CN107286010A - A kind of preparation method of potassium citrate - Google Patents
A kind of preparation method of potassium citrate Download PDFInfo
- Publication number
- CN107286010A CN107286010A CN201710625873.5A CN201710625873A CN107286010A CN 107286010 A CN107286010 A CN 107286010A CN 201710625873 A CN201710625873 A CN 201710625873A CN 107286010 A CN107286010 A CN 107286010A
- Authority
- CN
- China
- Prior art keywords
- potassium
- potassium citrate
- preparation
- chlorate
- crystal
- 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.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/487—Separation; Purification; Stabilisation; Use of additives by treatment giving rise to chemical modification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses a kind of preparation method of potassium citrate, it is comprised the following steps that：（1）Citric acid adds the reaction of ionic membrane liquid potassium hydroxide after being dissolved in water, controlling reaction temperature is at 50 DEG C -100 DEG C, and endpoint pH is 7.5；（2）Glucose is added in reaction solution, addition is 5 10 times of the weight content of contained potassium chlorate in raw material ionic membrane liquid potassium hydroxide；（3）Add at 80 DEG C -100 DEG C of the reaction solution of glucose and be incubated more than 1 hour；Condensing crystallizing is evaporated under reduced pressure after filtering；Centrifuge and crystal is washed with water, crystal obtains potassium citrate finished product after being dried through fluid bed.The preparation method of potassium citrate of the present invention, while potassium citrate is prepared, moreover it is possible to effectively remove potassium chlorate, the content of product potassium citrate is more than 99.5%, readily carbonizable substance touches the mark, and light transmittance is more than 98%, and the potassium chlorate content in potassium citrate is less than 10PPb.
Description
Technical field
The invention belongs to food additives field, it is related to a kind of preparation side for the potassium citrate that can effectively remove potassium chlorate
Method.
Background technology：
Potassium citrate is colourless crystallization or white crystalline powder, and soluble in water, taste is salty and cool.Buffering can be used in the food industry
Agent, mixture, stabilizer, antioxidant, emulsifying agent etc., can be used as anticoagulant, hypokalemia and alkalization urine in pharmaceuticals industry
The treatment of liquid, in recent years, the steady-state growth always of its demand.
Potassium citrate production method is citric acid to be dissolved in into water and potassium hydroxide reacts generation potassium citrate.Wherein lemon
Lemon acid is by molten powder class material（Such as corn, wooden heat）Fermented production；Potassium hydroxide be electrolysis with ion-exchange film potassium chloride and
Obtain, due to the characteristic of electrolysis, make the chlorate containing 40-100PPm in potassium hydroxide, the chlorate can enter final lemon
In sour potassium product.
Potassium chlorate is colorless plate crystal or white particle powder, is strong oxidizer, for explosive, fireworks, analysis
Reagent, rocket-powered missile propellant etc., with the development of aerospace industry and military project, there is chlorate and perchlorate in nature；
Chlorate and perchlorate are found in tealeaves, vegetables and milk powder, another derives from chlorine-containing disinfectant to chlorate, originally
Water and equipment disinfection often use chlorine-containing disinfectant, and such as bleaching powder, chlorine dioxide, chlorine atom have very strong lethality to microorganism,
It can also be reacted simultaneously with the organic matter in water, produce a variety of DBPs, one of them is exactly chlorate, either high
Chlorate or chlorate can all hinder thyroid gland to absorb iodine, and according to the difference of intake, chlorate can cause bad to health
Influence, it is accordingly required in particular to which, it is to be noted that the crowd of dysthyreosis, iodine deficiency patient, infants and children, especially children are in child
Period, enough thyroid hormones grow for it and have vital effect, in addition, chlorate can also destroy red blood
Ball, so as to influence the function of blood transportation oxygen.
In some high-end potassium citrates using in client such as infant formula and pharmaceuticals industry, to chloric acid in potassium citrate
Salt has strict demand, it is desirable to which chlorate content is less than 10PPb.This is accomplished by removing chlorate in potassium citrate production process.
Therefore, except the method for chlorate has great importance in research and development potassium citrate preparation process.
