CN106810465A - A kind of fluorocarbon resin and preparation method thereof - Google Patents
A kind of fluorocarbon resin and preparation method thereof Download PDFInfo
- Publication number
- CN106810465A CN106810465A CN201611056185.3A CN201611056185A CN106810465A CN 106810465 A CN106810465 A CN 106810465A CN 201611056185 A CN201611056185 A CN 201611056185A CN 106810465 A CN106810465 A CN 106810465A
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- Prior art keywords
- fluorocarbon resin
- component
- weight portions
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- resin according
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/58—Preparation of carboxylic acid halides
- C07C51/60—Preparation of carboxylic acid halides by conversion of carboxylic acids or their anhydrides or esters, lactones, salts into halides with the same carboxylic acid part
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C269/00—Preparation of derivatives of carbamic acid, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups
- C07C269/02—Preparation of derivatives of carbamic acid, i.e. compounds containing any of the groups, the nitrogen atom not being part of nitro or nitroso groups from isocyanates with formation of carbamate groups
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Polyurethanes Or Polyureas (AREA)
Abstract
The present invention relates to resin art, and in particular to a kind of fluorocarbon resin and preparation method thereof.The fluorine carbon monomer of perfluoro radical-containing is obtained as raw material with perfluoro caprylic acid, and fluorocarbon resin copolymer is obtained through polymerisation in solution with other esters monomers.And it is all of without fluororesin in terms of water resistance, alkali resistance, solvent resistance, hardness and surface anti-pollution characteristic to be superior to current market.
Description
Technical field
The present invention relates to resin art, and in particular to a kind of fluorocarbon resin and preparation method thereof.
Background technology
The characteristic of fluorocarbon resin low-surface-energy and low adhesive force, is allowed to excellent weatherability, cold resistance, high temperature resistant, corrosion resistant
The performances such as erosion, chemical proofing and clean surfaces.Can be used as perfluor carbon coating, fluorocarbon surfactant and the fluorine of function admirable
Carbon water and oil repellent agent etc..It is widely used in the key areas such as naval vessel, aircraft, bridge, building, leather chemical industry and medical science.By having
The method of machine Si modification, can not only give full play to the synergy of organosilicon and Organic fluoride, obtain the fluorine silicon tree of function admirable
Fat.And the consumption of fluorine carbon monomer, reduces cost can be reduced.
The content of the invention
It is an object of the invention to provide a kind of fluorocarbon resin and preparation method thereof.
In order to achieve the above object, the present invention is adopted the following technical scheme that：
A kind of fluorocarbon resin, comprising following raw material：Perfluoro caprylic acid, thionyl chloride, monoethanolamine, hexone, 2,4-
Toluene di-isocyanate(TDI).
A kind of preparation method of fluorocarbon resin, comprises the following steps：
（1）It is middle in flask to add the perfluoro caprylic acid of 100 weight portions, the thionyl chloride of 40 ~ 60 weight portions, 1 ~ 2 weight portion to urge
Agent, reacts 1 hour at 75 DEG C, and the cut for collecting 60 ~ 72 DEG C obtains component A；
（2）The monoethanolamine of 20 ~ 30 weight portions is slowly dropped in component A, 30 DEG C of reactions is warming up to and is obtained component B in 3 hours；
（3）By 2, the 4- toluene di-isocyanate(TDI)s of the hexone of 10 ~ 20 weight portions and 15 ~ 25 weight portions in nitrogen gas
It is added dropwise into component B under atmosphere protection, is recrystallized to give component C for light brown clear crystal；
（4）By in component C addition greases, react insulation reactions at 80 DEG C and obtain fluorocarbon resin.
Further, described catalyst is N, N- dimethyl formyls, tetrahydrofuran, in dibutyl tin laurate one
Kind；Preferably N, N- dimethyl formyl.
Further, described resin is methyl methacrylate, ethyl acrylate, the one kind in butyl acrylate；It is preferred that
It is methyl methacrylate.
Beneficial effect
Fluorocarbon resin made by the present invention, is superior in water resistance, alkali resistance, solvent resistance, hardness and surface anti-pollution characteristic
Not fluorine-containing resin.
Implementation method
Below by specific embodiment, technical scheme is further illustrated, but the present invention is not limited
In these examples.
Embodiment 1：
（1）Perfluoro caprylic acid, the thionyl chloride of 40 weight portions, the catalyst of 1 weight portion of 100 weight portions of middle addition in flask,
Reacted 1 hour at 75 DEG C, the cut for collecting 60 ~ 72 DEG C obtains component A；
（2）The monoethanolamine of 20 weight portions is slowly dropped in component A, 30 DEG C of reactions is warming up to and is obtained component B in 3 hours；
（3）2, the 4- toluene di-isocyanate(TDI)s of the hexone of 10 weight portions and 15 weight portions are protected in nitrogen atmosphere
Under be added dropwise into component B, be recrystallized to give component C for light brown clear crystal；
（4）By in component C addition greases, react insulation reactions at 80 DEG C and obtain fluorocarbon resin.
Embodiment 2：
（1）Perfluoro caprylic acid, the thionyl chloride of 50 weight portions, the catalyst of 1 weight portion of 100 weight portions of middle addition in flask,
Reacted 1 hour at 75 DEG C, the cut for collecting 60 ~ 72 DEG C obtains component A；
（2）The monoethanolamine of 25 weight portions is slowly dropped in component A, 30 DEG C of reactions is warming up to and is obtained component B in 3 hours；
（3）2, the 4- toluene di-isocyanate(TDI)s of the hexone of 15 weight portions and 20 weight portions are protected in nitrogen atmosphere
Under be added dropwise into component B, be recrystallized to give component C for light brown clear crystal；
（4）By in component C addition greases, react insulation reactions at 80 DEG C and obtain fluorocarbon resin.
