CN106179275A - A kind of preparation method of vinylene carbonate purification adsorbent - Google Patents
A kind of preparation method of vinylene carbonate purification adsorbent Download PDFInfo
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- CN106179275A CN106179275A CN201610691189.2A CN201610691189A CN106179275A CN 106179275 A CN106179275 A CN 106179275A CN 201610691189 A CN201610691189 A CN 201610691189A CN 106179275 A CN106179275 A CN 106179275A
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- Prior art keywords
- vinylene carbonate
- carbonate purification
- purification adsorbent
- vinyl
- norborene
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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
- B01J20/26—Synthetic macromolecular compounds
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
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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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F214/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F214/02—Monomers containing chlorine
- C08F214/04—Monomers containing two carbon atoms
- C08F214/08—Vinylidene chloride
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/44—Materials comprising a mixture of organic materials
- B01J2220/445—Materials comprising a mixture of organic materials comprising a mixture of polymers
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention provides the preparation method of a kind of vinylene carbonate purification adsorbent, a certain amount of vinylidene chloride is distributed in water, it is proportionally added into 5 norborene 1 methylcyclohexyl carboxylates, (3 acryloxypropyl) three (trimethylsiloxy group) silane, Ammonium persulfate. and polyvinyl alcohol, 2 ethylhexyl ether acrylic acid diethylene glycol esters, 2 acrylamide 2 methyl propane sulfonic acid, 1 vinyl 3 1-Butyl-1H-imidazole tetrafluoroborate, heat up, at 80 120 DEG C, react 10 18 hours, product filters, dry, i.e. obtain vinylene carbonate purification adsorbent.
Description
Technical field
The present invention relates to the preparation method of a kind of adsorbent, the system of a kind of vinylene carbonate purification adsorbent
Preparation Method.
Background technology
Vinylene carbonate, also known as 1,3-dioxole-2-ketone, vinyl carbonate.Colourless transparent liquid.As one
Plant the novel organic film for additive of lithium ion battery and additives for overcharge protection additive, be alternatively arranged as preparing the list of poly-ethylene carbonate
Body.It is the important additives making lithium battery electrolytes, the performance of lithium battery can be improved.
CN105384719A discloses the method for purification of a kind of vinylene carbonate, by molten for the crude product of vinylene carbonate
Solution, in the aromatic solvent mixed solution with aliphatic solvent, successively carries out polishing purification by cooling crystallize and rectification under vacuum,
Described rectification under vacuum operation is carried out in rectifying column, is provided with for except the porous adsorption layer of water in described rectifying column.
CN105541782A discloses the purification process of a kind of vinylene carbonate, and the method first passes through adsorption filtration and goes
Except major part impurity and moisture, then obtain highly purified vinylene carbonate by rectification under vacuum and cooling crystallize.
Existing vinylene carbonate purifying process, mostly uses activated carbon as adsorbent, has adsorption rate relatively slow,
Adsorbance is less, needs the shortcoming repeating to adsorb often, and product purity needs to improve.
Summary of the invention
It is an object of the invention to: providing the preparation method of a kind of vinylene carbonate purification adsorbent, it can be applied
In vinylene carbonate purification, its specific surface area is big, and adsorption rate is fast, and adsorbing contaminant amount is big, easy and simple to handle during application.
It is characterized in that preparation process includes:
A certain amount of vinylidene chloride is distributed in water, adds 5-norborene-1-methylcyclohexyl carboxylate in following ratio,
(3-acryloxypropyl) three (trimethylsiloxy group) silane, Ammonium persulfate. and polyvinyl alcohol, 2-ethylhexyl ether acrylic acid two
Glycol ester, 2-acrylamide-2-methyl propane sulfonic acid, 1-vinyl-3-1-Butyl-1H-imidazole tetrafluoroborate, heats up, at 80-120
DEG C, reacting 10-18 hour, product filters, and dries, i.e. obtains vinylene carbonate purification adsorbent.
