CN107254012A - A kind of preparation method of trifluorostyrene polymer - Google Patents
A kind of preparation method of trifluorostyrene polymer Download PDFInfo
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- CN107254012A CN107254012A CN201710329389.8A CN201710329389A CN107254012A CN 107254012 A CN107254012 A CN 107254012A CN 201710329389 A CN201710329389 A CN 201710329389A CN 107254012 A CN107254012 A CN 107254012A
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- trifluorostyrene
- emulsification
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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
- C08F112/00—Homopolymers 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 an aromatic carbocyclic ring
- C08F112/02—Monomers containing only one unsaturated aliphatic radical
- C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
- C08F112/14—Monomers containing only one unsaturated aliphatic radical containing one ring substituted by hetero atoms or groups containing heteroatoms
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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
- C08F6/00—Post-polymerisation treatments
- C08F6/14—Treatment of polymer emulsions
- C08F6/22—Coagulation
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- Polymers & Plastics (AREA)
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention discloses a kind of preparation method of trifluorostyrene polymer, comprise the following steps：（1）Pre-emulsification；（2）Emulsification；（3）Demulsification；（4）Post processing.A kind of preparation method of trifluorostyrene polymer of the present invention, pass through the control and the adjustment of emulsifying agent of concentration, using the method for emulsion polymerization, pass through the design of suitable polymerization technique parameter, the trifluorostyrene polymer of high-purity, high yield is prepared, there is directive significance to industrialized production.
Description
Technical field
The present invention relates to trifluorostyrene preparing technical field, more particularly to a kind of system of trifluorostyrene polymer
Preparation Method.
Background technology
Trifluorostyrene (α, β, β-trifluorostyrene, abbreviation TFS) is a kind of fluorochemical monomer, available for preparing
Polymer and fluoro-containing intermediate.The polymer Cpolytriflurostyrene, abbreviation PTFS of trifluorostyrene) possess heat-resisting
Property good, transparency it is high, dissolubility is good, and dielectric loss is low, radiation-resistant characteristic, PEM, amberplex, photoelectricity lead to
The fields such as news, filtering material, microelectronics are widely used potentiality.
The preparation of trifluorostyrene polymer is limited by monomer trifluorostyrene own structural characteristics.Due to trifluoro-benzene
Hydrogen atom in ethene in double bond is replaced by the strong fluorine atom of electronegativity, on the lone pair electrons and carbon-carbon double bond on fluorine atom
Pi-electron formation p- π repel the centre for causing the pi-electron in double bond to be concentrated mainly on C-C keys, and the tension force of double bond is very big, holds very much
Easily occur homolysis, thus the reaction of [2+2] Cyclodimerization easily occurs at room temperature for trifluorostyrene compound, it is poly- with traditional body
Diphenyl Freon C318 and some oligomer that the primary product obtained with radical polymerization is substitution are closed, therefore, to be obtained
Polymer with HMW can only use emulsion polymerization.The concentration of trifluorostyrene polymer prepared by existing method is low,
Unsuitable industrialized production.
The content of the invention
The present invention solves the technical problem of provide a kind of preparation method of trifluorostyrene polymer.
In order to solve the above technical problems, one aspect of the present invention is：A kind of trifluorostyrene is provided to birds of the same feather flock together
The preparation method of compound, comprises the following steps：
（1）Pre-emulsification：Added into the reactor with heating stirring function a certain amount of trifluorostyrene monomer, deionized water and
Emulsifying agent, after stirring and evenly mixing, pre-emulsification certain time at room temperature；
（2）Emulsification：To step（1）Add and risen under a certain amount of initiator, stirring in mixed solution after middle pre-emulsification
Certain emulsifying temperature, constant temperature emulsification a period of time, makes emulsification complete；
（3）Demulsification：By step（2）In obtained emulsion be transferred in another reactor, and add excessive saturation food thereto
Salt solution, quickly stirs 5~8min with more than 1000r/min stir speed (S.S.), makes its layering that is demulsified completely；
（4）Post processing：By step（3）Layering solution filtering after middle demulsification, takes solid filtrate priority boiling water and ethanol each
Washing 5~8 times, is finally putting into vacuum drying chamber and dries, obtain the trifluorostyrene polymer.
In a preferred embodiment of the present invention, the step（1）In, the trifluorostyrene monomer, deionized water and
The addition of emulsifying agent is：The mass concentration of the trifluorostyrene monomer in deionized water is 150~350g/L；The breast
The addition of agent is the 1/20~3/20 of trifluorostyrene monomer mass.
In a preferred embodiment of the present invention, the emulsifying agent be dodecyl sodium sulfate, lauryl sodium sulfate and
The mixture of lauryl amine hydrochloric acid sodium.
