CN105384718A - Low pollution and low cost synthesis method of vinylene carbonate - Google Patents
Low pollution and low cost synthesis method of vinylene carbonate Download PDFInfo
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- CN105384718A CN105384718A CN201510907724.9A CN201510907724A CN105384718A CN 105384718 A CN105384718 A CN 105384718A CN 201510907724 A CN201510907724 A CN 201510907724A CN 105384718 A CN105384718 A CN 105384718A
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- vinylene carbonate
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
- C07D317/32—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D317/34—Oxygen atoms
- C07D317/40—Vinylene carbonate; Substituted vinylene carbonates
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention specifically relates to a low pollution and low cost synthesis method of vinylene carbonate. The synthesis method comprises the following steps: step one, preparing a chlorinated ethylene carbonate liquid; step two, mixing the chlorinated ethylene carbonate liquid obtained in the step one, a certain amount of triethylamine or/and dimethyl carbonate, and BHT, and carrying out reactions for a while; step three, subjecting the reaction liquid obtained in the step two to reduced pressure rectification under a certain vacuum degree, and collecting the fraction at the temperate of 40 to 42 DEG C. According to the provided synthesis method, the chlorinated vinylene carbonate liquid is taken as the raw material directly, the rectification operation is not needed, the technology is simple, the operation is convenient, the raw material sources are wide, the cost is low; during the reaction process, no impurity that is hard to separate other than triethylamine hydrochloride solids is generated, and thus the synthesis method is very environment-friendly.
Description
Technical field
The present invention relates to lithium from battery manufacturing field, particularly relate to a kind of synthetic method of vinylene carbonate of low stain low cost.
Background technology
At present, along with people are more and more deep to the understanding of environment protection, and the supporting dynamics of country to environmentally friendly machine progressively increases, and has promoted the widespread use of lithium ion battery in the field such as electric bicycle, electromobile rapidly.But, the safety high of lithium ion battery be hinder the subject matter, particularly lithium ion battery of high-capacity lithium-ion power battery development overcharging, short circuit, mistake is put or thermal shocking can cause the potential safety hazard such as batteries caught fire, blast often.Therefore the safety issue solving battery is the key point of development and application high capacity lithium ion battery.And the approach improving lithium ion battery safety performance mainly contains two kinds of simple methods: one is be optimized positive and negative pole material; Another kind of then be that the electrolyte system of lithium cell is optimized, both optimized electrolysis additive.
Vinylene carbonate (VC) is a kind of a kind of important additives of electrolytic solution of lithium cell, serves vital effect to the safety of lithium cell.In prior art, the method difference of synthesized vinylene carbonate is little, all adopt the high-purity chloro that obtains after rectifying for NSC 11801 as reaction raw materials, one method is under non-protonic solvent and the alkaline matter such as triethylamine or sodium hydroxide and stablizer existence condition, reacts certain hour at a certain temperature and carrys out synthesized vinylene carbonate; Another kind does not use solvent, directly adds the alkaline matter such as triethylamine or sodium hydroxide and stablizer and carry out elimination reaction and carry out synthesized vinylene carbonate.A large amount of dichloro-NSC 11801 that aforesaid method can produce in process of production, can increase environmental protection pressure, increase cost.
Summary of the invention
The object of the present invention is to provide that a kind of reaction times is short, production efficiency is high, and the synthetic method of the vinylene carbonate of the catalyzer used low stain low cost with low cost.
For achieving the above object, the invention provides a kind of synthetic method of vinylene carbonate of low stain low cost, comprise the following steps:
Step one, the chlorated liquid of preparation NSC 11801 chlorination;
Step 2, the chlorated liquid of NSC 11801 chlorination step one obtained, a certain amount of triethylamine are or/and methylcarbonate and BHT react for some time at a certain temperature;
Step 3, reaction solution step 2 obtained carries out rectification under vacuum under certain vacuum degree, collects 40-42 DEG C of cut.
