CN107759793A - Photo-curable silicone resin and preparation method thereof - Google Patents
Photo-curable silicone resin and preparation method thereof Download PDFInfo
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- CN107759793A CN107759793A CN201710960493.7A CN201710960493A CN107759793A CN 107759793 A CN107759793 A CN 107759793A CN 201710960493 A CN201710960493 A CN 201710960493A CN 107759793 A CN107759793 A CN 107759793A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/445—Block-or graft-polymers containing polysiloxane sequences containing polyester sequences
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/80—Siloxanes having aromatic substituents, e.g. phenyl side groups
Abstract
The present invention proposes a kind of preparation method of photo-curable silicone resin, including S1) acid anhydrides, hydroxy-ethyl acrylate, polymerization inhibitor and catalyst are added in reactor under normal temperature, it is warming up to 80~85 DEG C, insulation 2~3 hours, every the acid number of half an hour test sample, acid number close to feed intake starting acid value half when enter in next step；S2) continue to be warming up to 100~105 DEG C, 20~40 parts of dropping end organic hydroxy silicate, control whole time for adding in 1.5~2 hours, be incubated 1 hour；S3 110~115 DEG C) are to slowly warm up to, insulation, during which every the acid number of 30 minutes test resins, stops reaction when acid number is less than 5, and starts to cool, obtains crude resin；S4) add diluent and account for the 20% of crude resin total amount, stir half an hour, treat that crude resin and diluent are well mixed and produce photo-curable silicone resin.There is the obtained resin oil resistivity pen repeatedly to wipe, and accord with the demands of the market.
Description
Technical field
The invention belongs to paint field, in particular to a kind of photo-curable silicone resin and preparation method thereof.
Background technology
There is certain requirement to resistance to greasy dirt in furniture timber floor and plastic cement, common UV resins are difficult to meet that this will
Ask.Therefore, in the market needs a satisfactory product.
The content of the invention
It is an object of the invention to propose a kind of photo-curable silicone resin and preparation method thereof, pass through acid anhydrides and hydroxyl third
Olefin(e) acid ester reacts to form carboxy acrylic ester, then with terminal hydroxy group organosilicon reaction, generates organic-silicon-modified acrylic resin,
There is the resin oil resistivity pen repeatedly to wipe, and accord with the demands of the market.
In order to solve the above technical problems, the present invention is achieved using following technical scheme：
A kind of preparation method of photo-curable silicone resin, comprises the following steps：
S1) by 40~60 parts of acid anhydrides, 15~30 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, start 20~40 parts of dropping end organic hydroxy silicate, control whole time for adding
In 1.5~2 hours, 1 hour is incubated；
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 to cool, obtain crude resin；
S4) add diluent and account for the 20% of crude resin total amount, stir half an hour, treat that crude resin and diluent are well mixed i.e.
Obtain photo-curable silicone resin.
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 terminal hydroxy group organosilicon is hydrosiloxane.
Preferably, the diluent is trimethylolpropane tris acrylic acid.
The invention also provides photo-curable silicone resin 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, then with terminal hydroxy group organosilicon reaction, generates organic-silicon-modified acrylic resin, the resin has
Oil resistivity pen repeatedly wipes, and accords with the demands of the market.Hydroxy acrylate in the present invention provides photolytic activity point.
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 photo-curable silicone resin that the present embodiment is related to, comprises the following steps：
S1) by phthalic anhydride 40kg, hydroxy-ethyl acrylate 15kg, hydroquinones 0.3kg and p-methyl benzenesulfonic acid 0.3kg under normal temperature
It 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, works as acid
Value close to feed intake starting acid value half when, into next step；
S2) continue to be warming up to 100~105 DEG C, start to drip hydrosiloxane 20kg, control whole time for adding 1.5~2
In hour, 1 hour is incubated；
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 to cool, obtain crude resin；
S4) add trimethylolpropane tris acrylic acid and account for the 20% of crude resin total amount, stir half an hour, treat crude resin and dilute
Release that agent is well mixed to produce photo-curable silicone resin.