In a preferred embodiment of the present invention, the dodecyl sodium sulfate, lauryl sodium sulfate and lauryl amine salt
The mixing quality ratio of sour sodium is 1：2~3:2~3.
In a preferred embodiment of the present invention, the step（1）In, the pre-emulsification time is 1.5~3h.
In a preferred embodiment of the present invention, the step（2）In, the initiator is that mass ratio is 2~3:1 mistake
The mixed system of potassium sulfate and the light sodium of sulfurous acid, the addition of the initiator is the 1/ of the trifluorostyrene monomer mass
200~1/100.
In a preferred embodiment of the present invention, the step（2）In, the condition of the emulsification is：55~60 DEG C of constant temperature
Hot bath, emulsification times are 55~65h.
In a preferred embodiment of the present invention, the step（4）In, the vacuum drying condition is：Vacuum 0.5
~0.8MPa, temperature is 60~80 DEG C, and the time is 15~20h.
The beneficial effects of the invention are as follows：A kind of preparation method of trifluorostyrene polymer of the present invention, passes through concentration
Control and the adjustment of emulsifying agent, using the method for emulsion polymerization, by the design of suitable polymerization technique parameter, are prepared high-purity
Degree, the trifluorostyrene polymer of high yield, have directive significance to industrialized production.
Embodiment
Presently preferred embodiments of the present invention is described in detail below so that advantages and features of the invention can be easier to by
It will be appreciated by those skilled in the art that apparent clearly being defined so as to be made to protection scope of the present invention.
The embodiment of the present invention includes：
Embodiment 1
A kind of preparation method of trifluorostyrene polymer, comprises the following steps：
（1）Pre-emulsification：Trifluorostyrene monomer, deionized water and emulsifying agent are added into the reactor with heating stirring function,
And make the mass concentration of trifluorostyrene monomer in deionized water be 150g/L；The addition of emulsifying agent is set to account for trifluorostyrene
The 1/20 of monomer mass；Finish, stir and evenly mix, at room temperature pre-emulsification 1.5h；
Wherein, the emulsifying agent is dodecyl sodium sulfate, lauryl sodium sulfate and lauryl amine hydrochloric acid sodium with 1：2:2 quality
Than the mixture of mixing；
（2）Emulsification：To step（1）Added in mixed solution after middle pre-emulsification and account for drawing for trifluorostyrene monomer mass 1/200
Send out and be warming up to 55 DEG C under agent, stirring under constant temperature heating water-bath, constant temperature emulsification 55h is complete to emulsifying；
Wherein, the initiator is that mass ratio is 2:The mixed system of the 1 light sodium of potassium peroxydisulfate and sulfurous acid；
（3）Demulsification：By step（2）In obtained emulsion be transferred in another reactor, and add excessive saturation food thereto
Salt solution, quickly stirs 5~8min with more than 1000r/min stir speed (S.S.), makes its layering that is demulsified completely；
（4）Post processing：By step（3）Layering solution filtering after middle demulsification, takes solid filtrate priority boiling water and ethanol each
Washing 5~8 times, it is 0.5~0.8MPa to be finally putting into vacuum drying chamber in vacuum, and temperature is true under conditions of 60~80 DEG C
Sky dries 15~20h, obtains the trifluorostyrene polymer.
Embodiment 2
A kind of preparation method of trifluorostyrene polymer, comprises the following steps：
（1）Pre-emulsification：Trifluorostyrene monomer, deionized water and emulsifying agent are added into the reactor with heating stirring function,
And make the mass concentration of trifluorostyrene monomer in deionized water be 350g/L；The addition of emulsifying agent is set to account for trifluorostyrene
The 3/20 of monomer mass；Finish, stir and evenly mix, at room temperature pre-emulsification 3h；
Wherein, the emulsifying agent is dodecyl sodium sulfate, lauryl sodium sulfate and lauryl amine hydrochloric acid sodium with 1： 3:3 matter
Measure the mixture than mixing；
（2）Emulsification：To step（1）Added in mixed solution after middle pre-emulsification and account for drawing for trifluorostyrene monomer mass 1/100
Send out and be warming up to 60 DEG C under agent, stirring under constant temperature heating water-bath, constant temperature emulsification 65h is complete to emulsifying；
Wherein, the initiator is that mass ratio is 3:The mixed system of the 1 light sodium of potassium peroxydisulfate and sulfurous acid；
（3）Demulsification：By step（2）In obtained emulsion be transferred in another reactor, and add excessive saturation food thereto
Salt solution, quickly stirs 5~8min with more than 1000r/min stir speed (S.S.), makes its layering that is demulsified completely；
（4）Post processing：By step（3）Layering solution filtering after middle demulsification, takes solid filtrate priority boiling water and ethanol each
Washing 5~8 times, it is 0.5~0.8MPa to be finally putting into vacuum drying chamber in vacuum, and temperature is true under conditions of 60~80 DEG C
Sky dries 15~20h, obtains the trifluorostyrene polymer.
