CN109942445A - Beet alkali hydrochlorate synthetic method - Google Patents
Beet alkali hydrochlorate synthetic method Download PDFInfo
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- CN109942445A CN109942445A CN201910141874.1A CN201910141874A CN109942445A CN 109942445 A CN109942445 A CN 109942445A CN 201910141874 A CN201910141874 A CN 201910141874A CN 109942445 A CN109942445 A CN 109942445A
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- beet alkali
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- alkali hydrochlorate
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Abstract
Beet alkali hydrochlorate synthetic method, chloroacetic acid is sequentially added into reaction flask, catalyst, ethyl alcohol, then heat up 100-115 DEG C of reflux, molecular sieve is dehydrated at reflux, 2-8 hours end of reaction, reaction solution is washed with water 2 times, the ethyl chloroacetate separated is evaporated under reduced pressure, ethyl chloride is added in reaction flask, a certain amount of water is added, start to be passed through front three amine gas, it is maintained at 20-45 DEG C, 2-6 hours end of reaction, add hydrochloric acid heating hydrolysis, distill out water and ethyl alcohol therein, 10-15 DEG C of crystallizations of cooling are centrifuged up to beet alkali hydrochlorate.The present invention, which is used, synthesizes ethyl chloride by chloroacetic acid and ethanol raw material, pure ethyl chloride is obtained to pass through again and trimethylamine synthesizing betaine carbethoxy hydrochloride, heating hydrolysis ethyl alcohol is carried out in presence of hydrochloric acid, beet alkali hydrochlorate is precipitated in concentrate cooling, 99% or more beet alkali hydrochlorate purity made from this method, yield reaches 97% or more, and is not in inorganic salts solid waste.
Description
Technical field
The present invention relates to furol biological process and utilization technology fields, and in particular to a kind of beet alkali hydrochlorate synthetic method.
Background technique
Beet alkali hydrochlorate is the general name of a kind of organic compound, also known as betaine HCL, for white to yellowish crystallization
Property powder, taste has moisture absorption in sour and astringent, and soluble easily in water, ethyl alcohol is insoluble in ether, chloroform, meets alkali reaction.Beet alkali salt
Hydrochlorate be it is a kind of it is efficient, high-quality, economical, be widely used in poultry, fowl, aquaculture food attractant-growth promoting auxotype additive.
Beet alkali hydrochlorate production technology is at present with monoxone and sodium hydroxide solution 1:1.2(molar ratio) at 20-40 DEG C
Then neutralization reaction controls temperature and is passed through the quaternized generation glycine betaine of trimethylamine at 15-40 DEG C, then with hydrochloric acid or sulfuric acid into
Row acidification, to reaction solution by vacuum distillation concentration, decrease temperature crystalline.And be centrifuged, drying and packaging obtains beet alkali hydrochlorate, existing
That there are purity is low using chloroacetic acid raw material for technique, will cause beet alkali salt containing impurity such as dichloroacetic acid, acetic acid, trichloroacetic acids
Hydrochlorate purity is not high；Prior art, which is neutralized using chloroacetic acid, is quaternized, a large amount of inorganic salts can be generated by reacting at several steps of salt consolidates
It is useless；Chloroacetic acid is using, with generation acetic acid sodium salt, there are chloroacetic acid hydrolysis in sodium hydroxide, to reduce chloroacetic acid receipts
Rate leads to the situation that purity is low；And prior art after generating glycine betaine hydrochloric acid will precipitation, have the analysis of a large amount of sodium chloride
Out, to cause that product purity is not high or product yield is low.
Summary of the invention
The present invention provides a kind of beet alkali hydrochlorate synthetic methods, are deposited with solving existing beet alkali hydrochlorate production technology
Purity difference, yield is low and leads to the problem of a large amount of inorganic salts solid wastes.