Embodiment 2
The preparation method for the photo-curable silicone resin that the present embodiment is related to, comprises the following steps：
S1) by maleic anhydride 50kg, hydroxyethyl methacrylate 20kg, hydroquinones 0.5kg and right under normal temperature
Toluenesulfonic acid 0.5kg is added in reactor, is warming up to 80~85 DEG C, 2~3 hours is incubated, during which every half an hour test specimens
The acid number of product, 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, start to drip hydrosiloxane 30kg, control whole time for adding 1.5~2
In hour, 1 hour is incubated；
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 to cool, obtain crude resin；
S4) add trimethylolpropane tris acrylic acid and account for the 20% of crude resin total amount, stir half an hour, treat crude resin and dilute
Release that agent is well mixed to produce photo-curable silicone resin.
Embodiment 3
The preparation method for the photo-curable silicone resin that the present embodiment is related to, comprises the following steps：
S1) by HHPA 60kg, hydroxypropyl acrylate and the common 30kg of methacrylic acid hydroxypropyl fat, para hydroxybenzene under normal temperature
Methyl ether 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
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, start to drip hydrosiloxane 40kg, control whole time for adding 1.5~2
In hour, 1 hour is incubated；
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 to cool, obtain crude resin；
S4) add trimethylolpropane tris acrylic acid and account for the 20% of crude resin total amount, stir half an hour, treat crude resin and dilute
Release that agent is well mixed to produce photo-curable silicone resin.
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 photo-curable silicone resin, it is characterised in that comprise the following steps：
S1) by 40~60 parts of acid anhydrides, 15~30 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, start 20~40 parts of dropping end organic hydroxy silicate, control whole time for adding to exist
In 1.5~2 hours, 1 hour is incubated；
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 to cool, obtain crude resin；
S4) add diluent and account for the 20% of crude resin total amount, stir half an hour, treat that crude resin and diluent are well mixed and produce light
Cured silicone resin.
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 terminal hydroxy group organosilicon is hydrosiloxane.
7. preparation method according to claim 1, it is characterised in that the diluent is trimethylolpropane tris propylene
Acid.
8. photo-curable silicone resin made from preparation method according to claims 1 to 7.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710960493.7A CN107759793A (en) | 2017-10-16 | 2017-10-16 | Photo-curable silicone resin and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710960493.7A CN107759793A (en) | 2017-10-16 | 2017-10-16 | Photo-curable silicone resin and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107759793A true CN107759793A (en) | 2018-03-06 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710960493.7A Pending CN107759793A (en) | 2017-10-16 | 2017-10-16 | Photo-curable silicone resin and preparation method thereof |
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| Country | Link |
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| CN (1) | CN107759793A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06184269A (en) * | 1992-12-17 | 1994-07-05 | Mitsui Toatsu Chem Inc | Optically curable resin composition having excellent adhesivity |
| US6071226A (en) * | 1994-10-11 | 2000-06-06 | Daicel Chemical Industries, Ltd. | (meth) Acrylate having an alkenyl group, an epoxy (meth) acrylate, a (meth) acrylic resin having alkenyl groups, a (meth) acrylic resin having epoxy groups, a thermosetting resin composition and coating composition |
| JP2000219714A (en) * | 1999-02-02 | 2000-08-08 | Hitachi Kasei Polymer Co Ltd | Photocurable resin composition |
| 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 |
-
2017
- 2017-10-16 CN CN201710960493.7A patent/CN107759793A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH06184269A (en) * | 1992-12-17 | 1994-07-05 | Mitsui Toatsu Chem Inc | Optically curable resin composition having excellent adhesivity |
| US6071226A (en) * | 1994-10-11 | 2000-06-06 | Daicel Chemical Industries, Ltd. | (meth) Acrylate having an alkenyl group, an epoxy (meth) acrylate, a (meth) acrylic resin having alkenyl groups, a (meth) acrylic resin having epoxy groups, a thermosetting resin composition and coating composition |
| JP2000219714A (en) * | 1999-02-02 | 2000-08-08 | Hitachi Kasei Polymer Co Ltd | Photocurable resin composition |
| 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 |
Non-Patent Citations (5)
| Title |
|---|
| 孟泉等: "碱溶性光敏预聚物的合成与光固化性能研究", 《功能材料》 * |
| 宋启煌: "《精细化工工艺学》", 30 June 1955, 化学工业出版社 * |
| 易家宝: "聚硅氧烷接枝改性丙烯酸树脂的合成研究", 《涂料工业》 * |
| 洪仲苓: "《化工有机原料深加工》", 30 June 1997, 化学工业出版社 * |
| 赵临襄: "《化学制药工艺学（第四版）》", 31 August 2015, 中国医药科技出版社 * |
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| PB01 | Publication | ||
| 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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180306 |