CN104478704A - Preparation method of anhydrous trisodium citrate - Google Patents
Preparation method of anhydrous trisodium citrate Download PDFInfo
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- CN104478704A CN104478704A CN201410798623.8A CN201410798623A CN104478704A CN 104478704 A CN104478704 A CN 104478704A CN 201410798623 A CN201410798623 A CN 201410798623A CN 104478704 A CN104478704 A CN 104478704A
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- Prior art keywords
- citric acid
- sodium hydroxide
- crystal
- sodium citrate
- citrate
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- 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
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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of anhydrous trisodium citrate (also known as anhydrous sodium citrate). The method comprises the following steps: with food-grade citric acid and sodium hydroxide as raw materials, dissolving sodium hydroxide to prepare a 25%-30% water solution, then slowly adding the food-grade citric acid crystal to the sodium hydroxide solution, stirring and carrying out neutral reaction, wherein the citric acid adding rate is controlled to adjust the pH value; reheating by using neutral heat generated in reaction to concentrate the material; cooling to a room temperature, separating out a lot of sodium citrate crystals, carrying out centrifugal separation, and recycling mother liquid; and feeding the crystal material to a hot air circulating oven, drying until the sodium citrate crystals become white particles, so as to achieve the requirements of anhydride, and controlling according to the regulation that the water content is smaller than 1%. The preparation method is high in raw material utilization rate, simple in preparation process, free of pollution, clean and environment-friendly.
Description
Technical field
The invention belongs to food, medicine, daily use chemicals raw materials technology field, be specifically related to a kind of production method of anhydrous sodium citrate.
Background technology
Owing to having the requirement of not water content at food-processing, daily use chemicals and medical material to Trisodium Citrate, moisture content≤1.0%, and Trisodium Citrate market only produced usually containing two crystal water, moisture content reaches 10.0-13.0%, in order to meet the requirement of market to Trisodium Citrate anhydride.The present invention adopts food grade citric acid and food grade sodium hydroxide neutralization reaction, and through concentrated, crystallization, hyperthermia drying dehydration, obtained anhydrous sodium citrate, avoids traditional technology citric acid and sodium carbonate is raw material, has a large amount of CO in neutralization reaction process
2exhaust gas emission, CO
2gas is considered to the main greenhouse gas endangering global environment.
Citric Acid, usp, Anhydrous Powder sodium is white granular crystallization or powder, odorless, and taste is salty, and micro-in wet air have deliquescence.
Summary of the invention
Goal of the invention: the production method that the invention provides a kind of anhydrous sodium citrate (also known as Citric Acid, usp, Anhydrous Powder sodium), raw material availability is high, and production technique is simple, and pollution-free, clean environment firendly.
Reaction principle is as follows: C
6h
8o
7+ 3NaOH → C
6h
5o
7na
3+ 3H
2o, the molecular structural formula of obtained anhydrous sodium citrate is as follows:
Technical scheme: a kind of production method of anhydrous sodium citrate, comprises the steps:
(a), with the citric acid of food grade and sodium hydroxide for raw material;
(b), sodium hydroxide dissolved be mixed with the aqueous solution of 25-30%;
(c), the Citric acid crystal of food grade is slowly added in sodium hydroxide solution, stir carry out neutralization reaction;
D (), control add the speed of citric acid, adjust ph is 7.6-9.0;
(e), utilize the neutralization heat of reaction, carry out reheating material is concentrated, the strength of solution of Trisodium Citrate controls between degree Beaume d:1.35-1.40;
(f), be then cooled to normal temperature, a large amount of Trisodium Citrate crystal is separated out, and carry out centrifugation, mother liquor can be recycled;
(g), crystal material is delivered to Hotaircirculatingoven, temperature controls between 150-180 DEG C, dry that 2.5-3.5 is little becomes white shape particle up to Trisodium Citrate by crystal, reach the requirement of anhydride, and control by the regulation of moisture content < 1%.
As optimization: in described step (b), sodium hydroxide dissolves the aqueous solution being mixed with 27%.
As optimization: in described step (d), pH value is 8.3.
As optimization: in described step (e), degree Beaume d is 1.37.
As optimization: in described step (g), temperature controls between 176 DEG C, dries 3 hours.
Beneficial effect: raw material availability of the present invention is high, production technique is simple, and pollution-free, clean environment firendly.
Concrete advantage is as follows:
1, because citric acid uses lenticular, the consumption of whole neutralization reaction is less, can decrease concentration time, reduce power consumption;
2, the technical requirement of table 1 index name
| Index name | Requirement |
| Citric Acid, usp, Anhydrous Powder sodium content | ≥99.0% |
| Vitriol | ≤0.01% |
| Acidity and basicity | Conform with the regulations |
| Molysite | ≤0.001% |
| Oxalate | ≤0.04% |
| Calcium salt | ≤0.02% |
| Readily carbonizable substance | ≤1.0 |
| Muriate | ≤0.005% |
| Lead salt (in Pb) | ≤0.0002% |
| Arsenic salt (As) | ≤0.0001% |
| Water-insoluble | Pass Test |
| Moisture content | ≤1% |
Obtained anhydrous sodium citrate meets the technical requirement of the index name of table 1 above.
Embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail.
Specific embodiment 1:
A production method for anhydrous sodium citrate, comprises the steps:
(a), with the citric acid of food grade and sodium hydroxide for raw material;
(b), by sodium hydroxide dissolve be mixed with 25% the aqueous solution;
(c), the Citric acid crystal of food grade is slowly added in sodium hydroxide solution, stir carry out neutralization reaction;
D (), control add the speed of citric acid, adjust ph is 7.6;
(e), utilize the neutralization heat of reaction, carry out reheating material is concentrated, the strength of solution of Trisodium Citrate controls between degree Beaume d:1.35;
(f), be then cooled to normal temperature, a large amount of Trisodium Citrate crystal is separated out, and carry out centrifugation, mother liquor can be recycled;
(g), crystal material is delivered to Hotaircirculatingoven, temperature controls between 150 DEG C, dries 2.5 and littlely becomes white shape particle up to Trisodium Citrate by crystal, reach the requirement of anhydride, and be carried out in accordance with regulations control.
Specific embodiment 2:
A production method for anhydrous sodium citrate, comprises the steps:
(a), with the citric acid of food grade and sodium hydroxide for raw material;
(b), by sodium hydroxide dissolve be mixed with 30% the aqueous solution;
(c), the Citric acid crystal of food grade is slowly added in sodium hydroxide solution, stir carry out neutralization reaction;
D (), control add the speed of citric acid, adjust ph is 9.0;
(e), utilize the neutralization heat of reaction, carry out reheating material is concentrated, the strength of solution of Trisodium Citrate controls between degree Beaume d:1.40;
(f), be then cooled to normal temperature, a large amount of Trisodium Citrate crystal is separated out, and carry out centrifugation, mother liquor can be recycled;
(g), crystal material is delivered to Hotaircirculatingoven, temperature controls between 180 DEG C, dries 3.5 and littlely becomes white shape particle up to Trisodium Citrate by crystal, reach the requirement of anhydride, and be carried out in accordance with regulations control.
Specific embodiment 3:
A production method for anhydrous sodium citrate, comprises the steps:
(a), with the citric acid of food grade and sodium hydroxide for raw material;
(b), by sodium hydroxide dissolve be mixed with 27% the aqueous solution;
(c), the Citric acid crystal of food grade is slowly added in sodium hydroxide solution, stir carry out neutralization reaction;
D (), control add the speed of citric acid, adjust ph is 8.3;
(e), utilize the neutralization heat of reaction, carry out reheating material is concentrated, the strength of solution of Trisodium Citrate controls between degree Beaume d:1.37;
(f), be then cooled to normal temperature, a large amount of Trisodium Citrate crystal is separated out, and carry out centrifugation, mother liquor can be recycled;
(g), crystal material is delivered to Hotaircirculatingoven, temperature controls between 176 DEG C, dries 3 and littlely becomes white shape particle up to Trisodium Citrate by crystal, reach the requirement of anhydride, and be carried out in accordance with regulations control.
Claims (5)
1. a production method for anhydrous sodium citrate, is characterized in that: comprise the steps:
(a), with the citric acid of food grade and sodium hydroxide for raw material;
(b), sodium hydroxide dissolved be mixed with the aqueous solution of 25-30%;
(c), the Citric acid crystal of food grade is slowly added in sodium hydroxide solution, stir carry out neutralization reaction;
D (), control add the speed of citric acid, adjust ph is 7.6-9.0;
(e), utilize the neutralization heat of reaction, carry out reheating material is concentrated, the strength of solution of Trisodium Citrate controls between degree Beaume d:1.35-1.40;
(f), be then cooled to normal temperature, a large amount of Trisodium Citrate crystal is separated out, and carry out centrifugation, mother liquor can be recycled;
(g), crystal material is delivered to Hotaircirculatingoven, temperature controls between 150-180 DEG C, dries that 2.5-3.5 is little becomes white shape particle up to Trisodium Citrate by crystal, reaches the requirement of anhydride, and is carried out in accordance with regulations control.
2. the production method of anhydrous sodium citrate as claimed in claim 1, is characterized in that: in described step (b), and sodium hydroxide dissolves the aqueous solution being mixed with 27%.
3. the production method of anhydrous sodium citrate as claimed in claim 1, it is characterized in that: in described step (d), pH value is 8.3.
4. the production method of anhydrous sodium citrate as claimed in claim 1, it is characterized in that: in described step (e), degree Beaume d is 1.37.
5. the production method of anhydrous sodium citrate as claimed in claim 1, it is characterized in that: in described step (g), temperature controls between 176 DEG C, dries 3 hours.
