CN107858026A - Fluorine carbon UV resins and preparation method thereof - Google Patents
Fluorine carbon UV resins and preparation method thereof Download PDFInfo
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- CN107858026A CN107858026A CN201710960676.9A CN201710960676A CN107858026A CN 107858026 A CN107858026 A CN 107858026A CN 201710960676 A CN201710960676 A CN 201710960676A CN 107858026 A CN107858026 A CN 107858026A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
- C09D4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00
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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
- C08F8/00—Chemical modification by after-treatment
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- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- General Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention proposes a kind of preparation method of fluorine carbon UV resins, comprises the following steps：S1) acid anhydrides, hydroxy acrylate, polymerization inhibitor and catalyst are added in reactor under normal temperature, are warming up to 80~85 DEG C, is incubated 2~3 hours, acid number is tested every half an hour, enters in next step when acid number is close to starting acid value half；S2) continue to be warming up to 100~105 DEG C, add Organic fluoride intermediate, react 3~4 hours；S3 110~115 DEG C) are to slowly warm up to, insulation, every the acid number of 30 minutes test resins, stops reaction when acid number is less than 5, and starts 80 DEG C of cooling, diluent is added and accounts for the 20% of resin total amount, being uniformly mixed to discharge.The present invention reacts to form carboxy acrylic ester by acid anhydrides and hydroxy acrylate, is then reacted with fluororesin, generates the acrylic resin of organic fluorine richness, wherein, hydroxy acrylate plays a part of introducing optical active group.
Description
Technical field
The invention belongs to paint field, in particular to a kind of fluorine carbon UV resins and preparation method thereof.
Background technology
Coating is in addition to the performance required for possessing traditional coating on external wall and bridge, it is also necessary to anti-ultraviolet property
It can require, and common UV resins are difficult to meet its xanthochromia requirement.
The content of the invention
It is an object of the invention to propose a kind of fluorine carbon UV resins and preparation method thereof, pass through acid anhydrides and hydroxy acrylate
Reaction forms carboxy acrylic ester, is then reacted with fluororesin, generates the acrylic resin of organic fluorine richness.
In order to solve the above technical problems, the present invention is achieved using following technical scheme：
A kind of preparation method of fluorine carbon UV resins, comprises the following steps：
S1) by 30~50 parts of acid anhydrides, 15~25 parts of hydroxy acrylate, 0.3~0.8 part of polymerization inhibitor and catalysis under normal temperature
0.3~0.8 part of agent is added in reactor, is warming up to 80~85 DEG C, 2~3 hours is incubated, during which every half an hour test sample
Acid number, when acid number close to feed intake starting acid value half when, into next step；
S2) continue to be warming up to 100~105 DEG C, add molecular weight in 30~50 parts of 30000~50000 Organic fluoride intermediate,
Reaction 3~4 hours；
S3 110~115 DEG C) are to slowly warm up to, insulation, during which every the acid number of 30 minutes test resins, when acid number is less than 5
Stop reaction, and start 80 DEG C of cooling, add diluent and account for the 20% of resin total amount, stir half an hour, treat resin and dilution
Agent is well mixed to discharge.
Preferably, the acid anhydrides is the one or more in phthalic anhydride, maleic anhydride, HHPA.
Preferably, the hydroxy acrylate is hydroxy-ethyl acrylate, hydroxyethyl methacrylate, acrylic acid hydroxypropyl
At least one of ester, methacrylic acid hydroxypropyl fat.
Preferably, the polymerization inhibitor is MEHQ or hydroquinones.
Preferably, the catalyst is p-methyl benzenesulfonic acid.
Preferably, the Organic fluoride intermediate is tetrafluoroethene or trifluoro-ethylene and hydroxy-ethyl acrylate or hydroxypropyl acrylate
Copolymer.
Preferably, the diluent is tetramethylol methane tetraacrylate.
The invention also provides fluorine carbon UV resins made from above-mentioned preparation method.
The present invention have the advantage that compared with prior art for：The present invention is reacted by acid anhydrides and hydroxy acrylate
Carboxy acrylic ester is formed, is then reacted with fluororesin, generates the acrylic resin of organic fluorine richness, wherein, hydroxy acrylic acid
Ester plays a part of introducing optical active group.The naval stores of the present invention has preferable anti-ultraviolet property, and is not easy to
Turn yellow, so as to increase the service life of product.