Embodiment 3：
（1）Perfluoro caprylic acid, the thionyl chloride of 60 weight portions, the catalyst of 2 weight portions of 100 weight portions of middle addition in flask,
Reacted 1 hour at 75 DEG C, the cut for collecting 60 ~ 72 DEG C obtains component A；
（2）The monoethanolamine of 30 weight portions is slowly dropped in component A, 30 DEG C of reactions is warming up to and is obtained component B in 3 hours；
（3）2, the 4- toluene di-isocyanate(TDI)s of the hexone of 20 weight portions and 25 weight portions are protected in nitrogen atmosphere
Under be added dropwise into component B, be recrystallized to give component C for light brown clear crystal；
（4）By in component C addition greases, react insulation reactions at 80 DEG C and obtain fluorocarbon resin.
Embodiment 4
By the fluorocarbon resin obtained by embodiment 1 ~ 3 and the not fluorine-containing resin in market carry out water resistance, alkali resistance, solvent resistance,
Hardness and surface anti-pollution characteristic are tested, and are contrasted.
Can be drawn by contrast, the fluorocarbon resin made by the present invention is better than market and sells free-floride in every detection data
Resin.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than the present invention is protected
The limitation of scope, although being elaborated to the present invention with reference to preferred embodiment, one of ordinary skill in the art should manage
Solution, can modify or equivalent, without deviating from the essence and model of technical solution of the present invention to technical scheme
Enclose.
Claims (6)
1. a kind of fluorocarbon resin, it is characterised in that comprising following raw material：Perfluoro caprylic acid, thionyl chloride, monoethanolamine, methyl is different
Butyl ketone, 2,4- toluene di-isocyanate(TDI)s.
2. the preparation method of a kind of fluorocarbon resin according to claim 1, it is characterised in that including：
（1）It is middle in flask to add the perfluoro caprylic acid of 100 weight portions, the thionyl chloride of 40 ~ 60 weight portions, 1 ~ 2 weight portion to urge
Agent, reacts 1 hour at 75 DEG C, and the cut for collecting 60 ~ 72 DEG C obtains component A；
（2）The monoethanolamine of 20 ~ 30 weight portions is slowly dropped in component A, 30 DEG C of reactions is warming up to and is obtained component B in 3 hours；
（3）By 2, the 4- toluene di-isocyanate(TDI)s of the hexone of 10 ~ 20 weight portions and 15 ~ 25 weight portions in nitrogen gas
It is added dropwise into component B under atmosphere protection, is recrystallized to give component C for light brown clear crystal；
（4）By in component C addition greases, react insulation reactions at 80 DEG C and obtain fluorocarbon resin.
3. the preparation method of a kind of fluorocarbon resin according to claim 3, it is characterised in that described catalyst is N, N-
Dimethyl formyl, tetrahydrofuran, the one kind in dibutyl tin laurate.
4. the preparation method of a kind of fluorocarbon resin according to claim 4, it is characterised in that described catalyst is N, N-
Dimethyl formyl.
5. the preparation method of a kind of fluorocarbon resin according to claim 3, it is characterised in that described resin is methyl-prop
E pioic acid methyl ester, ethyl acrylate, the one kind in butyl acrylate.
6. the preparation method of a kind of fluorocarbon resin according to claim 2, it is characterised in that described resin is methyl-prop
E pioic acid methyl ester.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611056185.3A CN106810465A (en) | 2016-11-26 | 2016-11-26 | A kind of fluorocarbon resin and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611056185.3A CN106810465A (en) | 2016-11-26 | 2016-11-26 | A kind of fluorocarbon resin and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106810465A true CN106810465A (en) | 2017-06-09 |
Family
ID=59106187
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611056185.3A Pending CN106810465A (en) | 2016-11-26 | 2016-11-26 | A kind of fluorocarbon resin and preparation method thereof |
Country Status (1)
| Country | Link |
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| CN (1) | CN106810465A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0068220A1 (en) * | 1981-06-22 | 1983-01-05 | Mobay Chemical Corporation | Low temperature storage stable liquid diphenylmethane diisocyanates |
| US20090143527A1 (en) * | 2007-01-30 | 2009-06-04 | Thames Shelby F | Glycerol Ester-Free Functionalized Vegetable Oil Derivatives and Their Latex Compounds |
| CN104086458A (en) * | 2014-07-09 | 2014-10-08 | 张家港瀚康化工有限公司 | Preparation method for isocyanate ethyl methacrylate |
-
2016
- 2016-11-26 CN CN201611056185.3A patent/CN106810465A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0068220A1 (en) * | 1981-06-22 | 1983-01-05 | Mobay Chemical Corporation | Low temperature storage stable liquid diphenylmethane diisocyanates |
| US20090143527A1 (en) * | 2007-01-30 | 2009-06-04 | Thames Shelby F | Glycerol Ester-Free Functionalized Vegetable Oil Derivatives and Their Latex Compounds |
| CN104086458A (en) * | 2014-07-09 | 2014-10-08 | 张家港瀚康化工有限公司 | Preparation method for isocyanate ethyl methacrylate |
Non-Patent Citations (2)
| Title |
|---|
| 周晓东等: "全氟碳涂料树脂四元共聚物的研究", 《中国涂料》 * |
| 周晓东等: "全氟碳涂料树脂胶乳的制备研究", 《有机氟工业》 * |
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| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170609 |
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| RJ01 | Rejection of invention patent application after publication |