The content of the invention
The technical problems to be solved by the invention be in view of the shortcomings of the prior art there is provided a kind of technique it is simple, be produced into
This is low and can effectively remove the preparation method of potassium chlorate potassium citrate.
The technical problems to be solved by the invention are realized by following technical scheme.The present invention is a kind of lemon
The preparation method of sour potassium, is comprised the following steps that：
（1）Citric acid adds the reaction of ionic membrane liquid potassium hydroxide after being dissolved in water, controlling reaction temperature is at 50 DEG C -100 DEG C, eventually
Point pH value is 7.5；
（2）Glucose is added in reaction solution, addition is the weight of contained potassium chlorate in raw material ionic membrane liquid potassium hydroxide
5-10 times of content；
（3）Add at 80 DEG C -100 DEG C of the reaction solution of glucose and be incubated more than 1 hour；
（4）By step（3）Condensing crystallizing is evaporated under reduced pressure after resulting solution filtering；
（5）By step（4）Gained potassium citrate crystal centrifuges and crystal is washed with water, and crystal obtains lemon after being dried through fluid bed
Lemon acid potassium finished product.
In a kind of technical scheme of the preparation method of potassium citrate of the present invention, further preferred technical scheme or
Person's technical characteristic is：
1st, step（1）Potassium chlorate containing 10-60PPM in middle raw material ionic membrane liquid potassium hydroxide.Can be with washing light in solution
Degree method is surveyed potassium chlorate content in potassium chlorate content, potassium citrate product and can detected with LC-MS-MS methods.
2nd, step（1）Controlling reaction temperature is at 70 DEG C.Too low increase cooling circulating water consumption, too high increase side reaction.
3rd, step（1）The citric acid mass content that citric acid is dissolved in the aqueous citric acid solution that water is obtained is 50%-70%, is entered
One step preferably 60%；The mass concentration of described ionic membrane liquid potassium hydroxide is 30%-50%, further preferred 40%.If lemon
Acid content is too low, adds water more, evaporation capacity during increase subsequent evaporation condensing crystallizing, increases steam consumption, improves cost；If lemon
Lemon acid content is too high, then citric acid viscosity is excessive, is unfavorable for follow-up work progress.If potassium hydroxide solution concentration is too low, enter to add
Evaporation capacity during subsequent evaporation condensing crystallizing, increases steam consumption, increases cost；If concentration of potassium hydroxide is too high, make part
Reaction is excessively fierce, side reaction increase, yield reduction.
4th, step（2）The addition of middle glucose is 7 times of potassium chlorate.The too low amount that may remove potassium chlorate does not reach will
Ask；Too high to increase cost, readily carbonizable substance is improved in product.
5th, its step（3）Plus the reaction solution of glucose is incubated 1-3 hours at 90 DEG C.Temperature is higher, is more conducive to chloric acid
Potassium and glucose response, temperature, which will cross high energy consumption, to be increased.
6th, step（4）During described reduction vaporization condensing crystallizing, its vacuum is in -0.09MPa, thickening temperature 70 DEG C-
100℃。
7th, step（5）The washing, leaching requirement is no less than the 10% of crystal weight, further preferred consumption 12%.Leaching requirement
Greatly, dissolution of crystals amount is increased, and increases mother liquor amount, and leaching requirement is small, and readily carbonizable substance can be exceeded.
Compared with prior art, the preparation method of potassium citrate of the present invention, while potassium citrate is prepared, moreover it is possible to effectively
Ground remove potassium chlorate, the content of product potassium citrate is more than 99.5%, and readily carbonizable substance touches the mark, light transmittance more than 98%,
Potassium chlorate content in potassium citrate is less than 10PPb.
Embodiment
Technical solution of the present invention is described further below, so that those skilled in the art are further understood that this hair
It is bright, without constituting the limitation to right of the present invention.
