CN108160039A - A kind of preparation method of fluorinated ethylene carbonate purification material - Google Patents
A kind of preparation method of fluorinated ethylene carbonate purification material Download PDFInfo
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- CN108160039A CN108160039A CN201711177369.XA CN201711177369A CN108160039A CN 108160039 A CN108160039 A CN 108160039A CN 201711177369 A CN201711177369 A CN 201711177369A CN 108160039 A CN108160039 A CN 108160039A
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- ethylene carbonate
- fluorinated ethylene
- preparation
- cellulose acetate
- purification material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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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
- C07D317/42—Halogen atoms or nitro radicals
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The present invention relates to a kind of preparation methods of fluorinated ethylene carbonate purification material.By weight, porous cellulose acetate microballoon is added in a kettle, instead, along 2,6 nonadiene, 1 alcohol, 5 norbornene of N hydroxyls, 2,3 dicarboximide, disuccinimidyl suberate, 2 (2 furans) 4 (5) (2 furans) 1H imidazoles, three potassium fluoborate of cyclohexenyl group, ammonium persulfate, water, neopelex, heating, reaction, product is filtered after reaction, washing, it is dry to purify material to get to fluorinated ethylene carbonate.
Description
Technical field
The present invention relates to a kind of preparation method of adsorbent, especially a kind of preparation of fluorinated ethylene carbonate purification material
Method.
Background technology
Additive of the fluorocarboxylic acid vinyl acetate as lithium-ion battery electrolytes can inhibit the decomposition of electrolyte, reduce electricity
The impedance in pond improves its resistance to low temperature, hence it is evident that improves battery specific capacity and cyclical stability：Using it as electrolyte solvent,
The charge/discharge cycle characteristics and current efficiency of the electrochemical devices such as secondary cell and capacitor can be improved.In addition, he can also use
Make medicine, pesticide intermediate.
CN103113345A discloses a kind of preparation method of electrolysis additive fluorinated ethylene carbonate, with chloro carbon
Vinyl acetate and hydrogen fluoride are raw material, and under nitrogen protection, controlling reaction temperature is 50~120 DEG C, is obtained after reaction containing fluoro
The mixture of ethylene carbonate；Distilation is carried out again obtains required product fluorinated ethylene carbonate.System of the present invention
Preparation Method, raw material is cheap and easy to get, and process route is simple, is generated without solid waste, product yield is more than 95%, exhaust gas fluorine
Change hydrogen and hydrogen chloride gas is absorbed by lye, basic non-environmental-pollution.
CN107033119A discloses a kind of preparation method of high-purity fluorinated ethylene carbonate.The preparation method include with
Lower step：1) chlorocarbonic acid vinyl acetate raw material and hydrogen fluoride liquid are reacted, obtains mixture；2) it is added in into mixture
Metal oxide carries out deacidification reaction, and filtering obtains filtrate；3) solvent mixing is added in into filtrate, decrease temperature crystalline obtains fluoro
Ethylene carbonate crystalline esters are removed water to get high-purity fluorinated ethylene carbonate.The preparation method of the high-purity fluorinated ethylene carbonate of the present invention
Reactive liquid solution is carried out as raw material using chlorocarbonic acid vinyl acetate and anhydrous liquid hydrogen fluoride, is removed through the reaction that deacidifies, decrease temperature crystalline, heating
Water process prepares high-purity fluorinated ethylene carbonate, and products obtained therefrom purity is more than 99.5%；The preparation method technology controlling and process is simple,
Side reaction is few, is easily purified, and reaction product purity is high, at low cost, is convenient for industrialized production.
Existing fluorinated ethylene carbonate must prepare or purifying technique, as adsorbent or uses knot using activated carbon mostly
Brilliant Methods For Purification fluorinated ethylene carbonate product has the shortcomings that implementation is complicated, and consumption energy is big.
Invention content
The purpose of the present invention is：There is provided a kind of preparation method of fluorinated ethylene carbonate purification material, it is characterised in that system
Standby step includes：
By weight, porous cellulose acetate microballoon is added in a kettle, instead, cis- 2,6- nonadienes -1- alcohol, N- hydroxyls -
5- norbornene -2,3- dicarboximides, disuccinimidyl suberate, 2- (2- furans) -4 (5)-(2- furans) -1H- miaows
Azoles, three potassium fluoborate of cyclohexenyl group, ammonium persulfate, neopelex, water are warming up to 70-90 DEG C, react 10-20h,
Product is filtered after reaction, washing, dry to purify material to get to fluorinated ethylene carbonate.
A kind of preparation method of the fluorinated ethylene carbonate purification material, it is characterised in that：Described is anti-, and cis- 2,
6- nonadiene -1- alcohol, quality dosage are the 1-6% of porous cellulose acetate microballoon.