Embodiment
The present invention is got information about to allow those skilled in the art to become apparent from, the present invention will be made below further
Explanation.
Embodiment 1
The preparation method for the fluorine carbon UV resins that the present embodiment is related to, comprises the following steps：
S1) by phthalic anhydride 30kg, hydroxy-ethyl acrylate 15kg, MEHQ 0.3kg and p-methyl benzenesulfonic acid under normal temperature
0.3kg is added in reactor, is warming up to 80~85 DEG C, is incubated 2~3 hours, during which every the acid number of half an hour test sample,
When acid number close to feed intake starting acid value half when, into next step；
S2) continue to be warming up to 100~105 DEG C, add molecular weight in 30000~50000 Organic fluoride intermediate 30kg, reaction
3~4 hours；Organic fluoride intermediate is the copolymer of tetrafluoroethene and hydroxy-ethyl acrylate
S3 110~115 DEG C) are to slowly warm up to, insulation, during which every the acid number of 30 minutes test resins, when acid number is less than 5
Stop reaction, and start 80 DEG C of cooling, add tetramethylol methane tetraacrylate and account for the 20% of resin total amount, stir half an hour,
Treat that resin and diluent are well mixed and can discharged.
Embodiment 2
The preparation method for the fluorine carbon UV resins that the present embodiment is related to, comprises the following steps：
S1) under normal temperature by maleic anhydride 40kg, hydroxyethyl methacrylate 20kg, MEHQ 0.5kg with
And p-methyl benzenesulfonic acid 0.5kg is added in reactor, 80~85 DEG C are warming up to, is incubated 2~3 hours, is during which surveyed every half an hour
The acid number of test agent, when acid number close to feed intake starting acid value half when, into next step；
S2) continue to be warming up to 100~105 DEG C, add molecular weight in 30000~50000 Organic fluoride intermediate 40kg, reaction
3~4 hours；Organic fluoride intermediate is the copolymer of tetrafluoroethene and hydroxypropyl acrylate.
S3 110~115 DEG C) are to slowly warm up to, insulation, during which every the acid number of 30 minutes test resins, when acid number is less than 5
Stop reaction, and start 80 DEG C of cooling, add tetramethylol methane tetraacrylate and account for the 20% of resin total amount, stir half an hour,
Treat that resin and diluent are well mixed and can discharged.
Embodiment 3
The preparation method for the fluorine carbon UV resins that the present embodiment is related to, comprises the following steps：
S1) by HHPA 50kg, hydroxypropyl acrylate and the common 25kg of methacrylic acid hydroxypropyl fat, hydroquinones under normal temperature
0.8kg and p-methyl benzenesulfonic acid 0.8kg are added in reactor, are warming up to 80~85 DEG C, are incubated 2~3 hours, during which every half
The acid number of hour test sample, when acid number close to feed intake starting acid value half when, into next step；
S2) continue to be warming up to 100~105 DEG C, add molecular weight in 30000~50000 Organic fluoride intermediate 50kg, reaction
3~4 hours；Organic fluoride intermediate is trifluoro-ethylene and hydroxy-ethyl acrylate or the copolymer of hydroxypropyl acrylate.
S3 110~115 DEG C) are to slowly warm up to, insulation, during which every the acid number of 30 minutes test resins, when acid number is less than 5
Stop reaction, and start 80 DEG C of cooling, add tetramethylol methane tetraacrylate and account for the 20% of resin total amount, stir half an hour,
Treat that resin and diluent are well mixed and can discharged.
Embodiment described above only expresses the part kind embodiment of the present invention, and its description is more specific and detailed, but
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that the ordinary skill people for this area
For member, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the present invention's
Protection domain.
