CN107629211A - The preparation method and applications of tackifier in a kind of silica gel - Google Patents
The preparation method and applications of tackifier in a kind of silica gel Download PDFInfo
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- CN107629211A CN107629211A CN201711030438.4A CN201711030438A CN107629211A CN 107629211 A CN107629211 A CN 107629211A CN 201711030438 A CN201711030438 A CN 201711030438A CN 107629211 A CN107629211 A CN 107629211A
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- tackifier
- silica gel
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Abstract
The present invention relates to polymeric material field, discloses a kind of preparation method of tackifier in silica gel, comprises the following steps：A. by hydrogen containing siloxane with containing vinyl silanes according to nH:nVi=2:1 1.5 ratio mixing；B. the chloroplatinic acid catalyst of 9 20ppm dosages is added, controlling reaction temperature is reacted 12 hours at 50 90 degrees Celsius；C. room temperature is cooled to, hydrogen containing siloxane and the inhibitor of gross weight containing vinyl silanes 0.5 2% is added, obtains tackifier finished product in silica gel.Obtained interior tackifier described in this method are applied to it has been significantly greatly increased to glass in silicon rubber, PET, TPU, aluminium sheet, copper sheet bonding force, do not influence its mobility, better effects are reached in commercial Application.
Description
Technical field
The present invention relates to polymeric material field, and in particular to the preparation method and applications of tackifier in a kind of silica gel.
Background technology
Addition-type silicon rubber is a kind of organosilicon material that is nonpoisonous and tasteless, having excellent weather resistance and electrical insulating property, is near
Develop one of faster high-grade organosilicon kind over year, with condensed type silicon rubber ratio there is sulfidation not produce accessory substance, receive
Shrinkage is small, can depth vulcanization the features such as, still, due to addition-type silicon rubber self-molecules present polarity is low, its solidify after with
Substrate bonding poor-performing.
Cementability for raising addition-type silicon rubber to institute's contact material, the method for typically taking tackifier in addition, so
And common interior tackifier due to the compatibility with silicon rubber or are easier to form hydrogen bond with silicon rubber, cause the silicon for adding tackifier
Rubber transparency is deteriorated, and mobility is deteriorated.
The content of the invention
The technical problems to be solved by the invention are to put forward a kind of preparation method and applications of tackifier in silica gel, are overcome
The defects of prior art, silica gel is significantly greatly increased to glass during use, PET, TPU, aluminium sheet, copper sheet bonding force, has not influenceed its stream
Dynamic property.
The technical problems to be solved by the invention are achieved by the following technical programs：
The preparation method of tackifier, comprises the following steps in a kind of silica gel：
A. by hydrogen containing siloxane with containing vinyl silanes according to nH:nVi=2:1-1.5（That is the hydrogen-based of hydrogen containing siloxane
The ratio between number and the vinyl number containing vinyl silanes）Ratio mixing；The hydrogen containing siloxane is at least 3 hydrogen atoms
The polysiloxanes being joined directly together with Si, the hydrogen atom are located at the end of the chain or side chain of polysiloxanes, or the end of the chain contains simultaneously with side chain
There is the hydrogen atom being joined directly together with Si；
B. the chloroplatinic acid catalyst of the 9-20ppm of total weight of material used in step a is added, controlling reaction temperature is Celsius in 50-90
Degree, react 1-2 hours；
C. room temperature is cooled to, the inhibitor of hydrogen containing siloxane and the 0.5-2% of gross weight containing vinyl silanes is added, obtains silica gel
Interior tackifier finished product.
Further, the hydrogen content of described hydrogen containing siloxane is 1.0-1.6%.
Further, the described vinyl silanes that contain include vinyltrimethoxy silane, vinyl triacetoxy silicon
Any one in alkane, VTES.
Further, described chloroplatinic acid catalyst includes isopropyl alcohol solution of chloroplatinic acid, chloroplatinic acid tetrahydrofuran solution, chlorine
Platinic acid-divinyl tetramethyl disiloxane complex, chloroplatinic acid -1,3,5,7- tetravinyls -1,3,5,7- tetramethyls-ring four
At least one of siloxanes.
Further, described inhibitor includes at least one of methyl butynol, ethynylcyclohexanol.
The application of tackifier finished product in a kind of described silica gel, using tackifier finished product in the silica gel as hydrogeneous poly- silica
Alkane does the silicone rubber crosslinking agent of add-on type, can also coordinate conventional containing hydrogen silicone oil crosslinked tackifier to be used together, interior tackifier add
Dosage is the 4-10% of silicon rubber weight.
The present invention has the advantages that：
Tackifier primary structure is the si-h bond and vinyltrimethoxy silane on containing hydrogen silicone oil in this（Or vinyl triacetyl
TMOS, VTES）On vinyl addition, by three methoxyl groups（Or acetoxyl group, ethyoxyl）Draw
Enter main chain, introduce the group as enhancing bonding force such as methoxyl group of main chain, different materials are bonded.The interior tackifier can
Crosslinking agent and thickening double action are functioned simultaneously as, and silicon rubber mobility will not be made to be deteriorated because of the addition of tackifier, to glass
Glass, PET, TPU, aluminium sheet, copper sheet have good cementability.