The technical solution adopted by the present invention to solve the technical problems is:
A kind of beet alkali hydrochlorate synthetic method, chloroacetic acid, catalyst, ethyl alcohol are sequentially added into reaction flask, is then heated up
100-115 DEG C of reflux, molecular sieve are dehydrated at reflux, and reaction solution is washed with water 2 times 2-8 hours end of reaction, point
Ethyl chloroacetate out is evaporated under reduced pressure, and ethyl chloride fraction is 72-76 DEG C/0.09kPa, and ethyl chloride is pure
Degree 99%, ethyl chloride yield 96%, wherein chloroacetic acid and ethyl alcohol molar ratio are 1:1.1-2, reaction equation are as follows:
CLCH2COOH + CH3CH2OH CLCH2COOCH2CH3 + H2O
The ethyl chloride that upper step is obtained is added in reaction flask, and a certain amount of water is added, starts to be passed through front three amine gas, body
It is that temperature is maintained at 20-45 DEG C, 2-6 hours end of reaction add hydrochloric acid heating hydrolysis, and 85-100 DEG C of reflux, which are collected, steams
The water and ethyl alcohol distillated, collection finish 10-15 DEG C of cooling crystallizations and are centrifuged up to beet alkali hydrochlorate, beet alkali hydrochlorate purity
99.63%, 94% or more beet alkali hydrochlorate yield, wherein trimethylamine and ethyl chloride mol ratio are as follows: 1.0-1.2:1,
Reaction equation are as follows:
CLCH2COOCH2CH3 + (CH3)N (H3C)NCH2COOCH2CH3·HCL
(H3C)NCH2COOCH2CH3·HCL (H3C)NCH2COOH·HCL + CH3CH2OH
Esterification reaction temperature occurs for above-mentioned chloroacetic acid and ethyl alcohol at 100 DEG C -115 DEG C, chloroacetic acid and ethyl alcohol mol ratio
Are as follows: 1:1.5-2.
This technique of the method for the present invention using first preparing high-purity ethyl chloride, then with the quaternized synthesizing betaine of trimethylamine
Carbethoxy hydrochloride finally hydrolyzes glycine betaine carbethoxy hydrochloride beet alkali hydrochlorate, is from start to end not in that inorganic salts are raw
Produce, ethyl chloride content is high, other impurities appearance is not had in technical process, thus after reducing process side reaction.This
Method is first synthetically produced ethyl chloride using monoxone and ethyl alcohol, and there is no chloroacetic acids to hydrolyze.This technique uses hydrochloric acid
Inorganic salts are not present in hydrolysis, and product can recycle completely, and mother liquor can be with recycled.
The present invention, which is used, synthesizes ethyl chloride by chloroacetic acid and ethanol raw material, obtains pure ethyl chloride again
By carrying out quaternized synthesizing betaine carbethoxy hydrochloride with trimethylamine, heating hydrolysis ethyl alcohol is carried out in presence of hydrochloric acid, is returned
Ethyl alcohol is received, beet alkali hydrochlorate is precipitated in concentrate cooling, and 99% or more beet alkali hydrochlorate purity made from this method, yield reaches
It to 97% or more, and is not in inorganic salts solid waste.
Specific embodiment
Example 1
A kind of beet alkali hydrochlorate synthetic method sequentially adds 94.5g chloroacetic acid, 12g catalyst, 59 second into reaction flask
Alcohol, then heat up 105 DEG C of reflux, and molecular sieve is dehydrated at reflux, and reaction solution is washed with water 2 by 3 hours end of reaction
Secondary, the ethyl chloroacetate separated carries out vacuum distillation 72 DEG C/0.09kPa of ethyl chloride fraction purity 99.7%, yield
97.4%。
The ethyl chloride that upper step is obtained is added in reaction flask, and a certain amount of water is added, starts to be passed through trimethylamine gas
Body, system temperature are maintained at 43-45 DEG C, 6 hours end of reaction.Hydrochloric acid heating hydrolysis is added, what 95 DEG C of reflux collections distilled out
Water and ethyl alcohol.Collection finishes 10 DEG C of crystallizations of cooling and is centrifuged up to beet alkali hydrochlorate.Purity 99.63%, yield 94.7%.
Example 2
A kind of beet alkali hydrochlorate synthetic method sequentially adds 94.5g chloroacetic acid, 15g catalyst, 92g second into reaction flask
Alcohol, then heat up 110 DEG C of reflux, and molecular sieve is dehydrated at reflux, and reaction solution is washed with water 2 by 5 hours end of reaction
Secondary, the ethyl chloroacetate separated carries out vacuum distillation 74 DEG C/0.09kPa of ethyl chloride fraction purity 99.61%, yield
96.3%。
The ethyl chloride that upper step is obtained is added in reaction flask, and a certain amount of water is added, starts to be passed through trimethylamine gas
Body, system temperature are maintained at 33-40 DEG C, 5 hours end of reaction.Hydrochloric acid heating hydrolysis is added, what 90 DEG C of reflux collections distilled out
Water and ethyl alcohol.Collection finishes 10 DEG C of crystallizations of cooling and is centrifuged up to beet alkali hydrochlorate.Purity 99.5%, yield 95.2%.
