CN106187744A - The method manufacturing sodium diacetate - Google Patents
The method manufacturing sodium diacetate Download PDFInfo
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- CN106187744A CN106187744A CN201610557624.2A CN201610557624A CN106187744A CN 106187744 A CN106187744 A CN 106187744A CN 201610557624 A CN201610557624 A CN 201610557624A CN 106187744 A CN106187744 A CN 106187744A
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- Prior art keywords
- reactor
- acetic acid
- sodium diacetate
- glacial acetic
- sodium
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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
Abstract
The invention discloses with method that gas phase reaction is main manufacture sodium diacetate, its step is as follows: first the sodium carbonate measured is put in reactor and opens stirring, then when 40 DEG C by the mass ratio of sodium carbonate and glacial acetic acid be 1:2.125 slowly in reactor drip glacial acetic acid, during dropping control temperature between 75～90 DEG C；Feed intake after terminating, by this course of reaction insulation reaction 30min at 75～90 DEG C；After gas phase reaction terminates, after negative pressure drying, cooling, i.e. obtain sodium diacetate crystalline particle.The present invention manufactures sodium diacetate by the gas phase reaction process in horizontal reactor, need not plus solvent medium, gained crystalline product granule is uniform, and good dispersion, production technology is simple, raw material is easy to get, production cost is low, high, simple to operate without " three wastes " discharge, product purity in course of reaction.
Description
Technical field
The present invention relates to the manufacture method of sodium diacetate, especially with method that gas phase reaction is main manufacture sodium diacetate.
Background technology
Sodium diacetate is multi-functional edible chemical, is mainly used as food and the preservative of feed industry, antifungus agent, chela
Mixture, flavoring agent, PH regulator, meat products preservative agent, be also the primary raw material of composite type mouldproof agent.There is high-effect anti-mould, guarantor
Fresh, have additional nutrients the effects such as value, be not only suitable for the safe storage of foodstuff seed, be also practically applicable to the anti-mildew fresh-keeping of feedstuff, increase
Nutritive value, improve palatability, be particularly suited for Semen Maydis, corn fresh-keeping.The most domestic and international large-scale production sodium diacetate
Technique mainly has sodium acetate-method of acetic acid, acetic acid～acetic anhydride-sodium carbonate method and acetic acid-caustic soda method etc., but, due to
Each reactant disposably adds in course of reaction, all there is the bad control of course of reaction, and response time length and mother solution return
Receive the problems such as difficult.Additionally, existing reactor is mostly reactor, it is anti-that traditional reactor is mostly used for liquid liquid
Should, do not possess gas-solid, liquid and solid phase reaction ability, (gas-solid reaction tradition reactor sealing property is not certain limitation
Good, reaction is not exclusively；Liquid and solid phase reaction equally exists this problem).Therefore existing these produce sodium diacetate techniques need to be changed
Enter.
Summary of the invention
In the case of the technical problem to be solved in the present invention is to provide for being not added with any solvent, with glacial acetic acid and sodium carbonate with
The method that gas phase reaction produces sodium diacetate.
For solving above-mentioned technical problem, the technical solution used in the present invention is: the method manufacturing sodium diacetate, including throwing
Material, dry and cooling step, its innovative point is: produce sodium diacetate with glacial acetic acid and sodium carbonate with gas phase reaction；
Material addition step: first the sodium carbonate measured is put in horizontal reactor and opens stirring, then 20～55
DEG C time slowly in reactor drip glacial acetic acid, during dropping control temperature between 75～90 DEG C, described sodium carbonate and glacial acetic acid
Mass ratio be 1:2.125；
Insulation reaction: after the end that feeds intake, insulation reaction 28～32min at 75～90 DEG C.Further, first measuring
Sodium carbonate put in horizontal reactor, feed intake carry out half time, open reactor stirring, open soda pop after the end that feeds intake and mix
Reactor is heated by clutch, hot water circulating pump and reacting by heating device, when in question response device, gas phase temperature rises to 40 DEG C, starts
Being that 1:2.125 slowly drips glacial acetic acid in reactor by the mass ratio of sodium carbonate and glacial acetic acid, time for adding is little less than 1
Time, control dropping temperature between 75～90 DEG C.
