CN103694102A - Method for preparing sodium diacetate - Google Patents
Method for preparing sodium diacetate Download PDFInfo
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- CN103694102A CN103694102A CN201410013676.4A CN201410013676A CN103694102A CN 103694102 A CN103694102 A CN 103694102A CN 201410013676 A CN201410013676 A CN 201410013676A CN 103694102 A CN103694102 A CN 103694102A
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- acetic acid
- sodium diacetate
- glacial acetic
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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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Abstract
The invention discloses a method for preparing sodium diacetate mainly through a gas-phase reaction, which comprises the following steps of firstly adding metered sodium carbonate into a reactor and stirring; slowly dropwise adding glacial acetic acid into the reactor at 40 DEG C according to a mass ratio of sodium carbonate to glacial acetic acid of 1:2.125 while controlling the temperature at 75-90 DEG C; after the feeding, performing a thermal insulation reaction of the reaction process for 30 minutes at 75-90 DEG C; after the gas-phase reaction, performing negative-pressure drying and cooling to obtain crystalline particles of sodium diacetate. According to the method disclosed by the invention, sodium diacetate is prepared through a gas-phase reaction process in a horizontal reactor without adding a solvent medium, and the obtained crystalline product particles are uniform and have good dispersity; moreover, the production process is simple, the raw materials are easily available, the production cost is low, the discharge of 'three wastes' in the reaction process is avoided, the product purity is high, and the operation is simple.
Description
Technical field
The present invention relates to a kind of manufacture method of sodium Diacetate, especially a kind ofly take the method for gas-phase reaction as main manufacture sodium Diacetate.
Background technology
Sodium Diacetate is a kind of multi-functional edible chemical,, as sanitas, mould inhibitor, sequestrant, seasonings, PH conditioning agent, the meat product preservatives of food and feed industry, is mainly also the main raw material of composite type mouldproof agent.There is high-effect anti-mould, fresh-keeping, the effects such as value that have additional nutrients, be both applicable to the safe storage of foodstuff seed, be also practically applicable to the anti-mildew fresh-keeping of feed, the value that has additional nutrients, improve palatability, be particularly useful for the fresh-keeping of corn, cereal.The technique of large-scale production sodium Diacetate mainly contains sodium-acetate-method of acetic acid, acetic acid～acetic anhydride-sodium carbonate method and acetic acid-sodium hydroxide method etc. both at home and abroad at present; yet; due to the disposable interpolation in reaction process of each reactant; all problems such as the bad control of reaction process, long reaction time and mother liquor recovery difficulty that exist.In addition, existing reactor is mostly reactor, and traditional reactor is used for greatly the reaction of liquid-liquid, solid do not possess gas-, liquid-solid state reaction ability, (gas-solid reaction tradition reactor sealing property is bad, and reaction is incomplete certain limitation; There is this problem in liquid and solid phase reaction equally.Therefore the existing technique that these produce sodium Diacetate haves much room for improvement.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of in the situation that not adding any solvent, with Glacial acetic acid and sodium carbonate, produces the method for sodium Diacetate with gas-phase reaction.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of method of manufacturing sodium Diacetate, and comprise and feed intake, be dried and cooling step, its innovative point is: with Glacial acetic acid and sodium carbonate, with gas-phase reaction, produce sodium Diacetate;
Step feeds intake: first the sodium carbonate measuring is put in horizontal reactor and opened and stir, then in the time of 35～45 ℃, slowly in reactor, drip Glacial acetic acid, during dropping, control temperature between 75～90 ℃, the mass ratio of described sodium carbonate and Glacial acetic acid is 1:2.125;
Insulation reaction: feed intake after end, insulation reaction 28～32min at 75～90 ℃.Further, first the sodium carbonate measuring is dropped in horizontal reactor, carry out a half feeding intake, unlatching reactor stirs, rear steam heater, hot water circulating pump and the reactor heating opened of the end that feeds intake heats reactor, and when in question response device, gas phase temperature rises to 40 ℃, starting by the mass ratio of sodium carbonate and Glacial acetic acid is that 1:2.125 slowly drips Glacial acetic acid in reactor, time for adding is no more than 1 hour, controls dropping temperature between 75～90 ℃.
Further, described step (2) is specially: Glacial acetic acid by reaction process insulation reaction 30min at 75～90 ℃, then samples censorship after dripping and finishing, free acetic acid content need be at 39.0 w%～41.0 w%, and sodium acetate content need be at 58.0 w%～60.0 w%.