Preferably, described step one specifically comprises:
A (), is placed in there-necked flask by a certain amount of NSC 11801;
B (), in there-necked flask after logical nitrogen one end time, turns on lamp source, starts logical chlorine;
(c), at a certain temperature insulation reaction for some time.
Preferably, in described step (a), chlorination reaction temperature is 40 ~ 100 DEG C; In described step (b), the time of logical nitrogen is 12-16min; In described step (c), the time of insulation reaction is 3 ~ 6h.
Preferably, in described step (a), chlorination reaction temperature is 45 ~ 80 DEG C; In described step (b), the time of logical nitrogen is 15min; In described step (c), the time of insulation reaction is 2 ~ 5h.
Preferably, in the chlorated liquid of NSC 11801 chlorination prepared by described step one, the content of dichloro-NSC 11801 answers≤8%, content >=70% of chlorocarbonic acid vinyl acetate.
Preferably, in described step 2, temperature of reaction is 35-80 DEG C, and the time of insulation reaction is 2 ~ 6h.
Preferably, in described step 2, temperature of reaction is 45-70 DEG C, and the time of insulation reaction is 4 ~ 5h.
Preferably, in described step 2, the weight ratio of methylcarbonate and triethylamine is 1: (1 ~ 2).
Preferably, in described step 2, the mol ratio of described triethylamine consumption and chlorocarbonic acid vinyl acetate is 1: the consumption of (1 ~ 3) described BHT is 0.003-0.01 times of the chlorated liquid weight of NSC 11801 chlorination.
Preferably, in described step 3, the vacuum tightness of rectification under vacuum is 2-3mm mercury column.
The invention has the beneficial effects as follows: the synthetic method of the vinylene carbonate of low stain low cost provided by the invention, directly adopt NSC 11801 chlorated liquid and do elimination reaction raw material to synthesize target product vinylene carbonate, without the need to distillation operation, simplify operation steps, technique is simple, simple operation, requires low to production unit; And raw material sources used are extensive, with low cost, effectively can reduce raw materials cost; In addition, because reaction conditions is gentle, the energy consumption in production process is lower; Significantly, the impurity that other is difficult to be separated can not be produced in reaction process except triethylamine hydrochloride solid, therefore this synthetic method very environmental protection.
Accompanying drawing explanation
Fig. 1 is the process flow sheet of the synthetic method of the vinylene carbonate of low stain low cost provided by the invention.
Embodiment
In order to more clearly state the present invention, below in conjunction with accompanying drawing, the present invention is further described.
Consult Fig. 1, the synthetic method of the vinylene carbonate of low stain low cost provided by the invention, comprises the following steps: comprise the following steps:
Step one, the chlorated liquid of preparation NSC 11801 chlorination;
A (), is placed in there-necked flask by a certain amount of NSC 11801;
B (), in there-necked flask after logical nitrogen one end time, turns on lamp source, starts logical chlorine;
(c), at a certain temperature insulation reaction for some time;
Step 2, the chlorated liquid of NSC 11801 chlorination step one obtained, a certain amount of triethylamine are or/and methylcarbonate (DMC) and stablizer (BHT) react for some time at a certain temperature;
Step 3, reaction solution step 2 obtained carries out rectification under vacuum under certain vacuum degree, collects 40-42 DEG C of cut.
The synthetic method of the vinylene carbonate of low stain low cost provided by the invention, directly adopts NSC 11801 chlorated liquid and does elimination reaction raw material to synthesize target product vinylene carbonate, without the need to distillation operation, simplify operation steps, technique is simple, simple operation, requires low to production unit; And raw material sources used are extensive, with low cost, effectively can reduce raw materials cost; In addition, because reaction conditions is gentle, the energy consumption in production process is lower; Significantly, the impurity that other is difficult to be separated can not be produced in reaction process except triethylamine hydrochloride solid, therefore this synthetic method very environmental protection.