Further, described step (2) is particularly as follows: after glacial acetic acid completion of dropwise addition, protect course of reaction at 75～90 DEG C
Temperature reaction 30min, then samples censorship, and free acetic acid content need to be at 39.0w%～41.0w%, and sodium acetate content need to be
58.0w%～60.0w%.
Further, in described step (3) under the conditions of-0.03～-0.05MPa be vacuum dried, drying time 1.5～
3h, the moisture content≤2.0w% of dried powder.
Further, material cool time 2～select 40～60 mesh sieve after 3 hours again in described step (3).
Further, after described step (3), packaging process is also included.
Compared with existing production technology, it is an advantage of the current invention that: reacted by the gas phase in horizontal reactor
Journey manufactures sodium diacetate, improves parallel reaction selectivity and reaction completeness, strengthening reaction interphase mass transfer；At horizontal reactor
Interior gas phase reaction process manufactures sodium diacetate and need not plus solvent medium, and gained crystalline product granule is uniform, and dispersibility
Good, production technology is simple, raw material is easy to get, production cost is low, in course of reaction without " three wastes " discharge, simple to operate.Reaction has
Sound response selectivity and safety, and the sodium diacetate white appearance produced, crystallize regular, and product purity is high, stay in grade.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme is elaborated.
Embodiment 1
(1) feed intake: open powder technology sodium carbonate feeding system, open reactor sodium carbonate and feed intake valve, will measure
Sodium carbonate join in horizontal reactor.Sodium carbonate feed intake half time, open reactor stirring, feed intake end after, close throw
Material system, opens steam heater, hot water circulating pump, reacting by heating device.
When gas phase temperature rises to 40 DEG C in question response device, open jacket condensator Inlet and outlet water valve, open exhaust-valve, close
Reactor is to the valve of pipe bundle condenser, and starting according to the mass ratio of sodium carbonate and glacial acetic acid is that 1:2.125 drips glacial acetic acid, drips
The speed added is 4.5Kg/min, guards against slug, makes temperature control at 78 DEG C；Treat that temperature is normal, without strip phenomenon, strengthen dropping
Speed, its speed is 6Kg/min, goes out if any material strip, slows down rate of addition, and time for adding is less than 1 hour.
(2) insulation: be incubated 28min after completion of dropwise addition, sample censorship, free acetic acid content 39.4w%, sodium acetate content
58.2w%, after sample passes, emptying is closed, and prepares next step and is dried.
(3) it is dried: open vacuum equipment, opens reactor to the valve of pipe bundle condenser, open pipe bundle condenser turnover
Penstock, gas-liquid separator turnover valve, control vacuum is-0.03MPa, controls temperature of reactor 80 DEG C, jacket temperature 100
℃.Be dried 1.5 hours, sample qualified after prepare blowing, during negative pressure drying, the acetic acid evaporated in reactor is condensed
Device condensation, gas-liquid separator separates obtain 8% spirit of vinegar, flow to spirit of vinegar receiving slit.
(4) cooling: temperature to 40 DEG C, is discharged to interior thermal agitation cold, opens cooling water valve, cools down 2～3 hours.
(5) packaging: after 40 mesh sieve, pack.
Recording product purity is 99.91%.
Embodiment 2
(1) feed intake: open powder technology sodium carbonate feeding system, open reactor sodium carbonate and feed intake valve, will measure
Sodium carbonate join in horizontal reactor.Sodium carbonate feed intake half time, open reactor stirring, feed intake end after, close throw
Material system, opens steam heater, hot water circulating pump, reacting by heating device.