Ingredients weight parts
Vinylidene chloride 100
5-norborene-1-methylcyclohexyl carboxylate 1-3
(3-acryloxypropyl) three (trimethylsiloxy group) silane 0.5-1
Ammonium persulfate. 0.4-0.8
Polyvinyl alcohol 2-3
2-ethylhexyl ether acrylic acid diethylene glycol ester 0.5-1
2-acrylamide-2-methyl propane sulfonic acid 0.5-1.5
1-vinyl-3-1-Butyl-1H-imidazole tetrafluoroborate 0.1-0.5
Water 1000
Described 5-norborene-1-methylcyclohexyl carboxylate is commercially available prod, as Shanghai Shu Ya Pharmaceutical Technology Co., Ltd is raw
The product produced；(3-acryloxypropyl) three (trimethylsiloxy group) silane is commercially available prod, such as Shanghai Chu Qing new material science and technology
The product that company limited produces；2-ethylhexyl ether acrylic acid diethylene glycol ester is commercially available prod, such as this chemistry science and technology of Tianjin Skien
The product that company limited produces；2-acrylamide-2-methyl propane sulfonic acid is commercially available prod, as Alpha chemical industry officials produce
Product；1-vinyl-3-1-Butyl-1H-imidazole tetrafluoroborate is commercially available prod, as Lanzhou Inst. of Chemical Physics, Chinese Academy of Sciences is raw
The product produced.
The product of the present invention has the advantages that
Introduce 5-norborene-1-methylcyclohexyl carboxylate, (3-acryloxypropyl) three (trimethylsiloxy group) silane,
Toluenesulfonic acid-(2-hydroxyl-3-butylene) ester, 1-vinyl-3-1-Butyl-1H-imidazole tetrafluoroborate has as polymerization monomer, adsorbent
Having higher heat stability and chemical stability, specific surface area is high, and adsorption rate is fast, and the amount of adsorbing contaminant is big, and product purity obtains
To improving.
Detailed description of the invention
Following instance only further illustrates the present invention, is not to limit the scope of protection of the invention.
Embodiment 1
In 2000L reactor, add 1000L water, 100Kg vinylidene chloride, 2Kg5-norborene-1-methyl cyclohexane yl carboxylic acid
Ester, 0.8Kg (3-acryloxypropyl) three (trimethylsiloxy group) silane, 0.6Kg Ammonium persulfate., 2.5Kg polyvinyl alcohol,
0.8Kg2-ethylhexyl ether acrylic acid diethylene glycol ester, 1Kg2-acrylamide-2-methyl propane sulfonic acid, 0.3Kg1-vinyl-3-
1-Butyl-1H-imidazole tetrafluoroborate, is warming up to 100 DEG C, reacts 14h, and product filters, and dries, and i.e. obtains vinylene carbonate and purifies use
Adsorbent.
Embodiment 2
In 2000L reactor, add 1000L water, 100Kg vinylidene chloride, 1Kg5-norborene-1-methyl cyclohexane yl carboxylic acid
Ester, 0.5Kg (3-acryloxypropyl) three (trimethylsiloxy group) silane, 0.4Kg Ammonium persulfate., 2Kg polyvinyl alcohol,
0.5Kg2-ethylhexyl ether acrylic acid diethylene glycol ester, 0.5Kg2-acrylamide-2-methyl propane sulfonic acid, 0.1Kg1-vinyl-
3-1-Butyl-1H-imidazole tetrafluoroborate, is warming up to 80 DEG C, reacts 10h, and product filters, and dries, and i.e. obtains vinylene carbonate and purifies
Use adsorbent.
Embodiment 3
In 2000L reactor, add 1000L water, 100Kg vinylidene chloride, 3Kg5-norborene-1-methyl cyclohexane yl carboxylic acid
Ester, 1Kg (3-acryloxypropyl) three (trimethylsiloxy group) silane, 0.8Kg Ammonium persulfate., 3Kg polyvinyl alcohol, 1Kg2-second
Base hexyl ether acrylic acid diethylene glycol ester, 1.5Kg2-acrylamide-2-methyl propane sulfonic acid, 0.5Kg1-vinyl-3-butyl miaow
Azoles tetrafluoroborate, is warming up to 120 DEG C, reacts 18h, and product filters, and dries, and i.e. obtains vinylene carbonate purification absorption
Agent.
Comparative example 1
Being added without 5-norborene-1-methylcyclohexyl carboxylate, other conditions are with embodiment 1.
Comparative example 2
Being added without 1Kg (3-acryloxypropyl) three (trimethylsiloxy group) silane, other conditions are with embodiment 1.
Comparative example 3
Being added without 2-ethylhexyl ether acrylic acid diethylene glycol ester, other conditions are with embodiment 1.
Comparative example 4
Being added without 2-acrylamide-2-methyl propane sulfonic acid, other conditions are with embodiment 1.
Comparative example 5
Being added without 1-vinyl-3-1-Butyl-1H-imidazole tetrafluoroborate, other conditions are with embodiment 1.
Comparative example 6
It is added without the adsorbent product that the present invention is produced, replaces with activated carbon.