Prove below in conjunction with specific embodiment:
Embodiment one
Weigh 250g content be 70% chlorocarbonic acid vinyl acetate and 0.9gBHT join in there-necked flask; Logical nitrogen 15 minutes in there-necked flask; Open electric stirring, temperature is also set to 45 DEG C by heating, under nitrogen protection; slowly in flask, 433g triethylamine/DMC solution is dripped by constant voltage water clock bucket; time for adding controls at about 1h, after dripping, and stopped reaction after continuation insulation reaction 1h; filtered while hot; filter cake 200gDMC washs, and then under 2.5mm Hg vacuum degree, carries out rectification under vacuum operation, collects 40-42 DEG C of cut 88.45g; draw as calculated: content 98.71%, yield is 72%.
Embodiment two
Weigh 250g content be 81% chlorocarbonic acid vinyl acetate and 1gBHT join in there-necked flask;
Logical nitrogen 12 minutes in there-necked flask; Open electric stirring, temperature is also set to 40 DEG C by heating, under nitrogen protection; slowly in flask, 500g triethylamine/DMC solution is dripped by constant voltage water clock bucket; time for adding controls at 1.5h, after dripping, and stopped reaction after continuation insulation reaction 1.5h; filtered while hot; filter cake 200gDMC washs, and then under 2mm Hg vacuum degree, carries out rectification under vacuum operation, collects 40-42 DEG C of cut 112.31g; draw as calculated: content 98.56%, yield is 79%.
Embodiment three
Weigh 250g content be about 81% chlorocarbonic acid vinyl acetate and 1.05gBHT join in there-necked flask, logical nitrogen 16 minutes in there-necked flask; Open electric stirring, temperature is also set to 100 DEG C by heating, under nitrogen protection; slowly in flask, 500g triethylamine/DMC solution is dripped by constant voltage water clock bucket; time for adding controls at 2h, after dripping, and stopped reaction after continuation insulation reaction 4h; filtered while hot; filter cake 200gDMC washs, and then under 3mm Hg vacuum degree, carries out rectification under vacuum operation, collects 40-42 DEG C of cut 92.4g; content 98.33%, yield is 65%.
As can be seen from the above experimental data, the synthetic method of the vinylene carbonate of low stain low cost provided by the invention, can stablize, produce vinylene carbonate reliably, has good yield.And, simplify technique, reduce production cost.
These are only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the prerequisite not departing from the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a synthetic method for the vinylene carbonate of low stain low cost, is characterized in that, comprises the following steps:
Step one, the chlorated liquid of preparation NSC 11801 chlorination;
Step 2, the chlorated liquid of NSC 11801 chlorination step one obtained, a certain amount of triethylamine are or/and methylcarbonate and BHT react for some time at a certain temperature;
Step 3, reaction solution step 2 obtained carries out rectification under vacuum under certain vacuum degree, collects 40-42 DEG C of cut.
2. the synthetic method of the vinylene carbonate of low stain low cost according to claim 1, is characterized in that, described step one specifically comprises:
A (), is placed in there-necked flask by a certain amount of NSC 11801;
B (), in there-necked flask after logical nitrogen one end time, turns on lamp source, starts logical chlorine;
(c), at a certain temperature insulation reaction for some time.
3. the synthetic method of the vinylene carbonate of low stain low cost according to claim 2, is characterized in that, in described step (a), chlorination reaction temperature is 40 ~ 100 DEG C; In described step (b), the time of logical nitrogen is 12-16min; In described step (c), the time of insulation reaction is 3 ~ 6h.
4. the synthetic method of the vinylene carbonate of low stain low cost according to claim 3, is characterized in that, in described step (a), chlorination reaction temperature is 45 ~ 80 DEG C; In described step (b), the time of logical nitrogen is 15min; In described step (c), the time of insulation reaction is 2 ~ 5h.
5. the synthetic method of the vinylene carbonate of the low stain low cost according to any one of claim 1-4, it is characterized in that, in the chlorated liquid of NSC 11801 chlorination prepared by described step one, the content of dichloro-NSC 11801 answers≤8%, content >=70% of chlorocarbonic acid vinyl acetate.