Further, vacuum-drying under-0.03～-0.05MPa condition in described step (3), time of drying, 1.5～3h, was dried moisture content≤2.0 w% of powder afterwards.
Further, in described step (3), material selects 40～60 mesh sieves to sieve again after 2～3 hours cooling times.
Further, in described step (3), also comprise afterwards packaging process.
Compare with existing production technique, the invention has the advantages that: by the gas phase reaction process in horizontal reactor, manufacture sodium Diacetate, improved parallel reactor selectivity and reacting completely property, strengthening reaction interphase mass transfer; Gas phase reaction process in horizontal reactor is manufactured sodium Diacetate does not need plus solvent medium, gained crystalline product uniform particles, and good dispersity, production technique is simple, raw material is easy to get, production cost is low, in reaction process without " three wastes " discharge, simple to operate.Reaction has sound response selectivity and security, and the sodium Diacetate outward appearance of producing is pure white, and crystallization is regular, and product purity is high, stay in grade.
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is elaborated.
embodiment 1
(1) feed intake: open powder technology sodium carbonate feeding system, open the reactor sodium carbonate valve that feeds intake, the sodium carbonate measuring is joined in horizontal reactor.The sodium carbonate half that feeds intake, opens reactor and stirs, and after feeding intake and finishing, closes feeding system, opens steam heater, hot water circulating pump, reactor heating.
When in question response device, gas phase temperature rises to 40 ℃, open jacket condensator Inlet and outlet water valve, open exhaust-valve, off-response device is to the valve of pipe bundle condenser, beginning is that 1:2.125 drips Glacial acetic acid according to the mass ratio of sodium carbonate and Glacial acetic acid, the speed dripping is 4.5Kg/min, guards against punching material, makes temperature be controlled at 78 ℃; Treat that temperature is normal, without band material phenomenon, strengthen rate of addition, its speed is 6Kg/min, if any material strip, goes out to slow down rate of addition, and time for adding is no more than 1 hour.
(2) insulation: drip and finish rear insulation 28min, sampling censorship, free acetic acid content 39.4 w%, sodium acetate content 58.2 w%, qualified rear emptying the closing of sample, prepares next step and is dried.
(3) dry: open vacuum apparatus, open reactor to the valve of pipe bundle condenser, open pipe bundle condenser Inlet and outlet water valve, gas-liquid separator turnover valve, controlling vacuum tightness is-0.03MPa to control 80 ℃ of temperature of reactor, 100 ℃ of jacket temperatures.Dry 1.5 hours, sample qualified rear preparation blowing, in negative pressure drying process, the acetic acid evaporating in reactor obtains 8% dilute acetic acid through condenser condenses, gas-liquid separator separates, flow to dilute acetic acid Receiving bin.
(4) cooling: temperature to 40 ℃, be discharged to the cold machine of interior heat agitated, open cooling water valve, cooling 2～3 hours.
(5) packing: after 40 mesh sieves sieve, pack.
Recording product purity is 99.91%.
embodiment 2
(1) feed intake: open powder technology sodium carbonate feeding system, open the reactor sodium carbonate valve that feeds intake, the sodium carbonate measuring is joined in horizontal reactor.The sodium carbonate half that feeds intake, opens reactor and stirs, and after feeding intake and finishing, closes feeding system, opens steam heater, hot water circulating pump, reactor heating.
When in question response device, gas phase temperature rises to 40 ℃, open jacket condensator Inlet and outlet water valve, open exhaust-valve, off-response device is to the valve of pipe bundle condenser, beginning is that 1:2.125 drips Glacial acetic acid according to the mass ratio of sodium carbonate and Glacial acetic acid, the speed dripping is 4.5Kg/min, guards against punching material, makes temperature be controlled at 88 ℃; Treat that temperature is normal, without band material phenomenon, strengthen rate of addition, its speed is 6Kg/min, if any material strip, goes out to slow down rate of addition, and time for adding is no more than 1 hour.
(2) insulation: drip and finish rear insulation 32min, sampling censorship, free acetic acid content 39.3 w%, sodium acetate content 58.5 w%, qualified rear emptying the closing of sample, prepares next step and is dried.
(3) dry: to open vacuum apparatus, open reactor to the valve of pipe bundle condenser, open pipe bundle condenser Inlet and outlet water valve, gas-liquid separator turnover valve, controlling vacuum tightness is-0.05MPa to control 80 ℃ of temperature of reactor, 100 ℃ of jacket temperatures, dry 2 hours, sample qualified rear preparation blowing, in negative pressure drying process, the acetic acid evaporating in reactor obtains 8% dilute acetic acid through condenser condenses, gas-liquid separator separates, flow to dilute acetic acid Receiving bin.