Embodiment 1, a kind of preparation method of potassium citrate, it is comprised the following steps that：
（1）Citric acid adds the reaction of ionic membrane liquid potassium hydroxide after being dissolved in water, controlling reaction temperature is at 50 DEG C, and endpoint pH exists
7.5；
（2）Glucose is added in reaction solution, addition is the weight of contained potassium chlorate in raw material ionic membrane liquid potassium hydroxide
5 times of content；
（3）Add at 80 DEG C of the reaction solution of glucose and be incubated more than 1 hour；
（4）By step（3）Condensing crystallizing is evaporated under reduced pressure after resulting solution filtering；
（5）By step（4）Gained potassium citrate crystal centrifuges and crystal is washed with water, and crystal obtains lemon after being dried through fluid bed
Lemon acid potassium finished product.
Embodiment 2, a kind of preparation method of potassium citrate, it is comprised the following steps that：
（1）Citric acid adds the reaction of ionic membrane liquid potassium hydroxide after being dissolved in water, controlling reaction temperature is in 100 DEG C, endpoint pH
7.5；
（2）Glucose is added in reaction solution, addition is the weight of contained potassium chlorate in raw material ionic membrane liquid potassium hydroxide
10 times of content；
（3）Add at 100 DEG C of the reaction solution of glucose and be incubated more than 1 hour；
（4）By step（3）Condensing crystallizing is evaporated under reduced pressure after resulting solution filtering；
（5）By step（4）Gained potassium citrate crystal centrifuges and crystal is washed with water, and crystal obtains lemon after being dried through fluid bed
Lemon acid potassium finished product.
Embodiment 3, a kind of preparation method of potassium citrate, it is comprised the following steps that：
（1）Citric acid adds the reaction of ionic membrane liquid potassium hydroxide after being dissolved in water, controlling reaction temperature is at 70 DEG C, and endpoint pH exists
7.5；
（2）Glucose is added in reaction solution, addition is the weight of contained potassium chlorate in raw material ionic membrane liquid potassium hydroxide
7 times of content；
（3）Add at 90 DEG C of the reaction solution of glucose and be incubated 2 hours；
（4）By step（3）Condensing crystallizing is evaporated under reduced pressure after resulting solution filtering；Be evaporated under reduced pressure condensing crystallizing when, its vacuum-
0.09MPa, thickening temperature is at 70 DEG C -100 DEG C.
（5）By step（4）Gained potassium citrate crystal centrifuges and crystal is washed with water, and leaching requirement is no less than crystal weight
The 10% of amount.Crystal obtains potassium citrate finished product after being dried through fluid bed.
A kind of embodiment 4, preparation method of potassium citrate, step is as follows：
（1）In 10m3Reactor in add 3 tons of citric acids, add 2 tons of deionized water, stirring and dissolving obtains solution A.
（2）About 4.9 tons of 48% potassium hydroxide solution is added dropwise into solution A, reaction temperature is controlled at 80 DEG C, and terminal pH value exists
7.5 ± 0.1, obtain about 9.9 tons of solution B.
（3）Solution B sample is taken, it is 316.8 grams of chloracid potassium in 32PPM, solution B to survey wherein potassium chlorate content.
（4）2.2KG glucose is added into B solution, being incubated 1.5 hours at 80 DEG C obtains solution D.
（5）Solution D is filtered, condensing crystallizing is evaporated under reduced pressure, the magma E containing potassium citrate crystal and mother liquor is obtained.
（6）Magma E is put into centrifuge and centrifuged, crystal is washed with 350KG deionized waters in separation process.Crystal
3.2 tons of potassium citrate finished product, mother liquor reuse are dried to obtain through fluid bed.
After testing, potassium citrate content 99.6%, light transmittance 98.8%；Readily carbonizable substance：Pass through detection；Potassium chlorate content：
8PPb。
A kind of embodiment 5, preparation method of potassium citrate, step is as follows：
（1）In 10m32 tons of sodium citrate mother liquors are added in reactor, addition goes 1 ton from water, adds 2 tons of citric acid, stirs molten
Solution, obtains solution A.
（2）About 3.9 tons of 40% potassium hydroxide solution is added dropwise into solution A, reaction temperature is controlled in 80 DEG C, terminal pH value
7.5, obtain about 8.9 tons of solution B.
（3）Solution B sample is taken to survey wherein chloracid potassium 26PPM, chloracid potassium total amount is at 231.4 grams in solution B.