Trifluorostyrene polymer prepared by the above method is white solid, after tested, its high purity more than 99%,
Yield is 81~89%.
The adjustment of control and emulsifier and consumption of the present invention by monomer concentration, using the method for emulsion polymerization,
By the design of suitable polymerization technique parameter, the trifluorostyrene polymer of high-purity, high yield is prepared, to industrialization
Production has directive significance.
In addition, by the adjustment of emulsifier and proportioning, with reference to initiator, effectively reducing emulsification times.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
Equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, is included within the scope of the present invention.
Claims (8)
1. a kind of preparation method of trifluorostyrene polymer, it is characterised in that comprise the following steps：
（1）Pre-emulsification：Added into the reactor with heating stirring function a certain amount of trifluorostyrene monomer, deionized water and
Emulsifying agent, after stirring and evenly mixing, pre-emulsification certain time at room temperature；
（2）Emulsification：To step（1）Add and risen under a certain amount of initiator, stirring in mixed solution after middle pre-emulsification
Certain emulsifying temperature, constant temperature emulsification a period of time, makes emulsification complete；
（3）Demulsification：By step（2）In obtained emulsion be transferred in another reactor, and add excessive saturation food thereto
Salt solution, quickly stirs 5~8min with more than 1000r/min stir speed (S.S.), makes its layering that is demulsified completely；
（4）Post processing：By step（3）Layering solution filtering after middle demulsification, takes solid filtrate priority boiling water and ethanol each
Washing 5~8 times, is finally putting into vacuum drying chamber and dries, obtain the trifluorostyrene polymer.
2. the preparation method of trifluorostyrene polymer according to claim 1, it is characterised in that the step（1）
In, the addition of the trifluorostyrene monomer, deionized water and emulsifying agent is：The trifluorostyrene monomer is in deionized water
In mass concentration be 150~350g/L；The addition of the emulsifying agent is the 1/20~3/20 of trifluorostyrene monomer mass.
3. the preparation method of trifluorostyrene polymer according to claim 1 or 2, it is characterised in that the emulsification
Agent is the mixture of dodecyl sodium sulfate, lauryl sodium sulfate and lauryl amine hydrochloric acid sodium.
4. the preparation method of trifluorostyrene polymer according to claim 3, it is characterised in that the dodecyl
The mixing quality ratio of sodium sulfonate, lauryl sodium sulfate and lauryl amine hydrochloric acid sodium is 1：2~3:2~3.
5. the preparation method of trifluorostyrene polymer according to claim 1, it is characterised in that the step（1）
In, the pre-emulsification time is 1.5~3h.
6. the preparation method of trifluorostyrene polymer according to claim 1, it is characterised in that the step（2）
In, the initiator is that mass ratio is 2~3:The mixed system of the 1 light sodium of potassium peroxydisulfate and sulfurous acid, the initiator plus
It is the 1/200~1/100 of the trifluorostyrene monomer mass to enter amount.
7. the preparation method of trifluorostyrene polymer according to claim 1, it is characterised in that the step（2）
In, the condition of the emulsification is：55~60 DEG C of constant temperature heating water-baths, emulsification times are 55~65h.
8. the preparation method of trifluorostyrene polymer according to claim 1, it is characterised in that the step（4）
In, the vacuum drying condition is：0.5~0.8MPa of vacuum, temperature is 60~80 DEG C, and the time is 15~20h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710329389.8A CN107254012A (en) | 2017-05-11 | 2017-05-11 | A kind of preparation method of trifluorostyrene polymer |
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| CN201710329389.8A CN107254012A (en) | 2017-05-11 | 2017-05-11 | A kind of preparation method of trifluorostyrene polymer |
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| CN107254012A true CN107254012A (en) | 2017-10-17 |
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| CN201710329389.8A Withdrawn CN107254012A (en) | 2017-05-11 | 2017-05-11 | A kind of preparation method of trifluorostyrene polymer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113549168A (en) * | 2021-08-19 | 2021-10-26 | 上海华谊三爱富新材料有限公司 | Preparation method of polytrifluorochloroethylene |
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2017
- 2017-05-11 CN CN201710329389.8A patent/CN107254012A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113549168A (en) * | 2021-08-19 | 2021-10-26 | 上海华谊三爱富新材料有限公司 | Preparation method of polytrifluorochloroethylene |
| WO2023019727A1 (en) * | 2021-08-19 | 2023-02-23 | 常熟三爱富中昊化工新材料有限公司 | Preparation method for polytrifluorostyrene |
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Application publication date: 20171017 |