 DEG C of crystallization discharging again, namely obtain crystallization three hypophosphite monohydrate tripotassium, then residue disposing mother liquor is added quantitative calcium chloride, can be precipitated as calcium phosphate or secondary calcium phosphate, mother liquor can obtain Repone K fertilizer through concentrated.
4, the method that the application provides both had been suitable for SILVER REAGENT anhydrous phosphoric acid tripotassium, the production of crystalline tripotassium, calcium phosphate, also can realize industrialization, carries out the production of technical grade anhydrous phosphoric acid tripotassium, crystalline potassium, calcium phosphate, accomplish zero release, environmentally safe.
Concrete embodiment
In order to understand the present invention, below in conjunction with embodiment, the invention will be further described: following embodiment is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Embodiment 1
A kind of anhydrous phosphoric acid tripotassium and crystalline tripotassium, calcium phosphate co-production, step is as follows:
(1) a certain amount of potassium hydroxide, is made into the solution of 50% (weight ratio), this solution is slowly joined in strong phosphoric acid, and its theoretical molar, than being 3:1, is reacted as follows:
3KOH+H3PO4→K3PO4+3H2O
(2) after completion of the reaction, heat filtering, filtrate concentrates, and being concentrated to density is 1.4-1.8g/cm
3time, be cooled to 40-60 DEG C, have crystallization, take out crystallization, namely obtain the Tripotassium phosphate containing a water, dry, wash with water once, in drying plant, be dried to constant weight, obtain anhydrous phosphoric acid tripotassium;
(3) mother liquor continues to be concentrated to and again occurs crystalline film, is cooled to 20-30 DEG C, leaches crystallization, dries, washes with water, dries nature and dries, obtain crystalline tripotassium;
(4) remain in mother liquor and add solid calcium chloride, can calcium phosphate precipitation be generated.Till solid calcium chloride is added to and produces without precipitation.
Embodiment 2
A kind of anhydrous phosphoric acid tripotassium and crystalline tripotassium, calcium phosphate co-production, step is as follows:
(1) get a certain amount of potassium hydroxide, be made into the solution of 40wt%, slowly add a certain amount of phosphoric acid, potassium hydroxide: the mol ratio of phosphoric acid is 3:1;
(2) after completion of the reaction, heat filtering, collects mother liquor and concentrates, be concentrated to when mass crystallization film occurs and stopped heating, cooling, when temperature is 50-60 DEG C, crystallization, filter and collect crystallization and filtrate respectively, crystallization dries while hot, by a small amount of hot water wash one time, then dries, in baking oven, 130 DEG C are dried to constant weight, obtain anhydrous phosphoric acid tripotassium;
(3) mother liquor concentrates, when density reaches 1.5-1.6g/cm
3time, be cooled to 10-20 DEG C, leach crystallization, dry, with cold wash 2 times, dry, in 60 DEG C of dryings, obtain three crystalline hydrate Tripotassium phosphates;
(4) remain again a certain amount of calcium chloride precipitation of recovery of mother liquor, reacting completely when being generated as without precipitation, drying, washing 3 times with water, obtain calcium phosphate.
Embodiment 3:
A kind of anhydrous phosphoric acid tripotassium and crystalline tripotassium, calcium phosphate co-production, step is as follows:
(1) get the aqueous solution that a certain amount of potassium hydroxide is made into 40wt%, slowly join in a certain amount of strong phosphoric acid, potassium hydroxide will dissolve safely, heat filter, collects mother liquor and cools, when having department's crystallization to occur bottom being concentrated to, cooling, when temperature is down to 40-60 DEG C, heat filtering, collects crystallization and mother liquor respectively;
(2) crystallization washes 1 time with water, then dries, and is dried to constant weight, obtains anhydrous phosphoric acid tripotassium;
(3) mother liquor proceeds to concentrate, and when being concentrated to crystallization and having occurred, is cooled to 25 DEG C, has had mass crystallization to occur, dries, and with cold wash 2 times, dries, naturally dries, obtain three water crystallization Tripotassium phosphates in dry air;
(4) in order to reclaim three water crystallization Tripotassium phosphates in mother liquor, mother liquor reconcentration after filtration, same to aforesaid operations, recyclable a part of three water crystallization Tripotassium phosphates.
(5) because Tripotassium phosphate solubleness is very large, also retain a part of Tripotassium phosphate in mother liquor, in order to devil liquor recovery, add a certain amount of solid calcium chloride, make calcium phosphate precipitation, after precipitation suction filtration, with water making beating washing 3 times, dry, dry and obtain calcium phosphate for 100 DEG C.
(6) the residue Repone K in waste liquid can be concentrated near dry, can be used as chemical fertilizer and use after cooling.
Claims (3)
1. anhydrous phosphoric acid tripotassium and crystalline tripotassium, a calcium phosphate co-production, it is characterized in that, step is as follows:
(1) potassium hydroxide is made into the solution of 40-50wt%, slowly joins in strong phosphoric acid, potassium hydroxide: the mol ratio of strong phosphoric acid is 3:1;
(2) after completion of the reaction, heat filtering, filtrate concentrates, and being concentrated to density is 1.4-1.8g/cm
3time, be cooled to 40-60 DEG C, have crystallization, take out crystallization, namely obtain the Tripotassium phosphate containing a water, dry, wash with water, be dried to constant weight, obtain anhydrous phosphoric acid tripotassium;
(3) mother liquor continues to be concentrated to and again occurs crystalline film, is cooled to 20-30 DEG C, leaches crystallization, dries, washes with water, then dries nature and dry, and obtains crystalline tripotassium;
(4) remain in mother liquor and add solid calcium chloride, can calcium phosphate precipitation be generated.
2. anhydrous phosphoric acid tripotassium according to claim 1 and crystalline tripotassium, calcium phosphate co-production, is characterized in that: through filtering reconcentration after described step disposing mother liquor (2), same to aforesaid operations, can reclaim a part of three water crystallization Tripotassium phosphates again.
3. anhydrous phosphoric acid tripotassium according to claim 1 and crystalline tripotassium, calcium phosphate co-production, is characterized in that: the residue Repone K of described step (3) in waste liquid can be concentrated near dry, uses after cooling as chemical fertilizer.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112390238A (en) * | 2019-08-15 | 2021-02-23 | 四川磷天化化工科技有限公司 | Production method of polyphosphoric acid trihydrotripotassium |
| CN115159485A (en) * | 2022-08-24 | 2022-10-11 | 连云港树人科创食品添加剂有限公司 | Preparation method of pure tricalcium phosphate |
-
2014
- 2014-11-24 CN CN201410680185.5A patent/CN104445126A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112390238A (en) * | 2019-08-15 | 2021-02-23 | 四川磷天化化工科技有限公司 | Production method of polyphosphoric acid trihydrotripotassium |
| CN115159485A (en) * | 2022-08-24 | 2022-10-11 | 连云港树人科创食品添加剂有限公司 | Preparation method of pure tricalcium phosphate |
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