(4) cooling: during temperature of charge to 40 ℃, to be discharged to the cold machine of interior heat agitated, to open cooling water valve, cooling 3 hours.
(5) packing: after 60 mesh sieves sieve, pack.
Recording product purity is 99.95%.
Comparative example 1
Sodium acetate and acetic acid liquid phase reaction in ethanol, this method complex manufacturing, investment of production equipment is large, and production cost is high, and the purity that product purity obtains not as the inventive method is high.
(1) feed intake: open the 5000L reactor ethanol valve that feeds intake, the ethanol measuring is joined in reactor.After ethanol has fed intake, open reactor and stir, open reactor manhole, in reactor, add the sodium acetate measuring, sodium acetate is opened reactor steam heating valve, reacting by heating still after feeding intake and finishing.
When question response temperature in the kettle rises to 40 ℃, open jacket condensator Inlet and outlet water valve, open exhaust-valve, off-response still, to the valve of pipe bundle condenser, starts to drip Glacial acetic acid, and the dripping quantity of Glacial acetic acid is 400Kg, the speed dripping is 3Kg/min, guards against punching material, makes temperature be controlled at 88 ℃; Treat that temperature is normal, without band material phenomenon, strengthen rate of addition, its speed is 5Kg/min, if any material strip, goes out to slow down rate of addition, and time for adding is no more than 2 hours.
(2) insulation: drip and finish rear insulation 15min, sampling censorship, free acetic acid content 39.8 w%, sodium acetate content 58.1 w%, qualified rear emptying the closing of sample, prepares next step and is dried.
(3) dry: to open vacuum apparatus, open reactor to the valve of pipe bundle condenser, open pipe bundle condenser Inlet and outlet water valve, gas-liquid separator turnover valve, controlling vacuum tightness is-0.05MPa to control 80 ℃ of temperature of reactor, 100 ℃ of jacket temperatures, dry 2 hours, sample qualified rear preparation blowing, in negative pressure drying process, the acetic acid evaporating in reactor obtains 8% dilute acetic acid through condenser condenses, gas-liquid separator separates, flow to dilute acetic acid Receiving bin.
(4) cooling: during temperature of charge to 40 ℃, to be discharged to pallet.
(5) packing: after 60 mesh sieves sieve, pack.
Recording product purity is 98.95%.
It is pointed out that above-mentioned preferred embodiment is only explanation technical conceive of the present invention and feature, its object is to allow person skilled in the art can understand content of the present invention and implement according to this, can not limit the scope of the invention with this.All equivalences that spirit is done according to the present invention change or modify, within all should being encompassed in protection scope of the present invention.
Claims (7)
1. manufacture a method for sodium Diacetate, comprise and feed intake, be dried and cooling step, it is characterized in that: with Glacial acetic acid and sodium carbonate, with gas-phase reaction, produce sodium Diacetate;
Step feeds intake: first the sodium carbonate measuring is put in horizontal reactor and opened and stir, then in the time of 35～45 ℃, slowly in reactor, drip Glacial acetic acid, during dropping, control temperature between 75～90 ℃, the mass ratio of described sodium carbonate and Glacial acetic acid is 1:2.125;
Insulation reaction: feed intake after end, insulation reaction 28～32min at 75～90 ℃.
2. a kind of method of manufacturing sodium Diacetate according to claim 1, it is characterized in that: first the sodium carbonate measuring is dropped in horizontal reactor, carry out a half feeding intake, unlatching reactor stirs, feed intake and finish rear unlatching steam heater and hot water circulating pump and reactor is heated, when in horizontal reactor, gas phase temperature rises to 40 ℃, starting by the mass ratio of sodium carbonate and Glacial acetic acid is that 1:2.125 slowly drips Glacial acetic acid in reactor, time for adding is no more than 1 hour, controls dropping temperature between 75～90 ℃.
3. a kind of method of manufacturing sodium Diacetate according to claim 1, it is characterized in that: after Glacial acetic acid drips and finishes, by reaction process insulation reaction 30min at 75～90 ℃, then sample censorship, free acetic acid content need be between 39.0 w%～41.0 w%, and sodium acetate content need be between 58.0 w%～60.0 w%.
4. a kind of method of manufacturing sodium Diacetate according to claim 1, is characterized in that: after described gas-phase reaction finishes, through negative pressure drying, after cooling, obtain sodium Diacetate crystalline particle.
