CN108101816A - The synthesis of the efficient trithiocarbonate of chain-transferring agent - Google Patents
The synthesis of the efficient trithiocarbonate of chain-transferring agent Download PDFInfo
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- CN108101816A CN108101816A CN201611054710.8A CN201611054710A CN108101816A CN 108101816 A CN108101816 A CN 108101816A CN 201611054710 A CN201611054710 A CN 201611054710A CN 108101816 A CN108101816 A CN 108101816A
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- necked flask
- added dropwise
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- acetone
- sodium hydroxide
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C329/00—Thiocarbonic acids; Halides, esters or anhydrides thereof
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- 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
- C08F2/00—Processes of polymerisation
- C08F2/38—Polymerisation using regulators, e.g. chain terminating agents, e.g. telomerisation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The present invention relates to the synthesis of the efficient trithiocarbonate of chain-transferring agent, petroleum ether 40mL is sequentially added in the three-necked flask of 250mL, 13 15mL of acetone, 14 16mL of chloroform, 4 6mL of carbon disulfide, layer is removed with disposable dropper, it is slowly added dropwise, in ice-water bath, under the conditions of magnetic agitation, 15 20min of nitrogen is passed through to discharge air, it is rear to add in tetrabutylammonium bromide 0.2008g；Sodium hydroxide about 40g is weighed, 50% solution is made into deionized water, is transferred to constant pressure funnel, is slowly dropped into three-necked flask, 90 120min are dripped off；Yellow oil generation has been observed during being added dropwise；After dripping sodium hydroxide solution, the reaction was continued at room temperature 12 16h；Then deionized water 30mL is added in into three-necked flask, then hydrochloric acid about 60ml is slowly added dropwise adjusts the pH of solution and be less than 4, yellow solid is generated in system and releases irritative gas；It filters, and khaki solid is washed to obtain with about 200mL deionized waters；It is again toluene with volume ratio: acetone=4: 1 mixed liquor washs obtain bright yellow solid, it is dry.
Description
Technical field
The present invention relates to the synthesis of the efficient trithiocarbonate of chain-transferring agent, belong to technical field of material chemistry.
Background technology
Block polymer, which is also named, inlays polymer, it is existed with the not exactly the same polymer splicing of two or more properties
A kind of copolymer with special nature formed together.And Thermo-sensitive block copolymer is by containing hydrophilic radical with dredging mostly
The macromolecular substances of water base group are polymerized, and the macro-radical more sensitive to temperature is contained generally in hydrophilic radical.
There are many kinds of the synthetic methods of block polymer, wherein reversible addition-fracture chain transfer polymerization (RAFT) method receives
Concern, advantage is more for monomer available, and reaction condition is mild.Reversible addition-fracture chain transfer polymerization (RAFT) method is a kind of
Living radical polymerization with controllability, it is the polymerization side that molecular weight and molecular distribution are controlled using chain-transferring agent
Method.The controllable preparation that block gathers with object has largely promoted the development and application of block copolymer.Such as poly- N- isopropyls
Base acrylamide (NIPAM) is a kind of non-ionic temperature sensing polymer, its its physicochemical property at 37 DEG C will change,
And with the increase of application range, it is clear that poly(N-isopropylacrylamide) (NIPAM) has been unable to meet the demand of development, this is just
The some properties that polymerize different monomers again to reduce or increase copolymer.Lucky RAFT methods disclosure satisfy that this demand,
And this method is mild, and cost is less, is more suitble to commercially produce.
The content of the invention
The technical problems to be solved by the invention are to provide the synthesis of the efficient trithiocarbonate of chain-transferring agent, technical solution
It is as follows：Petroleum ether 40mL, acetone 13-15mL, chloroform 14-16mL, carbon disulfide 4- are sequentially added in the three-necked flask of 250mL
6mL removes layer with disposable dropper, is slowly added dropwise, in ice-water bath, under the conditions of magnetic agitation, be passed through nitrogen 15-20min with
Air is discharged, it is rear to add in tetrabutylammonium bromide 0.2008g；Weigh sodium hydroxide about 40g, with deionized water be made into 50% it is molten
Liquid is transferred to constant pressure funnel, is slowly dropped into three-necked flask, and 90-120min is dripped off；Yellow oily has been observed during being added dropwise
Object generates；After dripping sodium hydroxide solution, the reaction was continued at room temperature 12-16h；Then deionization is added in into three-necked flask
Water 30mL, then hydrochloric acid about 60ml is slowly added dropwise adjusts the pH of solution and be less than 4, yellow solid is generated in system and releases irritation gas
Body；It filters, and khaki solid is washed to obtain with about 200mL deionized waters；It is again toluene with volume ratio: acetone=4: 1 mixing
Liquid washs, and obtains bright yellow solid, dry.
The beneficial effects of the invention are as follows：Preparation process simple environment protection, it is at low cost, it is applied widely.
Specific embodiment
Embodiment 1
Petroleum ether 40mL, acetone 13mL, chloroform 14mL, carbon disulfide 4mL are sequentially added in the three-necked flask of 250mL,
Layer is removed with disposable dropper, is slowly added dropwise, in ice-water bath, under the conditions of magnetic agitation, is passed through nitrogen 15min to discharge sky
Gas, it is rear to add in tetrabutylammonium bromide 0.2008g；Sodium hydroxide about 40g is weighed, 50% solution is made into deionized water, is transferred to
Constant pressure funnel, is slowly dropped into three-necked flask, and 90min is dripped off；Yellow oil generation has been observed during being added dropwise；It is added dropwise
After complete sodium hydroxide solution, the reaction was continued at room temperature 12h；Then deionized water 30mL is added in into three-necked flask, then slowly
The pH that hydrochloric acid about 60ml adjusting solution is added dropwise is less than 4, generates yellow solid in system and releases irritative gas；It filters, is used in combination
About 200mL deionized waters wash to obtain khaki solid；It is again toluene with volume ratio: acetone=4: 1 mixed liquor washs obtain bright Huang
Color solid, it is dry.