A kind of preparation method of the fluorinated ethylene carbonate purification material, it is characterised in that：N- hydroxyls-the 5-
Norbornene -2,3- dicarboximide, quality dosage are the 1-6% of porous cellulose acetate microballoon.
A kind of preparation method of the fluorinated ethylene carbonate purification material, it is characterised in that：The suberic acid two
Succinimide, quality dosage are the 1-6% of porous cellulose acetate microballoon.
A kind of preparation method of the fluorinated ethylene carbonate purification material, it is characterised in that：2- (the 2- furans
Mutter) -4 (5)-(2- furans) -1H- imidazoles, quality dosage is the 0.5-1.5% of porous cellulose acetate microballoon.
A kind of preparation method of the fluorinated ethylene carbonate purification material, it is characterised in that：The cyclohexenyl group
Three potassium fluoborates, quality dosage are the 0.1-0.5% of porous cellulose acetate microballoon.
A kind of preparation method of the fluorinated ethylene carbonate purification material, it is characterised in that：The ammonium persulfate,
Neopelex, quality dosage are the 0.5-2% of porous cellulose acetate microballoon.
A kind of preparation method of the fluorinated ethylene carbonate purification material, it is characterised in that：The water, quality
Dosage is the 300-700% of porous cellulose acetate microballoon.
The porous cellulose acetate microballoon, instead, cis- 2,6- nonadienes -1- alcohol, N- hydroxyl -5- norbornene -2,3-
Dicarboximide, disuccinimidyl suberate, 2- (2- furans) -4 (5)-(2- furans) -1H- imidazoles, cyclohexenyl group trifluoro boron
Sour potassium, ammonium persulfate are commercial product.
The product of the present invention has the advantages that：
（1）Adsorbent product has excellent mechanical performance, and heat resistance, endurance, adsorption effect is stablized in adsorption process, no
It is broken, it is easily isolated.
（2）Adsorbent product has larger specific surface area, and adsorption rate is fast, and absorption volume is big.
Specific embodiment
Following instance is only to further illustrate the present invention, and is not limitation the scope of protection of the invention.
Embodiment 1
In a kettle, porous cellulose acetate microballoon 100Kg is added in, instead, cis- 2,6- nonadienes -1- alcohol 3Kg, N- hydroxyl -5-
Norbornene -2,3- dicarboximide 1.5Kg, disuccinimidyl suberate 1.5Kg, 2- (2- furans) -4 (5)-(2- furans
Mutter) -1H- imidazoles 1Kg, cyclohexenyl group three potassium fluoborate 0.2Kg, ammonium persulfate 0.75Kg, neopelex 0.75Kg,
Water 450Kg, is warming up to 80 DEG C after mixing, reacts 15h, and product is filtered after reaction, washing, dry to get to fluorine
Material is purified for ethylene carbonate.
Embodiment 2
In a kettle, porous cellulose acetate microballoon 100Kg is added in, instead, cis- 2,6- nonadienes -1- alcohol 1Kg, N- hydroxyl -5-
Norbornene -2,3- dicarboximide 1Kg, disuccinimidyl suberate 1Kg, 2- (2- furans) -4 (5)-(2- furans) -1H-
Imidazoles 0.5Kg, cyclohexenyl group three potassium fluoborate 0.1Kg, ammonium persulfate 0.5Kg, neopelex 0.5Kg, water
300Kg, is warming up to 70 DEG C after mixing, reacts 10h, and product is filtered after reaction, washing, dry to get to fluoro
Ethylene carbonate purifies material.
Embodiment 3
In a kettle, porous cellulose acetate microballoon 100Kg is added in, instead, cis- 2,6- nonadienes -1- alcohol 6Kg, N- hydroxyl -5-
Norbornene -2,3- dicarboximide 6Kg, disuccinimidyl suberate 6Kg, 2- (2- furans) -4 (5)-(2- furans) -1H-
Imidazoles 1.5Kg, cyclohexenyl group three potassium fluoborate 0.5Kg, ammonium persulfate 2Kg, neopelex 2Kg, water 700Kg are mixed
90 DEG C are warming up to after closing uniformly, reacts 20h, and product is filtered after reaction, washing, dry to get to fluoro ethylene carbonate
Ester purifies material.
Comparative example 1
N- hydroxyl -5- norbornene -2,3- dicarboximides are added without, other conditions are the same as embodiment 1.
Comparative example 2
Disuccinimidyl suberate is added without, other conditions are the same as embodiment 1.
Comparative example 3
2- (2- furans) -4 (5)-(2- furans) -1H- imidazoles is added without, other conditions are the same as embodiment 1.