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| CN201410798623.8A CN104478704A (en) | 2014-12-22 | 2014-12-22 | Preparation method of anhydrous trisodium citrate |
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|---|---|---|---|
| CN201410798623.8A CN104478704A (en) | 2014-12-22 | 2014-12-22 | Preparation method of anhydrous trisodium citrate |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105037140A (en) * | 2015-06-26 | 2015-11-11 | 宁乡新阳化工有限公司 | Anhydrous sodium citrate production method |
| CN107188798A (en) * | 2017-05-27 | 2017-09-22 | 湖南新绿方药业有限公司 | A kind of process for refining of sodium citrate of controllable granularity and realize device |
| CN107286009A (en) * | 2017-06-19 | 2017-10-24 | 江苏润普食品科技股份有限公司 | A kind of method of utilization citric acid and sodium hydroxide synthesizing citric acid sodium |
| CN109438225A (en) * | 2018-11-21 | 2019-03-08 | 大自然生物集团有限公司 | A kind of preparation method of bulky grain anhydrous citric acid sodium |
| CN110407687A (en) * | 2019-08-16 | 2019-11-05 | 上海蓝滨石化设备有限责任公司 | Citric acid and its sodium salt co-generation system |
| CN114163324A (en) * | 2021-10-27 | 2022-03-11 | 莱芜泰禾生化有限公司 | Preparation method and preparation system of anhydrous trisodium citrate |
| CN114773182A (en) * | 2022-03-29 | 2022-07-22 | 南京化学试剂股份有限公司 | Synthetic method of medicinal sodium citrate |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0597235A1 (en) * | 1992-10-09 | 1994-05-18 | HAARMANN & REIMER CORPORATOPN | Production of citric acid and trisodium citrate from molasses |
| CN101607892A (en) * | 2009-08-07 | 2009-12-23 | 湖南尔康制药有限公司 | The production method of Sodium Citrate |
| CN101863756A (en) * | 2010-07-07 | 2010-10-20 | 南通市飞宇精细化学品有限公司 | Process for producing disodium citrate |
| CN102476993A (en) * | 2010-11-26 | 2012-05-30 | 中粮生物化学（安徽）股份有限公司 | Preparation method of sodium citrate |
| CN103044239A (en) * | 2012-12-17 | 2013-04-17 | 日照金禾博源生化有限公司 | Production method of sodium citrate |
-
2014
- 2014-12-22 CN CN201410798623.8A patent/CN104478704A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0597235A1 (en) * | 1992-10-09 | 1994-05-18 | HAARMANN & REIMER CORPORATOPN | Production of citric acid and trisodium citrate from molasses |
| CN101607892A (en) * | 2009-08-07 | 2009-12-23 | 湖南尔康制药有限公司 | The production method of Sodium Citrate |
| CN101863756A (en) * | 2010-07-07 | 2010-10-20 | 南通市飞宇精细化学品有限公司 | Process for producing disodium citrate |
| CN102476993A (en) * | 2010-11-26 | 2012-05-30 | 中粮生物化学（安徽）股份有限公司 | Preparation method of sodium citrate |
| CN103044239A (en) * | 2012-12-17 | 2013-04-17 | 日照金禾博源生化有限公司 | Production method of sodium citrate |
Non-Patent Citations (2)
| Title |
|---|
| 周本华等: "食品添加剂柠檬酸三钠绿色生产工艺的研究", 《食品工业科技》 * |
| 陈维新: "食品添加剂柠檬酸钠生产工艺的研究", 《广东轻工职业技术学院学报》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105037140A (en) * | 2015-06-26 | 2015-11-11 | 宁乡新阳化工有限公司 | Anhydrous sodium citrate production method |
| CN107188798A (en) * | 2017-05-27 | 2017-09-22 | 湖南新绿方药业有限公司 | A kind of process for refining of sodium citrate of controllable granularity and realize device |
| CN107286009A (en) * | 2017-06-19 | 2017-10-24 | 江苏润普食品科技股份有限公司 | A kind of method of utilization citric acid and sodium hydroxide synthesizing citric acid sodium |
| CN109438225A (en) * | 2018-11-21 | 2019-03-08 | 大自然生物集团有限公司 | A kind of preparation method of bulky grain anhydrous citric acid sodium |
| CN110407687A (en) * | 2019-08-16 | 2019-11-05 | 上海蓝滨石化设备有限责任公司 | Citric acid and its sodium salt co-generation system |
| CN114163324A (en) * | 2021-10-27 | 2022-03-11 | 莱芜泰禾生化有限公司 | Preparation method and preparation system of anhydrous trisodium citrate |
| CN114163324B (en) * | 2021-10-27 | 2023-12-08 | 莱芜泰禾生化有限公司 | Preparation method and preparation system of anhydrous trisodium citrate |
| CN114773182A (en) * | 2022-03-29 | 2022-07-22 | 南京化学试剂股份有限公司 | Synthetic method of medicinal sodium citrate |
| CN114773182B (en) * | 2022-03-29 | 2023-02-03 | 南京化学试剂股份有限公司 | Synthetic method of medicinal-grade sodium citrate |
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Application publication date: 20150401 |
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