（4）1.8 kilograms of glucose are added into B solution, 1.5 hours is incubated at 90 DEG C, obtains solution D.
（5）Solution D is filtered, condensing crystallizing is evaporated under reduced pressure, the magma E containing potassium citrate crystal and mother liquor is obtained.
（6）Magma E is put into centrifuge and centrifuged, crystal is washed with 300 kilograms of deionized waters in separation process.
Potassium citrate crystal is dried through vibrated fluidized bed, obtains 3.0 tons of potassium citrate finished product.Mother liquor reuse.
After testing, potassium citrate content：99.5%；Light transmittance 98.6%；Readily carbonizable substance：Pass through detection；Potassium chlorate：5PPb.
Claims (9)
1. a kind of preparation method of potassium citrate, it is characterised in that it is comprised the following steps that：
（1）Citric acid adds the reaction of ionic membrane liquid potassium hydroxide after being dissolved in water, controlling reaction temperature is at 50 DEG C -100 DEG C, eventually
Point pH value is 7.5；
（2）Glucose is added in reaction solution, addition is the weight of contained potassium chlorate in raw material ionic membrane liquid potassium hydroxide
5-10 times of content；
（3）Add at 80 DEG C -100 DEG C of the reaction solution of glucose and be incubated more than 1 hour；
（4）By step（3）Condensing crystallizing is evaporated under reduced pressure after resulting solution filtering；
（5）By step（4）Gained potassium citrate crystal centrifuges and crystal is washed with water, and crystal obtains lemon after being dried through fluid bed
Lemon acid potassium finished product.
2. the preparation method of potassium citrate according to claim 1, it is characterised in that：Step（1）Middle raw material ionic membrane liquid
Potassium chlorate containing 10-60PPM in potassium hydroxide.
3. the preparation method of potassium citrate according to claim 1, it is characterised in that：Step（1）Controlling reaction temperature is 70
℃。
4. the preparation method of potassium citrate according to claim 1, it is characterised in that：Step（1）Citric acid is dissolved in water and obtained
Aqueous citric acid solution in citric acid mass content be 50%-70%；The mass concentration of described ionic membrane liquid potassium hydroxide
For 30%-50%.
5. the preparation method of potassium citrate according to claim 1, it is characterised in that：Step（2）The addition of middle glucose
For 7 times of potassium chlorate content.
6. the preparation method of potassium citrate, its step according to claim 1（3）Plus the reaction solution of glucose is protected at 90 DEG C
It is warm 1-3 hours.
7. the preparation method of potassium citrate according to claim 1, it is characterised in that：Step（4）Described reduction vaporization is dense
When sheepshank is brilliant, its vacuum is in -0.09MPa, thickening temperature is at 70 DEG C -100 DEG C.
8. the preparation method of potassium citrate according to claim 1, it is characterised in that：Step（5）The washing, leaching requirement is not
Less than the 10% of crystal weight.
9. the preparation method of potassium citrate according to claim 1, it is characterised in that:Potassium chlorate in gained potassium citrate product
Content is less than 10PPb.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710625873.5A CN107286010A (en) | 2017-07-27 | 2017-07-27 | A kind of preparation method of potassium citrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710625873.5A CN107286010A (en) | 2017-07-27 | 2017-07-27 | A kind of preparation method of potassium citrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107286010A true CN107286010A (en) | 2017-10-24 |
Family
ID=60103564
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710625873.5A Pending CN107286010A (en) | 2017-07-27 | 2017-07-27 | A kind of preparation method of potassium citrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107286010A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108794323A (en) * | 2018-05-23 | 2018-11-13 | 连云港树人科创食品添加剂有限公司 | A kind of preparation method of sodium citrate |
| CN109369371A (en) * | 2018-11-21 | 2019-02-22 | 大自然生物集团有限公司 | A kind of anhydrous citric acid potassium crystal form and preparation method thereof |