Embodiment
With reference to embodiment, the present invention will be described in detail, and embodiment is only the preferred embodiment of the present invention,
It is not limitation of the invention.
Embodiment 1-3 uses product of the raw material for conventional commercial, and silicon rubber described in embodiment 4-6 is conventional commercial silicon rubber
Glue.
Embodiment 1
The preparation method of tackifier, comprises the following steps in a kind of silica gel：
A. by 1000g Methyl Hydrogen Polysiloxane Fluids（Hydrogen content 1.0%）Mixed with 740g vinyltrimethoxy silanes, i.e., according to nH:
nVi=2:1 ratio mixing；
B. the isopropyl alcohol solution of chloroplatinic acid of the 20ppm dosages of total weight of material used in step a is added, controlling reaction temperature is taken the photograph 80
Family name's degree, react 1 hour；
C. room temperature is cooled to, Methyl Hydrogen Polysiloxane Fluid and the methyl butynol of vinyltrimethoxy silane gross weight 2% is added, obtains
Tackifier finished product in silica gel.
Embodiment 2
The preparation method of tackifier, comprises the following steps in a kind of silica gel：
A. by 1000g Methyl Hydrogen Polysiloxane Fluids（Hydrogen content 1.6%）Mixed with 2784g vinyltriacetoxy silanes, i.e., according to
nH:nVi=2:1.5 ratio mixing；
B. chloroplatinic acid tetrahydrofuran solution, the chloroplatinic acid-divinyl four of the 9ppm dosages of total weight of material used in step a are added
Tetramethyldisiloxane complex, controlling reaction temperature are reacted 2 hours at 80 degrees Celsius；
C. room temperature is cooled to, adds Methyl Hydrogen Polysiloxane Fluid and the methyl butyne of vinyltriacetoxy silane gross weight 0.5%
Alcohol, obtain tackifier finished product in silica gel.
Embodiment 3
The preparation method of tackifier, comprises the following steps in a kind of silica gel：
A. by 1000g Methyl Hydrogen Polysiloxane Fluids with（Hydrogen content 1.2%）Mixed with 1368g VTESs, i.e., according to
nH:nVi=2:1.2 ratio mixing；
B. chloroplatinic acid-the divinyl tetramethyl disiloxane for adding the 15ppm dosages of total weight of material used in step a coordinates
Thing, chloroplatinic acid -1,3,5,7- tetravinyls -1,3,5,7- tetramethyls-cyclotetrasiloxane, controlling reaction temperature at 80 degrees Celsius,
Reaction 1.5 hours；
C. room temperature is cooled to, adds Methyl Hydrogen Polysiloxane Fluid and the ethynylcyclohexanol of VTES gross weight 1%,
Obtain tackifier finished product in silica gel.
Embodiment 4
Using tackifier finished product does as hydrogen containing siloxane the silicone rubber crosslinking tackifier of add-on type and added in silica gel described in embodiment 1
Add in silicon rubber, addition is the 4% of silicon rubber weight.
Embodiment 5
Using tackifier finished product does as hydrogen containing siloxane the silicone rubber crosslinking tackifier of add-on type and added in silica gel described in embodiment 1
Add in silicon rubber, addition is the 10% of silicon rubber weight.
Embodiment 6
Using tackifier finished product does as hydrogen containing siloxane the silicone rubber crosslinking tackifier of add-on type and added in silica gel described in embodiment 1
Add in silicon rubber, addition is the 7% of silicon rubber weight.