Embodiment 2
Petroleum ether 40mL, acetone 15mL, chloroform 16mL, carbon disulfide 6mL are sequentially added in the three-necked flask of 250mL,
Layer is removed with disposable dropper, is slowly added dropwise, in ice-water bath, under the conditions of magnetic agitation, is passed through nitrogen 20min to discharge sky
Gas, it is rear to add in tetrabutylammonium bromide 0.2008g；Sodium hydroxide about 40g is weighed, 50% solution is made into deionized water, is transferred to
Constant pressure funnel, is slowly dropped into three-necked flask, and 120min is dripped off；Yellow oil generation has been observed during being added dropwise；Drop
After adding sodium hydroxide solution, the reaction was continued at room temperature 16h；Then deionized water 30mL is added in into three-necked flask, then is delayed
The slow pH that hydrochloric acid about 60ml adjusting solution is added dropwise is less than 4, generates yellow solid in system and releases irritative gas；It filters, and
Khaki solid is washed to obtain with about 200mL deionized waters；It is again toluene with volume ratio: acetone=4: 1 mixed liquor washs obtain bright
Yellow solid, it is dry.
Embodiment 3
Petroleum ether 40mL, acetone 14mL, chloroform 15mL, carbon disulfide 5mL are sequentially added in the three-necked flask of 250mL,
Layer is removed with disposable dropper, is slowly added dropwise, in ice-water bath, under the conditions of magnetic agitation, is passed through nitrogen 18min to discharge sky
Gas, it is rear to add in tetrabutylammonium bromide 0.2008g；Sodium hydroxide about 40g is weighed, 50% solution is made into deionized water, is transferred to
Constant pressure funnel, is slowly dropped into three-necked flask, and 100min is dripped off；Yellow oil generation has been observed during being added dropwise；Drop
After adding sodium hydroxide solution, the reaction was continued at room temperature 14h；Then deionized water 30mL is added in into three-necked flask, then is delayed
The slow pH that hydrochloric acid about 60ml adjusting solution is added dropwise is less than 4, generates yellow solid in system and releases irritative gas；It filters, and
Khaki solid is washed to obtain with about 200mL deionized waters；It is again toluene with volume ratio: acetone=4: 1 mixed liquor washs obtain bright
Yellow solid, it is dry.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and
Within principle, any modifications, equivalent replacements and improvements are made should all be included in the protection scope of the present invention.
Claims (2)
1. the synthesis of the efficient trithiocarbonate of chain-transferring agent, which is characterized in that including：In the three-necked flask of 250mL successively
Petroleum ether 40mL, acetone 13-15mL, chloroform 14-16mL, carbon disulfide 4-6mL are added in, removes layer with disposable dropper, slowly
It is added dropwise, in ice-water bath, under the conditions of magnetic agitation, is passed through nitrogen 15-20min to discharge air, adds in tetrabutylammonium bromide afterwards
0.2008g；Sodium hydroxide about 40g is weighed, 50% solution is made into deionized water, constant pressure funnel is transferred to, is slowly dropped into
Three-necked flask, 90-120min are dripped off；Yellow oil generation has been observed during being added dropwise；After dripping sodium hydroxide solution,
The reaction was continued at room temperature 12-16h；Then deionized water 30mL is added in into three-necked flask, then hydrochloric acid about 60ml is slowly added dropwise
The pH for adjusting solution is less than 4, generates yellow solid in system and releases irritative gas；It filters, and with about 200mL deionized waters
Wash to obtain khaki solid；It is again toluene with volume ratio: acetone=4: 1 mixed liquor washs obtain bright yellow solid, it is dry.
2. preparation method according to claim 1, which is characterized in that the reaction temperature is 20-25 degree.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611054710.8A CN108101816A (en) | 2016-11-25 | 2016-11-25 | The synthesis of the efficient trithiocarbonate of chain-transferring agent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611054710.8A CN108101816A (en) | 2016-11-25 | 2016-11-25 | The synthesis of the efficient trithiocarbonate of chain-transferring agent |
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| Publication Number | Publication Date |
|---|---|
| CN108101816A true CN108101816A (en) | 2018-06-01 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201611054710.8A Withdrawn CN108101816A (en) | 2016-11-25 | 2016-11-25 | The synthesis of the efficient trithiocarbonate of chain-transferring agent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108727239A (en) * | 2018-06-29 | 2018-11-02 | 烟台智本知识产权运营管理有限公司 | A kind of synthesis of chain-transferring agent trithiocarbonate |
| CN117534900A (en) * | 2024-01-09 | 2024-02-09 | 瑞声光电科技(常州)有限公司 | Rubber sound membrane, sound production device and application thereof |
-
2016
- 2016-11-25 CN CN201611054710.8A patent/CN108101816A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108727239A (en) * | 2018-06-29 | 2018-11-02 | 烟台智本知识产权运营管理有限公司 | A kind of synthesis of chain-transferring agent trithiocarbonate |
| CN117534900A (en) * | 2024-01-09 | 2024-02-09 | 瑞声光电科技(常州)有限公司 | Rubber sound membrane, sound production device and application thereof |
| CN117534900B (en) * | 2024-01-09 | 2024-04-09 | 瑞声光电科技(常州)有限公司 | Rubber sound membrane, sound production device and application thereof |
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| PB01 | Publication | ||
| PB01 | Publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180601 |
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| WW01 | Invention patent application withdrawn after publication |