| CN112174812A (en) * | 2020-11-04 | 2021-01-05 | 日照金禾博源生化有限公司 | Preparation method of potassium citrate with ultralow chlorate content |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2610105A (en) * | 1951-03-26 | 1952-09-09 | Dow Chemical Co | Process of simultaneously purifying and dehydrating caustic alkali solutions containing chlorates |
| US4676971A (en) * | 1985-12-24 | 1987-06-30 | Ppg Industries, Inc. | Method for removing chlorate from alkali metal hydroxide |
| CN101041602A (en) * | 2007-03-09 | 2007-09-26 | 陕西汉唐环保农业有限公司 | Dextroglucose plants organic nutrient solution and producing technique |
-
2017
- 2017-07-27 CN CN201710625873.5A patent/CN107286010A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2610105A (en) * | 1951-03-26 | 1952-09-09 | Dow Chemical Co | Process of simultaneously purifying and dehydrating caustic alkali solutions containing chlorates |
| US4676971A (en) * | 1985-12-24 | 1987-06-30 | Ppg Industries, Inc. | Method for removing chlorate from alkali metal hydroxide |
| CN101041602A (en) * | 2007-03-09 | 2007-09-26 | 陕西汉唐环保农业有限公司 | Dextroglucose plants organic nutrient solution and producing technique |
Non-Patent Citations (1)
| Title |
|---|
| 田君等: "如何有效控制烧碱中氯酸盐的含量", 《中国氯碱》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108794323A (en) * | 2018-05-23 | 2018-11-13 | 连云港树人科创食品添加剂有限公司 | A kind of preparation method of sodium citrate |
| CN109369371A (en) * | 2018-11-21 | 2019-02-22 | 大自然生物集团有限公司 | A kind of anhydrous citric acid potassium crystal form and preparation method thereof |
| CN112174812A (en) * | 2020-11-04 | 2021-01-05 | 日照金禾博源生化有限公司 | Preparation method of potassium citrate with ultralow chlorate content |
| CN112174812B (en) * | 2020-11-04 | 2022-12-13 | 日照金禾博源生化有限公司 | Preparation method of potassium citrate with ultralow chlorate content |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100427394C (en) | Method for preparing lithium chloride free from water | |
| CN107286010A (en) | A kind of preparation method of potassium citrate | |
| CN102311100A (en) | Method for preparing potassium hydrogen peroxymonosulfate composite salt | |
| US2320635A (en) | Manufacture of high test bleach | |
| CN108640089A (en) | Potassium hydrogen persulfate composite salts serialization making apparatus and preparation method | |
| CN105399867A (en) | Preparation method for heparin sodium | |
| CN106810442B (en) | A kind of production method of high-quality adipic acid | |
| CN112357890A (en) | Method for controlling growth of potassium hydrogen peroxymonosulfate composite salt crystal | |
| CN108794323A (en) | A kind of preparation method of sodium citrate | |
| CN101337929A (en) | Process for synthesizing quinclorac by oxidizing reaction | |
| CN102408347A (en) | Method for preparing monopotassium L-aspartate dihydrate by separation process | |
| US4432959A (en) | Process of producing sodium cyanuarate | |
| CN117163968A (en) | Method for preparing boric acid and borax from MVR boron concentrate in lithium extraction process of salt lake | |
| DE1155133B (en) | Process for the production of calcium di (dichloroisocyanurate) and its hydrates | |
| CN106495189A (en) | A kind of production method of high-purity food-grade potassium chloride | |
| CN110078097A (en) | A kind of technique of instant solution process for preparing potassium nitrate by double decomposition | |
| CN102476813B (en) | Production process of medical large-particle potassium chloride | |
| CN108439435A (en) | A kind of method that direct method prepares potassium nitrate | |
| CN104725281A (en) | Method for producing urea peroxide | |
| CN108190921A (en) | A kind of preparation method of high-purity lithium salts | |
| CN103787870B (en) | A kind of minimizing technology of Trisodium Citrate readily carbonizable substance | |
| CN110498431A (en) | A kind of preparation method of high-purity spherical shape potassium chloride | |
| CN109336053B (en) | Method for extracting iodine from saline water after secondary zinc oxide rinsing | |
| CN112174812B (en) | Preparation method of potassium citrate with ultralow chlorate content | |
| CN106966425A (en) | A kind of method of white vitriol particle increase |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20171024 |
|
| RJ01 | Rejection of invention patent application after publication |