When gas phase temperature rises to 40 DEG C in question response device, open jacket condensator Inlet and outlet water valve, open exhaust-valve, close
Reactor is to the valve of pipe bundle condenser, and starting according to the mass ratio of sodium carbonate and glacial acetic acid is that 1:2.125 drips glacial acetic acid, drips
The speed added is 4.5Kg/min, guards against slug, makes temperature control at 88 DEG C；Treat that temperature is normal, without strip phenomenon, strengthen dropping
Speed, its speed is 6Kg/min, goes out if any material strip, slows down rate of addition, and time for adding is less than 1 hour.
(2) insulation: be incubated 32min after completion of dropwise addition, sample censorship, free acetic acid content 39.3w%, sodium acetate content
58.5w%, after sample passes, emptying is closed, and prepares next step and is dried.
(3) it is dried: open vacuum equipment, opens reactor to the valve of pipe bundle condenser, open pipe bundle condenser turnover
Penstock, gas-liquid separator turnover valve, control vacuum is-0.05MPa, controls temperature of reactor 80 DEG C, jacket temperature 100
DEG C, be dried 2 hours, sample qualified after prepare blowing, during negative pressure drying, the condensed device of acetic acid evaporated in reactor
Condensation, gas-liquid separator separates obtain 8% spirit of vinegar, flow to spirit of vinegar receiving slit.
(4) cooling: during temperature of charge to 40 DEG C, is discharged to interior thermal agitation cold, opens cooling water valve, cools down 3 hours.
(5) packaging: after 60 mesh sieve, pack.
Recording product purity is 99.95%.
Comparative example 1
Sodium acetate and acetic acid liquid phase reactor in ethanol, this method complex manufacturing, investment of production equipment is big, production cost
Height, and the purity that product purity obtains not as the inventive method is high.
(1) feed intake: open 5000L reactor ethanol and feed intake valve, the ethanol measured is joined in reactor.Ethanol
After having fed intake, open reactor stirring, open reactor manhole, in reactor, add the sodium acetate measured, sodium acetate
Feed intake and after terminating, open reactor steam heating valve, reacting by heating still.
When question response temperature in the kettle rises to 40 DEG C, open jacket condensator Inlet and outlet water valve, open exhaust-valve, close reaction
Still, to the valve of pipe bundle condenser, starts to drip glacial acetic acid, and the dripping quantity of glacial acetic acid is 400Kg, and the speed of dropping is 3Kg/
Min, guards against slug, makes temperature control at 88 DEG C；Treating that temperature is normal, without strip phenomenon, strengthen rate of addition, its speed is 5Kg/
Min, goes out if any material strip, slows down rate of addition, and time for adding is less than 2 hours.
(2) insulation: be incubated 15min after completion of dropwise addition, sample censorship, free acetic acid content 39.8w%, sodium acetate content
58.1w%, after sample passes, emptying is closed, and prepares next step and is dried.
(3) it is dried: open vacuum equipment, opens reactor to the valve of pipe bundle condenser, open pipe bundle condenser turnover
Penstock, gas-liquid separator turnover valve, control vacuum is-0.05MPa, controls temperature of reactor 80 DEG C, jacket temperature 100
DEG C, be dried 2 hours, sample qualified after prepare blowing, during negative pressure drying, the condensed device of acetic acid evaporated in reactor
Condensation, gas-liquid separator separates obtain 8% spirit of vinegar, flow to spirit of vinegar receiving slit.
(4) cooling: during temperature of charge to 40 DEG C, be discharged to pallet.
(5) packaging: after 60 mesh sieve, pack.
Recording product purity is 98.95%.
It is pointed out that above-mentioned preferred embodiment is only technology design and the feature of the explanation present invention, its object is to
Allow person skilled in the art will appreciate that present disclosure and to implement according to this, the protection of the present invention can not be limited with this
Scope.All equivalence changes made according to spirit of the invention or modification, all should contain within protection scope of the present invention.