Embodiment 4
The vinylene carbonate crude product solution of purity about 98% is passed through and makes equipped with 500g embodiment 1-3 and comparative example 1-6
In the 1000mL exchange column of adsorbent product, temperature 50 C, flow velocity 0.5BV/h, under the conditions of absorption purify, use gas chromatographic detection
The weight/mass percentage composition of effluent, is shown in Table 1.
Table 1: the vinylene carbonate purity after the vinylene carbonate adsorbent purification that different process is produced.
These are only the specific embodiment of the present invention, but the technical characteristic of the present invention is not limited thereto.Any with this
Based on bright, for solving essentially identical technical problem, it is achieved essentially identical technique effect, done simple change, etc.
With replacement or modification etc., all it is covered by among protection scope of the present invention.
Claims (2)
1. a vinylene carbonate purification adsorbent, it is characterised in that include following material component:
Ingredients weight parts
Vinylidene chloride 100
5-norborene-1-methylcyclohexyl carboxylate 1-3
(3-acryloxypropyl) three (trimethylsiloxy group) silane 0.5-1
Ammonium persulfate. 0.4-0.8
Polyvinyl alcohol 2-3
2-ethylhexyl ether acrylic acid diethylene glycol ester 0.5-1
2-acrylamide-2-methyl propane sulfonic acid 0.5-1.5
1-vinyl-3-1-Butyl-1H-imidazole tetrafluoroborate 0.1-0.5
Water 1000.
2. the preparation method of a vinylene carbonate purification adsorbent, it is characterised in that comprise the following steps:
By weight, 100 parts of vinylidene chlorides are distributed in 1000 parts of water, by following addition 1-3 part 5-norborene-1-first
Butylcyclohexyl carboxylate, 0.5-1 part (3-acryloxypropyl) three (trimethylsiloxy group) silane, 0.4-0.8 part Ammonium persulfate.
With 2-3 part polyvinyl alcohol, 0.5-1 part 2-ethylhexyl ether acrylic acid diethylene glycol ester, 0.5-1.5 part 2-acrylamide-2-methyl
Propane sulfonic acid, 0.1-0.5 part 1-vinyl-3-1-Butyl-1H-imidazole tetrafluoroborate, heat up, at 80-120 DEG C, 10-18 is little in reaction
Time, product filters, and dries, i.e. obtains vinylene carbonate purification adsorbent.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610691189.2A CN106179275A (en) | 2016-08-21 | 2016-08-21 | A kind of preparation method of vinylene carbonate purification adsorbent |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610691189.2A CN106179275A (en) | 2016-08-21 | 2016-08-21 | A kind of preparation method of vinylene carbonate purification adsorbent |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA610922A (en) * | 1960-12-20 | M. Thomas Robert | Purification of vinylene carbonate | |
| CN101171243A (en) * | 2005-05-12 | 2008-04-30 | 赛拓有限责任公司 | Method of purifying vinylene carbonate |
| CN101195610A (en) * | 2006-12-07 | 2008-06-11 | 比亚迪股份有限公司 | Method for purifying vinylene carbonate |
| CN103539771A (en) * | 2013-10-17 | 2014-01-29 | 中国海洋石油总公司 | Vinylene carbonate purifying method |
| CN105597711A (en) * | 2016-03-09 | 2016-05-25 | 张玲 | Preparation method of binary acid refined adsorbing material |
| CN105833854A (en) * | 2016-06-13 | 2016-08-10 | 王金明 | Preparation method of purified vanadium adsorption material |
-
2016
- 2016-08-21 CN CN201610691189.2A patent/CN106179275A/en not_active Withdrawn
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA610922A (en) * | 1960-12-20 | M. Thomas Robert | Purification of vinylene carbonate | |
| CN101171243A (en) * | 2005-05-12 | 2008-04-30 | 赛拓有限责任公司 | Method of purifying vinylene carbonate |
| CN101195610A (en) * | 2006-12-07 | 2008-06-11 | 比亚迪股份有限公司 | Method for purifying vinylene carbonate |
| CN103539771A (en) * | 2013-10-17 | 2014-01-29 | 中国海洋石油总公司 | Vinylene carbonate purifying method |
| CN105597711A (en) * | 2016-03-09 | 2016-05-25 | 张玲 | Preparation method of binary acid refined adsorbing material |
| CN105833854A (en) * | 2016-06-13 | 2016-08-10 | 王金明 | Preparation method of purified vanadium adsorption material |
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Address after: The new school district 322009 town Zhejiang city Yiwu province 5 Building 1 unit 201 room Applicant after: Wang Jinzhen Address before: 315042 Zhejiang province Jiangdong District of Ningbo City Road 265 Lane 17 No. 104 Min'an room Applicant before: Wang Jinzhen |
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Application publication date: 20161207 |