5. a kind of method of manufacturing sodium Diacetate according to claim 4, is characterized in that: vacuum-drying under-0.03～-0.05MPa condition, time of drying, 1.5～3h, was dried moisture content≤2.0 w% of powder afterwards.
6. a kind of method of manufacturing sodium Diacetate according to claim 4, is characterized in that: material selects 40～60 mesh sieves to sieve again after 2～3 hours cooling times.
7. a kind of method of manufacturing sodium Diacetate according to claim 1, is characterized in that: after material is cooling, also comprise packaging process.
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| CN201410013676.4A CN103694102B (en) | 2014-01-13 | 2014-01-13 | A kind of method manufacturing sodium Diacetate |
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| CN201410013676.4A CN103694102B (en) | 2014-01-13 | 2014-01-13 | A kind of method manufacturing sodium Diacetate |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104492366A (en) * | 2014-12-30 | 2015-04-08 | 南通奥凯生物技术开发有限公司 | Special high-purity sodium diacetate production line device and operation method |
| CN104892397A (en) * | 2015-04-02 | 2015-09-09 | 秦健 | Method for producing 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 |
| CN106946696A (en) * | 2017-04-02 | 2017-07-14 | 南通博泰美术图案设计有限公司 | The method for manufacturing sodium Diacetate |
| CN107245033A (en) * | 2017-06-25 | 2017-10-13 | 南通峰巢工业设计有限公司 | The method for manufacturing sodium Diacetate |
| CN108218689A (en) * | 2016-12-15 | 2018-06-29 | 刘辉 | A kind of grain mold proof insect-proof agent sodium Diacetate |
| CN108218693A (en) * | 2016-12-15 | 2018-06-29 | 刘辉 | A kind of food, feed addictive 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 |
| CN113493375A (en) * | 2021-07-26 | 2021-10-12 | 连云港诺信食品配料有限公司 | Synthesis method of edible sodium diacetate |
| DE102021121665B3 (en) | 2021-08-20 | 2022-08-11 | Few Chemicals Gmbh | Process for the production of sodium diacetate, sodium acetate and/or sodium acetate trihydrate |
Citations (1)
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| CN1280120A (en) * | 1999-07-12 | 2001-01-17 | 河北省邢台市人民制药厂 | Process for preparing sodium diacetate |
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2014
- 2014-01-13 CN CN201410013676.4A patent/CN103694102B/en active Active
Patent Citations (1)
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|---|---|---|---|---|
| CN1280120A (en) * | 1999-07-12 | 2001-01-17 | 河北省邢台市人民制药厂 | Process for preparing sodium diacetate |
Non-Patent Citations (1)
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| 王霞等: ""一步法生产双乙酸钠新工艺"", 《云南化工》, vol. 27, no. 6, 31 December 2000 (2000-12-31), pages 3 - 4 * |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104492366A (en) * | 2014-12-30 | 2015-04-08 | 南通奥凯生物技术开发有限公司 | Special high-purity sodium diacetate production line device and operation method |
| CN104492366B (en) * | 2014-12-30 | 2016-04-20 | 南通奥凯生物技术开发有限公司 | A kind of high-purity sodium Diacetate special production line device and method of operating |
| CN104892397A (en) * | 2015-04-02 | 2015-09-09 | 秦健 | Method for producing 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 |
| CN108218689A (en) * | 2016-12-15 | 2018-06-29 | 刘辉 | A kind of grain mold proof insect-proof agent sodium Diacetate |
| CN108218693A (en) * | 2016-12-15 | 2018-06-29 | 刘辉 | A kind of food, feed addictive sodium Diacetate |
| CN106946696A (en) * | 2017-04-02 | 2017-07-14 | 南通博泰美术图案设计有限公司 | The method for manufacturing sodium Diacetate |
| CN107245033A (en) * | 2017-06-25 | 2017-10-13 | 南通峰巢工业设计有限公司 | The method for 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 |
| CN110229060B (en) * | 2019-06-26 | 2022-02-08 | 连云港树人科创食品添加剂有限公司 | Preparation method of food-grade sodium diacetate |
| CN113493375A (en) * | 2021-07-26 | 2021-10-12 | 连云港诺信食品配料有限公司 | Synthesis method of edible sodium diacetate |
| DE102021121665B3 (en) | 2021-08-20 | 2022-08-11 | Few Chemicals Gmbh | Process for the production of sodium diacetate, sodium acetate and/or sodium acetate trihydrate |
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| CN103694102B (en) | 2015-11-25 |
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