CN113493375A - Synthesis method of edible sodium diacetate - Google Patents

Synthesis method of edible sodium diacetate Download PDF

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Publication number
CN113493375A
CN113493375A CN202110843186.7A CN202110843186A CN113493375A CN 113493375 A CN113493375 A CN 113493375A CN 202110843186 A CN202110843186 A CN 202110843186A CN 113493375 A CN113493375 A CN 113493375A
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CN
China
Prior art keywords
sodium diacetate
synthesizing
acetic acid
reaction
edible
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Pending
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CN202110843186.7A
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Chinese (zh)
Inventor
吴宜民
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Lianyungang Nuoxin Food Ingredients Co ltd
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Lianyungang Nuoxin Food Ingredients Co ltd
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Application filed by Lianyungang Nuoxin Food Ingredients Co ltd filed Critical Lianyungang Nuoxin Food Ingredients Co ltd
Priority to CN202110843186.7A priority Critical patent/CN113493375A/en
Publication of CN113493375A publication Critical patent/CN113493375A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/41Preparation of salts of carboxylic acids
    • C07C51/412Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C51/00Preparation of carboxylic acids or their salts, halides or anhydrides
    • C07C51/42Separation; Purification; Stabilisation; Use of additives

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to the technical field of sodium diacetate preparation, in particular to a method for synthesizing edible sodium diacetate, which comprises the following steps: adding acetic acid into a reaction kettle, stirring, adding sodium carbonate, detecting the pH value to be 4.5-5.0 on line, heating for reaction, crystallizing, performing spin filtration, drying, cooling and crushing to obtain the edible sodium diacetate. The energy consumption in the reaction process is considered, the reaction tail gas is absorbed, and the filtered mother liquor is recycled, so that the production cost is saved, and the environmental pollution is reduced.

Description

Synthesis method of edible sodium diacetate
The technical field is as follows: the invention relates to a synthetic method of a food additive, in particular to a synthetic method of food-grade sodium diacetate.
Background art: the sodium diacetate is a molecular compound which associates acetic acid and sodium acetate through intramolecular hydrogen bonds, can be used as additives of foods, grains and the like, and has the effects of corrosion prevention, insurance, nutrition increase and the like. The principle is that the unimolecular acetic acid in sodium diacetate molecules has good compatibility with lipoid compounds, and effectively permeates cell walls to permeate into cell bodies of fungus tissues to interfere the interaction of enzymes among cells to inactivate proteins, thereby playing the roles of mildew prevention and bacteriostasis. The prior art for producing sodium diacetate mainly comprises a sodium acetate-acetic acid method, an acetic acid-caustic soda method, an acetic acid-acetic anhydride-soda ash method and an acetic acid-sodium carbonate method. Wherein the acetic acid-sodium carbonate method has the lowest cost. And the recovery of tail gas and waste liquid in the production process by adopting the acetic acid-sodium carbonate method is not mentioned.
The invention content is as follows: aiming at the defects of the prior art, the invention provides a method for synthesizing edible sodium diacetate, which comprises the following steps,
the method comprises the following steps: adding acetic acid into a reaction kettle, stirring, slowly adding sodium carbonate solid powder, detecting the pH range to be 4.5-5.0 on line, heating to 50-70 ℃, reacting for 3-5 hours, after the reaction is finished, crystallizing, cooling to 20-30 ℃ while stirring, crystallizing for 2-3 hours, adding the reaction liquid into a centrifuge, performing spin filtration until no liquid flows out, and collecting filter cakes and filtrate. And putting the filter cake into an oven, setting the temperature to be 70-80 ℃, drying for 2-3 hours to obtain sodium diacetate solid, cooling, crushing by a crusher, putting into the oven again, setting the temperature to be 60-70 ℃, and drying for 4-5 hours to obtain the food-grade sodium diacetate solid.
Step two: and (5) a recycling step, namely filling sodium hydroxide solid in the reaction kettle in the step one for tail gas absorption, and reacting with the filtrate acetic acid subjected to the filter throwing in the step one when the sodium hydroxide is completely consumed. The steps are the same as the first step.
Further, the centrifuge used in the first step is an antiseptic centrifuge.
Further, the oven used in the first step is a blast oven.
Further, the consumption of the second step is finished by the complete reaction of the sodium hydroxide.
Further, the content of water in acetic acid in the filtrate in the second step is not more than 10%.
Further, in the second step, over 10% of water in the acetic acid in the filtrate is removed by using a molecular sieve.
The specific embodiment is as follows:
the present invention is further described below.
Example 1
Adding acetic acid into a reaction kettle with a tail gas absorption device, stirring, slowly adding sodium carbonate solid powder, detecting the pH value to be 4.5 on line, heating to 50 ℃, reacting for 5 hours, after the reaction is finished, crystallizing, cooling to 20 ℃ while stirring, crystallizing for 2 hours, adding the reaction liquid into an anticorrosive centrifuge, filtering until no liquid flows out, and collecting filter cakes and filtrate. And (3) putting the filter cake into a blast oven, setting the temperature to be 70 ℃, drying for 3 hours to obtain sodium diacetate solid, crushing by using a crusher, putting into the oven again, setting the temperature to be 70 ℃, and drying for 4 hours to obtain the food-grade sodium diacetate solid. The recovery scheme comprises the following steps: adding the filter-swinging filtrate acetic acid into a reaction kettle for stirring when the moisture content of the filter-swinging filtrate acetic acid is detected to be lower than 10 percent by a moisture determinator, slowly adding the solid after the reaction of sodium hydroxide in an exhaust gas absorption device, detecting the pH value to be 4.5 on line, heating to 50 ℃, reacting for 5 hours, crystallizing after the reaction is finished, cooling to 20 ℃ while stirring, and adding the reaction solution for corrosion prevention after the crystallization is carried out for 2 hours.