In order to further illustrate the present invention, the silicon rubber described in embodiment 4-6 is tested as follows：By above-mentioned silicon rubber
Coated on the base material for needing to be bonded, base material and mixture are then put into 120 degree of baking ovens together and toasted 10 minutes, you can is completed
Addition-type silicon rubber is bonded on base material, then tests the kinematic viscosity, transparency, adhesive property of silicon rubber（Test is cut in drawing,
Using PET, TPU of standard specification, aluminium, copper, glass sheet, two sheets are taken respectively, two panels front end coats silicon rubber after cleaning,
It is sticked one another and waits to be fully cured, every kind of material does 4 groups of drawings and cuts experiment, and XD-121W tensile testing machines carry out tensile shear testing, as a result taken
Average value）.Test result such as following table：
Table 1：Not plus interior tackifier silicon rubber adhesive property test;
| Project | The silicon rubber that embodiment 4 is not added before interior tackifier | The silicon rubber that embodiment 5 is not added before interior tackifier | The silicon rubber that embodiment 6 is not added before interior tackifier |
| Copper sheet draws and cut | 1.014Mpa interfacial failure | 0.878Mpa interfacial failures | 0.918Mpa interfacial failures |
| Aluminium flake draws and cut | 1.015Mpa interfacial failure | 1.009Mpa interfacial failure | 0.939Mpa interfacial failures |
| Sheet glass draws and cut | 0.716Mpa interfacial failures | 0.680Mpa interfacial failures | 0.803Mpa interfacial failures |
| TPU draws and cut | 0.817Mpa interfacial failures | 0.881Mpa interfacial failures | 0.921Mpa interfacial failures |
| PET draws and cut | 1.018Mpa interfacial failure | 0.982Mpa interfacial failures | 1.002Mpa interfacial failure |
| Kinematic viscosity（W centistokes） | 11.1W | 12.0W | 11.5W |
Table 2：The silicon rubber adhesive property of interior tackifier is added to test;
| Project | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Copper sheet draws and cut | 8.134Mpa cohesional failure | 6.353Mpa cohesional failure | 6.954Mpa cohesional failure |
| Aluminium flake draws and cut | 7.945Mpa cohesional failure | 6.547Mpa cohesional failure | 7.388Mpa cohesional failure |
| Sheet glass draws and cut | 7.941Mpa cohesional failure | 6.371Mpa cohesional failure | 7.011Mpa cohesional failure |
| TPU draws and cut | 8.237Mpa cohesional failure | 6.156Mpa cohesional failure | 7.358Mpa cohesional failure |
| PET draws and cut | 8.127Mpa cohesional failure | 6.368Mpa cohesional failure | 7.374Mpa cohesional failure |
| Kinematic viscosity（W centistokes） | 10.5W | 9.5W | 10.1W |
Claims (6)
1. the preparation method of tackifier in a kind of silica gel, it is characterised in that comprise the following steps：
A. by hydrogen containing siloxane with containing vinyl silanes according to nH:nVi=2:1-1.5 ratio mixing；
B. the 9-20ppm of the total weight of material of step a chloroplatinic acid catalyst is added, controlling reaction temperature is at 50-90 degrees Celsius, instead
Answer 1-2 hours；
C. room temperature is cooled to, the inhibitor of hydrogen containing siloxane and the 0.5-2% of gross weight containing vinyl silanes is added, obtains silica gel
Interior tackifier finished product.
2. the preparation method of tackifier in silica gel according to claim 1, it is characterised in that described hydrogen containing siloxane
Hydrogen content be 1.0-1.6%.
3. the preparation method of tackifier in silica gel according to claim 1, it is characterised in that described contains vinyl silanes
Including any one in vinyltrimethoxy silane, vinyltriacetoxy silane, VTES.
4. the preparation method of tackifier in silica gel according to claim 1, it is characterised in that described chloroplatinic acid catalyst
Including isopropyl alcohol solution of chloroplatinic acid, chloroplatinic acid tetrahydrofuran solution, chloroplatinic acid-divinyl tetramethyl disiloxane complex,
At least one of chloroplatinic acid -1,3,5,7- tetravinyls -1,3,5,7- tetramethyls-cyclotetrasiloxane.
5. the preparation method of tackifier in silica gel according to claim 1, it is characterised in that described inhibitor includes first
At least one of base butynol, ethynylcyclohexanol.
6. the application of tackifier finished product in the silica gel described in a kind of claim 1-5 any one, it is characterised in that by the silicon
Tackifier finished product does the silicone rubber crosslinking tackifier of add-on type as hydrogen containing siloxane and is added into silicon rubber in glue, addition
For the 4-10% of silicon rubber weight.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109337644A (en) * | 2018-09-30 | 2019-02-15 | 广州机械科学研究院有限公司 | A kind of add-on type room temperature two-component casting glue and preparation method thereof |
| CN110055010A (en) * | 2019-05-10 | 2019-07-26 | 广州回天新材料有限公司 | A kind of synthesis preparation method of room temperature tackifier |
| CN111363103A (en) * | 2020-03-27 | 2020-07-03 | 无锡市百合花胶粘剂厂有限公司 | Preparation method of tackifier for addition type organic silicon adhesive |
| CN113501961A (en) * | 2021-07-26 | 2021-10-15 | 浙江励德有机硅材料有限公司 | Tackifier, self-adhesive two-component addition type organic silicon pouring sealant prepared from tackifier and preparation method of self-adhesive two-component addition type organic silicon pouring sealant |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109337644A (en) * | 2018-09-30 | 2019-02-15 | 广州机械科学研究院有限公司 | A kind of add-on type room temperature two-component casting glue and preparation method thereof |
| CN110055010A (en) * | 2019-05-10 | 2019-07-26 | 广州回天新材料有限公司 | A kind of synthesis preparation method of room temperature tackifier |
| CN111363103A (en) * | 2020-03-27 | 2020-07-03 | 无锡市百合花胶粘剂厂有限公司 | Preparation method of tackifier for addition type organic silicon adhesive |
| CN111363103B (en) * | 2020-03-27 | 2023-01-10 | 无锡市百合花胶粘剂厂有限公司 | Preparation method of tackifier for addition type organic silicon adhesive |
| CN113501961A (en) * | 2021-07-26 | 2021-10-15 | 浙江励德有机硅材料有限公司 | Tackifier, self-adhesive two-component addition type organic silicon pouring sealant prepared from tackifier and preparation method of self-adhesive two-component addition type organic silicon pouring sealant |
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