CN111004590B - Tackifier, preparation method thereof and silicone rubber composition - Google Patents
Tackifier, preparation method thereof and silicone rubber composition Download PDFInfo
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- CN111004590B CN111004590B CN201911154924.6A CN201911154924A CN111004590B CN 111004590 B CN111004590 B CN 111004590B CN 201911154924 A CN201911154924 A CN 201911154924A CN 111004590 B CN111004590 B CN 111004590B
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
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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
- C08G77/08—Preparatory processes characterised by the catalysts used
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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
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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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
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Abstract
The invention provides a tackifier, which has a structure shown in a formula I. The tackifier can obviously improve the bonding effect between the silicone rubber and the resin base material difficult to bond, so that the silicone rubber and the resin base material difficult to bond are fully bonded, and the tackifier has good metal stripping performance and good industrial application prospect; breaks through the limitation that the common tackifier can only improve the adhesiveness of the conventional general thermoplastic resin base material but can not adhere the resin base material difficult to adhere, and can not influence other performances of the silicone rubber. The experimental results show that: the cohesive failure of the silicon rubber to stainless steel and aluminum sheets is 0%; the cohesive failure on glass fiber PA, PEI, PPSU and PC is more than 90%.
Description
Technical Field
The invention belongs to the technical field of bonding materials, and particularly relates to a tackifier, a preparation method thereof and a silicone rubber composition.
Background
Silicone rubber has been widely used in various fields, for example, as a seal ring for a breathing mask for medical and diving equipment, a seal gasket for various electric appliances (e.g., ovens and microwave ovens), a seal member for automobile parts such as a high-pressure boot for a spark plug and other connectors, because of its excellent properties of high and low temperature resistance, weather aging resistance, ozone resistance, electrical insulation, flame resistance, non-toxicity, non-corrosiveness, and physiological inertness. In many of these applications, silicone rubber is generally bonded to a metal substrate or a resin substrate to perform sealing or protection, however, in the case of general silicone rubber, adhesion to the substrate is often poor and peeling from the substrate is easy.
Currently, in order to improve adhesion of silicone rubber to a substrate, the following three methods are generally used: (1) firstly, coating a primer on the surface of a resin substrate, and then further coating silicon rubber to solidify the resin substrate so as to realize the adhesion of the silicon rubber and the substrate; (2) the molecular structure of the silicon rubber is improved, so that the cohesiveness of the silicon rubber is improved; (3) an adhesion promoter is introduced into the silicone rubber to improve the adhesion between the silicone rubber and the substrate. The method using the primer and the modified silicon rubber molecular structure is complex in operation, long in time consumption and high in cost; the method for introducing the tackifier is simple and easy to implement, shortens the operation time, reduces the cost, improves the working efficiency, and becomes an effective method for improving the cohesiveness of the silicon rubber and the base material.
However, the tackifier in the prior art can improve adhesion of silicone rubber to conventional thermoplastic resins such as to plastics such as an acrylonitrile-butadiene-styrene (ABS) resin, a Polycarbonate (PC) resin, a Polyethylene (PE) resin, a polypropylene (PP) resin, and the like; most patents report tackifiers which solve the adhesion performance between silicone rubbers, but most silicone rubbers and plastics are prepared by metal mold pressing or injection, and silicone rubbers are very easy to stick to a metal mold or difficult to release from a film by adding the tackifiers, so that the silicone rubbers with self-adhesiveness have no industrial application value.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a tackifier, which can improve adhesion between silicone rubber and a resin substrate that is difficult to adhere and is easy to release a film, a method for producing the same, and a silicone rubber composition.
The invention provides a tackifier, which has a structure shown in a formula I:
wherein Me is methyl, and R is selected from methyl, ethyl or phenyl;
x is more than or equal to 1, Y is more than or equal to 0, X + Y is more than or equal to 1 and less than or equal to 20, and X is more than or equal to Y;
2≤n≤20。
preferably, n is 4-10; x is 7-9; and Y is 7-9.
Preferably, n is 6-9; x is 8; and Y is 8.
The invention provides a preparation method of the tackifier according to the technical scheme, which comprises the following steps:
a) mixing a compound with a structure shown in a formula II with toluene and a platinum catalyst to obtain a first mixture; mixing heptamethyltrisiloxane with a structure of formula III and toluene to obtain a second mixture;
b) dropwise adding the second mixture into the first mixture at the temperature of 30-80 ℃ for reaction to obtain an intermediate product with a structure shown in the formula IV;
c) mixing the intermediate product with the structure shown in the formula IV, a cyclosiloxane compound and a balancing catalyst, reacting at 30-70 ℃, and neutralizing to obtain a tackifier; the cyclosiloxane compound is selected from tetramethylcyclotetrasiloxane and/or methylphenylcyclotetrasiloxane.