6. the synthetic method of the vinylene carbonate of low stain low cost according to claim 1, is characterized in that, in described step 2, temperature of reaction is 35-80 DEG C, and the time of insulation reaction is 2 ~ 6h.
7. the synthetic method of the vinylene carbonate of low stain low cost according to claim 6, is characterized in that, in described step 2, temperature of reaction is 45-70 DEG C, and the time of insulation reaction is 4 ~ 5h.
8. the synthetic method of the vinylene carbonate of low stain low cost according to claim 1, is characterized in that, in described step 2, the weight ratio of methylcarbonate and triethylamine is 1: (1 ~ 2).
9. the synthetic method of the vinylene carbonate of low stain low cost according to claim 5, it is characterized in that, in described step 2, the mol ratio of described triethylamine consumption and chlorocarbonic acid vinyl acetate is 1: (1 ~ 3), and the consumption of described BHT is 0.003-0.01 times of the chlorated liquid weight of NSC 11801 chlorination.
10. the synthetic method of the vinylene carbonate of low stain low cost according to claim 1, is characterized in that, in described step 3, the vacuum tightness of rectification under vacuum is 2-3mm mercury column.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112624925A (en) * | 2020-12-27 | 2021-04-09 | 江苏瀚康新材料有限公司 | Method for preparing dimethyl carbonate by using waste |
| CN113336736A (en) * | 2021-05-31 | 2021-09-03 | 多氟多新材料股份有限公司 | Method for preparing vinylene carbonate |
| CN114605373A (en) * | 2022-03-22 | 2022-06-10 | 营口昌成新材料科技有限公司 | Preparation method of vinylene carbonate |
| KR20230134980A (en) | 2022-03-15 | 2023-09-22 | 주식회사 테크늄 | Method for manufacturing compositions comprising vinylene carbonate and vinylene carbonate compounds |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1817879A (en) * | 2005-12-21 | 2006-08-16 | 中国科学院山西煤炭化学研究所 | Preparation of vinylene carbonate |
| CN101161647A (en) * | 2007-11-26 | 2008-04-16 | 中国海洋石油总公司 | Preparation method of vinylene carbonate for lithium ion-cell |
| CN101367788A (en) * | 2008-09-28 | 2009-02-18 | 中国海洋石油总公司 | Preparation method of vinylene carbonate for lithium cell |
-
2015
- 2015-12-09 CN CN201510907724.9A patent/CN105384718A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1817879A (en) * | 2005-12-21 | 2006-08-16 | 中国科学院山西煤炭化学研究所 | Preparation of vinylene carbonate |
| CN101161647A (en) * | 2007-11-26 | 2008-04-16 | 中国海洋石油总公司 | Preparation method of vinylene carbonate for lithium ion-cell |
| CN101367788A (en) * | 2008-09-28 | 2009-02-18 | 中国海洋石油总公司 | Preparation method of vinylene carbonate for lithium cell |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112624925A (en) * | 2020-12-27 | 2021-04-09 | 江苏瀚康新材料有限公司 | Method for preparing dimethyl carbonate by using waste |
| CN112624925B (en) * | 2020-12-27 | 2023-08-01 | 江苏瀚康新材料有限公司 | Method for preparing dimethyl carbonate by utilizing waste |
| CN113336736A (en) * | 2021-05-31 | 2021-09-03 | 多氟多新材料股份有限公司 | Method for preparing vinylene carbonate |
| KR20230134980A (en) | 2022-03-15 | 2023-09-22 | 주식회사 테크늄 | Method for manufacturing compositions comprising vinylene carbonate and vinylene carbonate compounds |
| CN114605373A (en) * | 2022-03-22 | 2022-06-10 | 营口昌成新材料科技有限公司 | Preparation method of vinylene carbonate |
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Application publication date: 20160309 |