Claims (8)
1. a kind of preparation method of fluorine carbon UV resins, it is characterised in that comprise the following steps：
S1) by 30~50 parts of acid anhydrides, 15~25 parts of hydroxy acrylate, 0.3~0.8 part of polymerization inhibitor and catalyst under normal temperature
0.3~0.8 part is added in reactor, is warming up to 80~85 DEG C, 2~3 hours is incubated, during which every half an hour test sample
Acid number, when acid number close to feed intake starting acid value half when, into next step；
S2) continue to be warming up to 100~105 DEG C, add molecular weight in 30~50 parts of 30000~50000 Organic fluoride intermediate, reaction
3~4 hours；
S3 110~115 DEG C) are to slowly warm up to, insulation, during which every the acid number of 30 minutes test resins, is stopped when acid number is less than 5
Only react, and start 80 DEG C of cooling, add diluent and account for the 20% of resin total amount, stir half an hour, treat that resin and diluent mix
Conjunction can uniformly discharge.
2. preparation method according to claim 1, it is characterised in that the acid anhydrides is phthalic anhydride, maleic anhydride, hexahydro
One or more in phthalic anhydride.
3. preparation method according to claim 1, it is characterised in that, the hydroxy acrylate be hydroxy-ethyl acrylate,
At least one of hydroxyethyl methacrylate, hydroxypropyl acrylate, methacrylic acid hydroxypropyl fat.
4. preparation method according to claim 1, it is characterised in that the polymerization inhibitor is for MEHQ or to benzene
Diphenol.
5. preparation method according to claim 1, it is characterised in that the catalyst is p-methyl benzenesulfonic acid.
6. preparation method according to claim 1, it is characterised in that the Organic fluoride intermediate is tetrafluoroethene or trifluoro
Ethene and hydroxy-ethyl acrylate or the copolymer of hydroxypropyl acrylate.
7. preparation method according to claim 1, it is characterised in that the diluent is tetramethylol methane tetraacrylate.
8. fluorine carbon UV resins made from preparation method according to claims 1 to 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710960676.9A CN107858026A (en) | 2017-10-16 | 2017-10-16 | Fluorine carbon UV resins and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710960676.9A CN107858026A (en) | 2017-10-16 | 2017-10-16 | Fluorine carbon UV resins and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107858026A true CN107858026A (en) | 2018-03-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201710960676.9A Pending CN107858026A (en) | 2017-10-16 | 2017-10-16 | Fluorine carbon UV resins and preparation method thereof |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087294A (en) * | 2011-10-28 | 2013-05-08 | 安庆飞凯高分子材料有限公司 | Modified epoxy acrylic acid resin, preparation method and uses thereof |
| CN103342793A (en) * | 2013-05-31 | 2013-10-09 | 成都彭州立源高分子材料有限公司 | Organic fluorine silicon hybrid photosensitive resin and synthesis method thereof |
| CN104292973A (en) * | 2014-10-28 | 2015-01-21 | 成都纳硕科技有限公司 | High drying property ultraviolet photo-curing printing ink for circuit boards |
| CN105837723A (en) * | 2016-04-12 | 2016-08-10 | 湖南省金海科技有限公司 | Ultraviolet light curing fluorocarbon resin and manufacturing method thereof |
| KR20170085632A (en) * | 2016-01-14 | 2017-07-25 | 주식회사 케이씨씨 | Antifouling paint composition comprising fluorinated (meth)acrylate |
-
2017
- 2017-10-16 CN CN201710960676.9A patent/CN107858026A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103087294A (en) * | 2011-10-28 | 2013-05-08 | 安庆飞凯高分子材料有限公司 | Modified epoxy acrylic acid resin, preparation method and uses thereof |
| CN103342793A (en) * | 2013-05-31 | 2013-10-09 | 成都彭州立源高分子材料有限公司 | Organic fluorine silicon hybrid photosensitive resin and synthesis method thereof |
| CN104292973A (en) * | 2014-10-28 | 2015-01-21 | 成都纳硕科技有限公司 | High drying property ultraviolet photo-curing printing ink for circuit boards |
| KR20170085632A (en) * | 2016-01-14 | 2017-07-25 | 주식회사 케이씨씨 | Antifouling paint composition comprising fluorinated (meth)acrylate |
| CN105837723A (en) * | 2016-04-12 | 2016-08-10 | 湖南省金海科技有限公司 | Ultraviolet light curing fluorocarbon resin and manufacturing method thereof |
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Application publication date: 20180330 |
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