Comparative example 4
Three potassium fluoborate of cyclohexenyl group is added without, other conditions are the same as embodiment 1.
Embodiment 4
The fluorinated ethylene carbonate crude product that mass percent concentration is about 97% is passed through equipped with 500g embodiments 1-3 and comparison
Example 1-5 adsorbent products 1000L exchange columns, temperature 60 C, flow velocity 0.5BV/h, under the conditions of adsorb purification, examined with gas-chromatography
The mass percentage of efflux is surveyed, is shown in Table 1.
Table 1：Fluorinated ethylene carbonate product purity after the adsorbent product absorption that different process is produced.
Claims (8)
1. a kind of preparation method of fluorinated ethylene carbonate purification material, it is characterised in that include the following steps：
By weight, porous cellulose acetate microballoon is added in a kettle, instead, cis- 2,6- nonadienes -1- alcohol, N- hydroxyls -
5- norbornene -2,3- dicarboximides, disuccinimidyl suberate, 2- (2- furans) -4 (5)-(2- furans) -1H- miaows
Azoles, three potassium fluoborate of cyclohexenyl group, ammonium persulfate, neopelex, water are warming up to 70-90 DEG C, react 10-20h,
Product is filtered after reaction, washing, dry to purify material to get to fluorinated ethylene carbonate.
2. a kind of preparation method of fluorinated ethylene carbonate purification material according to claim 1, it is characterised in that：It is described
Anti-, cis- 2,6- nonadienes -1- alcohol, quality dosage be porous cellulose acetate microballoon 1-6%.
3. a kind of preparation method of fluorinated ethylene carbonate purification material according to claim 1, it is characterised in that：It is described
N- hydroxyl -5- norbornene -2,3- dicarboximides, quality dosage be porous cellulose acetate microballoon 1-6%.
4. a kind of preparation method of fluorinated ethylene carbonate purification material according to claim 1, it is characterised in that：It is described
Disuccinimidyl suberate, quality dosage be porous cellulose acetate microballoon 1-6%.
5. a kind of preparation method of fluorinated ethylene carbonate purification material according to claim 1, it is characterised in that：It is described
2- (2- furans) -4 (5)-(2- furans) -1H- imidazoles, quality dosage be porous cellulose acetate microballoon 0.5-1.5%.
6. a kind of preparation method of fluorinated ethylene carbonate purification material according to claim 1, it is characterised in that：It is described
Three potassium fluoborate of cyclohexenyl group, quality dosage be porous cellulose acetate microballoon 0.1-0.5%.
7. a kind of preparation method of fluorinated ethylene carbonate purification material according to claim 1, it is characterised in that：It is described
Ammonium persulfate, neopelex, quality dosage be porous cellulose acetate microballoon 0.5-2%.
8. a kind of preparation method of fluorinated ethylene carbonate purification material according to claim 1, it is characterised in that：It is described
Water, quality dosage be porous cellulose acetate microballoon 300-700%.
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| CN201711177369.XA CN108160039A (en) | 2017-11-23 | 2017-11-23 | A kind of preparation method of fluorinated ethylene carbonate purification material |
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| CN201711177369.XA CN108160039A (en) | 2017-11-23 | 2017-11-23 | A kind of preparation method of fluorinated ethylene carbonate purification material |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717390A (en) * | 2009-10-29 | 2010-06-02 | 张家港市华盛化学有限公司 | Purifying process of difluoroethylene carbonate |
| CN101870652A (en) * | 2009-04-24 | 2010-10-27 | 中国科学院福建物质结构研究所 | Refining method of fluoro ethylene carbonate with high purity |
| CN102079741A (en) * | 2010-12-21 | 2011-06-01 | 东莞市杉杉电池材料有限公司 | Novel dewatering and purifying method of ethylene carbonate (EC) |
| CN106311167A (en) * | 2016-08-21 | 2017-01-11 | 王琪宇 | Method for preparing adsorbent for purification of fluoroethylene carbonate |
-
2017
- 2017-11-23 CN CN201711177369.XA patent/CN108160039A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101870652A (en) * | 2009-04-24 | 2010-10-27 | 中国科学院福建物质结构研究所 | Refining method of fluoro ethylene carbonate with high purity |
| CN101717390A (en) * | 2009-10-29 | 2010-06-02 | 张家港市华盛化学有限公司 | Purifying process of difluoroethylene carbonate |
| CN102079741A (en) * | 2010-12-21 | 2011-06-01 | 东莞市杉杉电池材料有限公司 | Novel dewatering and purifying method of ethylene carbonate (EC) |
| CN106311167A (en) * | 2016-08-21 | 2017-01-11 | 王琪宇 | Method for preparing adsorbent for purification of fluoroethylene carbonate |
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Application publication date: 20180615 |