CN105418456A - Preparation method of butanediol bis(propionitrile) ether - Google Patents
Preparation method of butanediol bis(propionitrile) ether Download PDFInfo
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- CN105418456A CN105418456A CN201510888447.1A CN201510888447A CN105418456A CN 105418456 A CN105418456 A CN 105418456A CN 201510888447 A CN201510888447 A CN 201510888447A CN 105418456 A CN105418456 A CN 105418456A
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- propionitrile
- ether
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- butyleneglycol
- catalyzer
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C253/00—Preparation of carboxylic acid nitriles
- C07C253/30—Preparation of carboxylic acid nitriles by reactions not involving the formation of cyano groups
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
Abstract
The invention discloses a preparation method of butanediol bis(propionitrile) ether. The preparation method comprises the following step of: reacting 1,4-butanediol and acrylonitrile serving as reaction raw materials under the catalysis of a catalyst aqueous solution at specific temperature to generate butanediol bis(propionitrile) ether, wherein the catalyst is at least one of oxide, hydroxide, carbonate and bicarbonate of alkali metal or oxide, hydroxide, carbonate and bicarbonate of alkaline earth metal, and the specific temperature is -10-70 DEG C. The preparation method of butanediol bis(propionitrile) ether has the advantages that the process is simple, no wastes are generated, the molar yield is more than or equal to 90%, the preparation process has low requirement on temperature, and thus the preparation cost is greatly lowered.
Description
Technical field
The present invention relates to lithium-ion battery electrolytes additive agent field, being specifically related to can as the preparation method of two (propionitrile) ether of the butyleneglycol of lithium-ion battery electrolytes additive.
Background technology
The structural formula of two (propionitrile) ether of butyleneglycol is:
two (propionitrile) ether of butyleneglycol a kind ofly can make the new additive agent that lithium-ion battery electrolytes result of use is more excellent, the lithium ion battery adding two (propionitrile) ether of butyleneglycol can suppress at high temperature to store or discharge and recharge time the Swelling that occurs, in addition, the cycle life of lithium ion battery discharge and recharge can also be improved.At present, the present inventor does not find the preparation method of two (propionitrile) ether of butyleneglycol in bibliographical information.
Summary of the invention
Technical problem to be solved by this invention is: by provide a kind of technique simple, produce without waste, the preparation method of butyleneglycol pair (propionitrile) ether that molar yield is high.
In order to solve the problem, the technical solution adopted in the present invention is: the preparation method of two (propionitrile) ether of butyleneglycol, be characterized in: preparation process is as follows: with 1,4-butyleneglycol and vinyl cyanide are reaction raw materials, under the catalysis of the aqueous solution of specified temp and catalyzer, reaction generates two (propionitrile) ether of butyleneglycol, described catalyzer is at least one in the oxide compound of alkali-metal oxide compound, oxyhydroxide, carbonate, supercarbonate or alkaline-earth metal, oxyhydroxide, carbonate, supercarbonate, and described specified temp is-10 DEG C ~ 70 DEG C.
Further, the preparation method of two (propionitrile) ether of aforesaid butyleneglycol, wherein: 1, the mol ratio of 4-butyleneglycol and vinyl cyanide is 1: 2, the mass concentration of the aqueous solution of catalyzer is 1% ~ 10%, and catalyzer and BDO weight ratio are 1: (10 ~ 20).
Further, the preparation method of two (propionitrile) ether of aforesaid butyleneglycol, wherein: the mass concentration of the aqueous solution of catalyzer is 3% ~ 5%.
Further, the preparation method of two (propionitrile) ether of aforesaid butyleneglycol, wherein: specified temp is 30 DEG C ~ 70 DEG C.
Further, the preparation method of two (propionitrile) ether of aforesaid butyleneglycol, wherein: the reaction times is 16 ~ 24 hours.
Further, the preparation method of two (propionitrile) ether of aforesaid butyleneglycol, wherein: after question response, the water in reactant is removed in distillation, then under the pressure of-0.01Mpa, rectification under vacuum is carried out to reactant, collect 135 DEG C ~ 140 DEG C cuts, thus obtain two (propionitrile) ether of the butyleneglycol after purifying.
Reaction equation of the present invention is:
Advantage of the present invention is: the preparation method of two (propionitrile) ether of butyleneglycol of the present invention, its technique simply, without waste produces, molar yield can reach more than 90%.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
In band mechanical stirring, thermometer, Dropping feeder, in the there-necked flask of prolong, add 1, 4-butyleneglycol 90.1g (1mol) and vinyl cyanide 106g (2mol) stir, then slowly heat up, the potassium hydroxide aqueous solution 352g that concentration is 5% is dripped at the temperature of 30 DEG C, at the temperature of 30 DEG C, 24 hours are incubated after dropwising, then the water in reactant is removed in distillation, rectification under vacuum under the pressure of-0.01Mpa again, collect 135 DEG C ~ 140 DEG C cuts, thus obtain two (propionitrile) ether 185.3g (content is 98.52%) of highly purified butyleneglycol, molar yield is 92.79%.
Embodiment 2
In band mechanical stirring, thermometer, Dropping feeder, in the there-necked flask of prolong, add 1, 4-butyleneglycol 90.1g (1mol) and vinyl cyanide 106g (2mol) stir, then slowly heat up, the aqueous sodium carbonate 330g that concentration is 4% is dripped at the temperature of 50 DEG C, at the temperature of 50 DEG C, 20 hours are incubated after dropwising, then the water in reactant is removed in distillation, rectification under vacuum under the pressure of-0.01Mpa again, collect 135 DEG C ~ 140 DEG C cuts, thus obtain two (propionitrile) ether 184.5g (content is 98.38%) of highly purified butyleneglycol, molar yield is 92.56%.