Example 3
A kind of beet alkali hydrochlorate synthetic method sequentially adds 94.5g chloroacetic acid, 10g catalyst, 72 second into reaction flask
Alcohol, then heat up 100 DEG C of reflux, and molecular sieve is dehydrated at reflux, and reaction solution is washed with water 2 by 8 hours end of reaction
Secondary, the ethyl chloroacetate separated carries out vacuum distillation 72-73 DEG C of ethyl chloride fraction/0.09kPa purity 99.9%, yield
96.4%。
The ethyl chloride that upper step is obtained is added in reaction flask, and a certain amount of water is added, starts to be passed through trimethylamine gas
Body, system temperature are maintained at 35-40 DEG C, 5 hours end of reaction.Hydrochloric acid heating hydrolysis is added, 100 DEG C of reflux collections distill out
Water and ethyl alcohol.Collection finishes 15-20 DEG C of cooling crystallizations and is centrifuged up to beet alkali hydrochlorate.Purity 99.80%, yield 94.3%.
Claims (2)
1. a kind of beet alkali hydrochlorate synthetic method, it is characterized in that sequentially adding chloroacetic acid, catalyst, second into reaction flask
Alcohol, then heat up 100-115 DEG C of reflux, and molecular sieve is dehydrated at reflux, and 2-8 hours end of reaction use reaction solution
Water washing 2 times, the ethyl chloroacetate separated is evaporated under reduced pressure, ethyl chloride fraction be 72-76 DEG C/0.09kPa, one
Ethyl chloroacetate purity 99%, ethyl chloride yield 96%, wherein chloroacetic acid and ethyl alcohol molar ratio are 1:1.1-2, instead
Answer equation are as follows:
CLCH2COOH + CH3CH2OH CLCH2COOCH2CH3 + H2O
The ethyl chloride that upper step is obtained is added in reaction flask, and a certain amount of water is added, starts to be passed through front three amine gas, body
It is that temperature is maintained at 20-45 DEG C, 2-6 hours end of reaction add hydrochloric acid heating hydrolysis, and 85-100 DEG C of reflux, which are collected, steams
The water and ethyl alcohol distillated, collection finish 10-15 DEG C of cooling crystallizations and are centrifuged up to beet alkali hydrochlorate, beet alkali hydrochlorate purity
99.63%, 94% or more beet alkali hydrochlorate yield, wherein trimethylamine and ethyl chloride mol ratio are as follows: 1.0-1.2:1,
Reaction equation are as follows:
CLCH2COOCH2CH3 + (CH3)N (H3C)NCH2COOCH2CH3·HCL
(H3C)NCH2COOCH2CH3·HCL (H3C)NCH2COOH·HCL + CH3CH2OH
2. beet alkali hydrochlorate synthetic method according to claim 1, it is characterized in that chloroacetic acid and ethyl alcohol are esterified
Reaction temperature is at 100 DEG C -115 DEG C, chloroacetic acid and ethyl alcohol mol ratio are as follows: 1:1.5-2.
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| CN201910141874.1A CN109942445A (en) | 2019-02-26 | 2019-02-26 | Beet alkali hydrochlorate synthetic method |
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| CN201910141874.1A CN109942445A (en) | 2019-02-26 | 2019-02-26 | Beet alkali hydrochlorate synthetic method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108774146A (en) * | 2018-08-16 | 2018-11-09 | 青岛科技大学 | A kind of preparation method of glycine betaine methyl ester hydrochloride |
| CN110818580A (en) * | 2019-11-27 | 2020-02-21 | 山东省化工研究院 | Synthesis process of betaine hydrochloride |
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| CN108774146A (en) * | 2018-08-16 | 2018-11-09 | 青岛科技大学 | A kind of preparation method of glycine betaine methyl ester hydrochloride |
| CN110818580A (en) * | 2019-11-27 | 2020-02-21 | 山东省化工研究院 | Synthesis process of betaine hydrochloride |
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