Claims (7)
1. the method manufacturing sodium diacetate, including feeding intake, being dried and cooling step, it is characterised in that: with glacial acetic acid and sodium carbonate
Sodium diacetate is produced with gas phase reaction；
Material addition step: first the sodium carbonate measured is put in horizontal reactor and opens stirring, then when 20～55 DEG C
Slowly dripping glacial acetic acid in reactor, during dropping, control temperature is between 75～90 DEG C, described sodium carbonate and the matter of glacial acetic acid
Amount ratio is 1:2.125；
Insulation reaction: after the end that feeds intake, insulation reaction 28～32min at 75～90 DEG C.
The method of manufacture sodium diacetate the most according to claim 1, it is characterised in that: first the sodium carbonate measured is put into
In horizontal reactor, feed intake carry out half time, open reactor stirring, open steam heater and hot water after the end that feeds intake and follow
Ring pump and to reactor heat, when gas phase temperature rises to 40 DEG C in horizontal reactor, start the matter by sodium carbonate and glacial acetic acid
Amount than slowly dripping glacial acetic acid in reactor for 1:2.125, and time for adding is less than 1 hour, control dropping temperature 75～
Between 90 DEG C.
The method of manufacture sodium diacetate the most according to claim 1, it is characterised in that: after glacial acetic acid completion of dropwise addition, will be anti-
Answering process insulation reaction 30min at 75～90 DEG C, then sample censorship, free acetic acid content need to be at 39.0w%～41.0w%
Between, sodium acetate content need to be between 58.0w%～60.0w%.
The method of manufacture sodium diacetate the most according to claim 1, it is characterised in that: after the reaction of described gas phase terminates, warp
Sodium diacetate crystalline particle is obtained after negative pressure drying, cooling.
The method of manufacture sodium diacetate the most according to claim 4, it is characterised in that: in-0.03～-0.05MPa condition
Lower vacuum drying, drying time 1.5～3h, the moisture content≤2.0w% of dried powder.
The method of manufacture sodium diacetate the most according to claim 4, it is characterised in that: material cool time 2～after 3 hours
Select 40～60 mesh sieve again.
The method of manufacture sodium diacetate the most according to claim 1, it is characterised in that: also include sacker after material cooling
Sequence.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610557624.2A CN106187744A (en) | 2016-07-14 | 2016-07-14 | The method manufacturing sodium diacetate |
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| CN201610557624.2A CN106187744A (en) | 2016-07-14 | 2016-07-14 | The method manufacturing sodium diacetate |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN108059595A (en) * | 2017-11-20 | 2018-05-22 | 连云港诺信食品配料有限公司 | A kind of preparation process of diacetic acid potassium |
| CN108218693A (en) * | 2016-12-15 | 2018-06-29 | 刘辉 | A kind of food, feed addictive sodium Diacetate |
| CN108218689A (en) * | 2016-12-15 | 2018-06-29 | 刘辉 | A kind of grain mold proof insect-proof agent 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 |
Citations (3)
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| JPH10259133A (en) * | 1997-03-14 | 1998-09-29 | Nikkiso Co Ltd | Particulate agent for dialysis and its production |
| 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 |
| CN104892397A (en) * | 2015-04-02 | 2015-09-09 | 秦健 | Method for producing sodium diacetate |
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2016
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Patent Citations (3)
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| JPH10259133A (en) * | 1997-03-14 | 1998-09-29 | Nikkiso Co Ltd | Particulate agent for dialysis and its production |
| 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 |
| CN104892397A (en) * | 2015-04-02 | 2015-09-09 | 秦健 | Method for producing sodium diacetate |
Non-Patent Citations (2)
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| TIAN MINGLEI ET AL: "Direct synthesis of sodium diacetate in industrial production process control", 《 JOURNAL OF THE KOREAN CHEMICAL SOCIETY》 * |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108218693A (en) * | 2016-12-15 | 2018-06-29 | 刘辉 | A kind of food, feed addictive sodium Diacetate |
| CN108218689A (en) * | 2016-12-15 | 2018-06-29 | 刘辉 | A kind of grain mold proof insect-proof agent 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 |
| CN108059595A (en) * | 2017-11-20 | 2018-05-22 | 连云港诺信食品配料有限公司 | A kind of preparation process of diacetic acid potassium |
| 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 |
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