Embodiment 3
In band mechanical stirring, thermometer, Dropping feeder, in the there-necked flask of prolong, add 1, 4-butyleneglycol 90.1g (1mol) and vinyl cyanide 106g (2mol) stir, then slowly heat up, the potassium hydroxide aqueous solution 293g that concentration is 3% is dripped at the temperature of 70 DEG C, at the temperature of 70 DEG C, 16 hours are incubated after dropwising, then the water in reactant is removed in distillation, rectification under vacuum under the pressure of-0.01Mpa again, collect 135 DEG C ~ 140 DEG C cuts, thus obtain two (propionitrile) ether 183.2g (content is 98.23%) of highly purified butyleneglycol, molar yield is 91.77%.
Beneficial effect of the present invention is: the preparation method of two (propionitrile) ether of butyleneglycol of the present invention, and its technique simply, without waste produces, molar yield can reach more than 90%; And less demanding to temperature of preparation process, thus greatly reduce preparation cost.
Claims (6)
1. the preparation method of two (propionitrile) ether of butyleneglycol, it is characterized in that: preparation process is as follows: with 1,4-butyleneglycol and vinyl cyanide are reaction raw materials, under the catalysis of the aqueous solution of specified temp and catalyzer, reaction generates two (propionitrile) ether of butyleneglycol, described catalyzer is at least one in the oxide compound of alkali-metal oxide compound, oxyhydroxide, carbonate, supercarbonate or alkaline-earth metal, oxyhydroxide, carbonate, supercarbonate, and described specified temp is-10 DEG C ~ 70 DEG C.
2. the preparation method of two (propionitrile) ether of butyleneglycol according to claim 1, it is characterized in that: the mol ratio of BDO and vinyl cyanide is 1: 2, the mass concentration of the aqueous solution of catalyzer is 1% ~ 10%, catalyzer and BDO weight ratio are 1: (10 ~ 20).
3. the preparation method of two (propionitrile) ether of butyleneglycol according to claim 2, is characterized in that: the mass concentration of the aqueous solution of catalyzer is 3% ~ 5%.
4. the preparation method of two (propionitrile) ether of the butyleneglycol according to claim 1 or 2 or 3, is characterized in that: specified temp is 30 DEG C ~ 70 DEG C.
5. the preparation method of two (propionitrile) ether of the butyleneglycol according to claim 1 or 2 or 3, is characterized in that: the reaction times is 16 ~ 24 hours.
6. the preparation method of two (propionitrile) ether of the butyleneglycol according to claim 1 or 2 or 3, it is characterized in that: after question response, the water in reactant is removed in distillation, then under the pressure of-0.01Mpa, rectification under vacuum is carried out to reactant, collect 135 DEG C ~ 140 DEG C cuts, thus obtain two (propionitrile) ether of the butyleneglycol after purifying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510888447.1A CN105418456A (en) | 2015-12-07 | 2015-12-07 | Preparation method of butanediol bis(propionitrile) ether |
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| CN201510888447.1A CN105418456A (en) | 2015-12-07 | 2015-12-07 | Preparation method of butanediol bis(propionitrile) ether |
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| CN105418456A true CN105418456A (en) | 2016-03-23 |
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| CN201510888447.1A Pending CN105418456A (en) | 2015-12-07 | 2015-12-07 | Preparation method of butanediol bis(propionitrile) ether |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106146344A (en) * | 2016-07-26 | 2016-11-23 | 张家港瀚康化工有限公司 | The preparation method of ethylene glycol bis (propionitrile) ether |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE786182A (en) * | 1971-07-23 | 1973-01-12 | Basf Ag | PROCESS FOR THE PREPARATION OF ALCOXY-PROPYLAMINES |
| CN103429566A (en) * | 2011-03-18 | 2013-12-04 | 株式会社Lg化学 | Method for preparing a dinitrile compound |
| WO2014104861A1 (en) * | 2012-12-31 | 2014-07-03 | 한국화학연구원 | Environmentally friendly plasticizer, and resin composition using same |
| CN103980156A (en) * | 2014-05-22 | 2014-08-13 | 中国科学院福建物质结构研究所 | Method for preparing alkyl diol (di-propionitrile) ether |
| WO2015147321A1 (en) * | 2014-03-28 | 2015-10-01 | 宇部興産株式会社 | Electrolyte for electrochemical device, electrolytic solution, and electrochemical device |
-
2015
- 2015-12-07 CN CN201510888447.1A patent/CN105418456A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE786182A (en) * | 1971-07-23 | 1973-01-12 | Basf Ag | PROCESS FOR THE PREPARATION OF ALCOXY-PROPYLAMINES |
| CN103429566A (en) * | 2011-03-18 | 2013-12-04 | 株式会社Lg化学 | Method for preparing a dinitrile compound |
| WO2014104861A1 (en) * | 2012-12-31 | 2014-07-03 | 한국화학연구원 | Environmentally friendly plasticizer, and resin composition using same |
| WO2015147321A1 (en) * | 2014-03-28 | 2015-10-01 | 宇部興産株式会社 | Electrolyte for electrochemical device, electrolytic solution, and electrochemical device |
| CN103980156A (en) * | 2014-05-22 | 2014-08-13 | 中国科学院福建物质结构研究所 | Method for preparing alkyl diol (di-propionitrile) ether |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106146344A (en) * | 2016-07-26 | 2016-11-23 | 张家港瀚康化工有限公司 | The preparation method of ethylene glycol bis (propionitrile) ether |
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