Claims (6)

1. A method for synthesizing edible sodium diacetate is characterized by comprising the following steps,
the method comprises the following steps: adding acetic acid into a reaction kettle, stirring, slowly adding sodium carbonate solid powder, detecting the pH range to be 4.5-5.0 on line, heating to 50-70 ℃, reacting for 3-5 hours, after the reaction is finished, crystallizing, cooling to 20-30 ℃ while stirring, crystallizing for 2-3 hours, adding the reaction liquid into a centrifuge, performing spin filtration until no liquid flows out, and collecting filter cakes and filtrate. And putting the filter cake into an oven, setting the temperature to be 70-80 ℃, drying for 2-3 hours to obtain sodium diacetate solid, cooling, crushing by using a crusher, putting into the oven again, setting the temperature to be 60-70 ℃, and drying for 4-5 hours to obtain the food-grade sodium diacetate solid.
Step two: and (5) a recycling step, namely filling sodium hydroxide solid in the reaction kettle in the step one for tail gas absorption, and reacting with the filtrate acetic acid subjected to the filter throwing in the step one when the sodium hydroxide is completely consumed. The steps are the same as the first step.
2. A method for synthesizing edible sodium diacetate is characterized in that a centrifuge used in the step one is an antiseptic centrifuge.
3. A method for synthesizing edible sodium diacetate is characterized in that the oven used in the step one is a blast oven.
4. A method for synthesizing edible sodium diacetate is characterized in that the complete reaction of sodium hydroxide is completed after the consumption in the second step.
5. A method for synthesizing edible sodium diacetate is characterized in that the content of water in acetic acid in the filtrate in the second step is not more than 10%.
6. A method for synthesizing edible sodium diacetate is characterized in that more than 10 percent of water in acetic acid in the filtrate in the second step is removed by molecular sieve.
CN202110843186.7A 2021-07-26 2021-07-26 Synthesis method of edible sodium diacetate Pending CN113493375A (en)

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CN202110843186.7A CN113493375A (en) 2021-07-26 2021-07-26 Synthesis method of edible sodium diacetate

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CN202110843186.7A CN113493375A (en) 2021-07-26 2021-07-26 Synthesis method of edible sodium diacetate

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CN113493375A true CN113493375A (en) 2021-10-12

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114933526A (en) * 2022-06-02 2022-08-23 肖家福 Preparation process of feed-grade sodium diacetate

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1765867A (en) * 2005-11-24 2006-05-03 湖南株洲化工集团有限责任公司 Sodium Diacetate production method
CN103694102A (en) * 2014-01-13 2014-04-02 南通奥凯生物技术开发有限公司 Method for preparing sodium diacetate
CN106187744A (en) * 2016-07-14 2016-12-07 南通中兴多元复合钢管有限公司 The method manufacturing sodium diacetate
CN110229060A (en) * 2019-06-26 2019-09-13 连云港树人科创食品添加剂有限公司 A kind of preparation method of food-grade sodium Diacetate
WO2020029113A1 (en) * 2018-08-08 2020-02-13 南通奥凯生物技术开发有限公司 Specialized production line device for high-purity sodium diacetate, and operation method
CN112409162A (en) * 2020-11-23 2021-02-26 南通奥凯生物技术开发有限公司 Preparation process of high-purity feed mildew preventive sodium diacetate

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1765867A (en) * 2005-11-24 2006-05-03 湖南株洲化工集团有限责任公司 Sodium Diacetate production method
CN103694102A (en) * 2014-01-13 2014-04-02 南通奥凯生物技术开发有限公司 Method for preparing sodium diacetate
CN106187744A (en) * 2016-07-14 2016-12-07 南通中兴多元复合钢管有限公司 The method manufacturing sodium diacetate
WO2020029113A1 (en) * 2018-08-08 2020-02-13 南通奥凯生物技术开发有限公司 Specialized production line device for high-purity sodium diacetate, and operation method
CN110229060A (en) * 2019-06-26 2019-09-13 连云港树人科创食品添加剂有限公司 A kind of preparation method of food-grade sodium Diacetate
CN112409162A (en) * 2020-11-23 2021-02-26 南通奥凯生物技术开发有限公司 Preparation process of high-purity feed mildew preventive sodium diacetate

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114933526A (en) * 2022-06-02 2022-08-23 肖家福 Preparation process of feed-grade sodium diacetate

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