CN113493375A - Synthesis method of edible sodium diacetate - Google Patents
Synthesis method of edible sodium diacetate Download PDFInfo
- 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
- Authority
- CN
- China
- Prior art keywords
- sodium diacetate
- synthesizing
- acetic acid
- reaction
- edible
- 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
- 239000001632 sodium acetate Substances 0.000 title claims abstract description 23
- 235000017454 sodium diacetate Nutrition 0.000 title claims abstract description 22
- OPGYRRGJRBEUFK-UHFFFAOYSA-L disodium;diacetate Chemical compound [Na+].[Na+].CC([O-])=O.CC([O-])=O OPGYRRGJRBEUFK-UHFFFAOYSA-L 0.000 title claims abstract 12
- 238000001308 synthesis method Methods 0.000 title description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 16
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract description 5
- 238000001914 filtration Methods 0.000 claims abstract description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 23
- 239000007787 solid Substances 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 11
- 239000012065 filter cake Substances 0.000 claims description 6
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000012295 chemical reaction liquid Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 230000002421 anti-septic effect Effects 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- 239000002808 molecular sieve Substances 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000005265 energy consumption Methods 0.000 abstract 1
- 238000003912 environmental pollution Methods 0.000 abstract 1
- 239000012452 mother liquor Substances 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 description 11
- 239000007789 gas Substances 0.000 description 4
- QNPCWVPCAXGWPL-UHFFFAOYSA-L disodium hydrogen carbonate acetate Chemical compound [Na+].[Na+].CC([O-])=O.OC([O-])=O QNPCWVPCAXGWPL-UHFFFAOYSA-L 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005536 corrosion prevention Methods 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 210000005056 cell body Anatomy 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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
Landscapes
- 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
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.
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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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CN202110843186.7A Pending CN113493375A (en) | 2021-07-26 | 2021-07-26 | Synthesis method of edible sodium diacetate |
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Cited By (1)
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)
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 |
-
2021
- 2021-07-26 CN CN202110843186.7A patent/CN113493375A/en active Pending
Patent Citations (6)
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)
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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