Preferably, the temperature of the reaction in the step b) is 65-75 ℃.
Preferably, the equilibration catalyst in step c) is selected from one or more of concentrated sulfuric acid, trifluoromethanesulfonic acid, macroporous cation exchange resins, and acid clays.
Preferably, the platinum catalyst in the step a) is selected from one or more of a Speier catalyst, a Karstedt catalyst and a Lamoreaux catalyst;
the platinum catalyst accounts for 5-30 ppm of the total mass of all the raw materials.
The invention provides a silicon rubber composition, which comprises silicon rubber and a tackifier;
the tackifier is the tackifier prepared by the technical scheme.
The invention provides a tackifier, which has a structure shown in a formula I. The tackifier can obviously improve the bonding effect between the silicone rubber and the resin base material difficult to bond, so that the silicone rubber and the resin base material difficult to bond are fully bonded, and the tackifier has good metal stripping performance and good industrial application prospect; breaks through the limitation that the common tackifier can only improve the adhesiveness of the conventional general thermoplastic resin base material but can not adhere the resin base material difficult to adhere, and can not influence other performances of the silicone rubber. The experimental results show that: the cohesive failure of the silicon rubber to stainless steel and aluminum sheets is 0%; the cohesive failure on glass fiber PA, PEI, PPSU and PC is more than 90%.
Drawings
FIG. 1 is an infrared test chart of tackifier A of structural formula 101 prepared in example 1 of the present invention;
FIG. 2 is an infrared test chart of tackifier C of structural formula 103 prepared in example 3 of the present invention.
Detailed Description
The invention provides a tackifier, which has a structure shown in a formula I:
wherein Me is methyl, and R is selected from methyl, ethyl or phenyl;
x is more than or equal to 1, Y is more than or equal to 0, X + Y is more than or equal to 1 and less than or equal to 20, and X is more than or equal to Y;
2≤n≤20。
in the invention, n is preferably 4-10; more preferably, n is 6 to 9;
in the invention, X is more than or equal to 1, Y is more than or equal to 0, X + Y is more than or equal to 1 and less than or equal to 20, and X is more than or equal to Y; more preferably, X is 7-9; y is 7-9; most preferably, X ═ 8; and Y is 8.
In a specific embodiment of the present invention, the adhesion-promoting structure is specifically represented by formula 101, formula 102, or formula 103:
the invention provides a preparation method of the tackifier according to the technical scheme, which comprises the following steps:
a) mixing a compound with a structure shown in a formula II with toluene and a platinum catalyst to obtain a first mixture;
mixing heptamethyltrisiloxane with a structure of formula III and toluene to obtain a second mixture;
b) dropwise adding the second mixture into the first mixture at the temperature of 30-80 ℃ for reaction to obtain an intermediate product with a structure shown in the formula IV;
c) mixing the intermediate product with the structure shown in the formula IV with a siloxane compound and an acidic substance, reacting at 30-70 ℃, and neutralizing to obtain a tackifier; the siloxane compound is selected from tetramethylcyclotetrasiloxane and/or methylphenylcyclotetrasiloxane.
The method provided by the invention has the advantages of mild conditions, simplicity, strong operability and easiness in industrial production.
The compound with the structure of formula II is mixed with toluene and a platinum catalyst to obtain a first mixture. In the invention, the platinum catalyst is selected from one or more of Speier catalyst, Karstedt catalyst and Lamoreaux catalyst.
In the invention, the mass ratio of the compound with the structure of formula II to toluene is preferably 1.8-2.3: 3, and more preferably 2: 3; the platinum catalyst accounts for 5-30 ppm of the total mass of all the raw materials; in a specific embodiment, the platinum catalyst accounts for 15ppm of the total mass of all raw materials.
In the compound with the structure of the formula II, n is 2-20, preferably 4-10, and more preferably 6-9. In a specific embodiment, the compound with the structure of formula II is 1, 6-hexanediol diacrylate or 1, 9-hexanediol diacrylate; the 1, 6-hexanediol diacrylate has a structure shown in a formula 201; the 1, 9-hexanediol diacrylate has a structure represented by formula 202:
heptamethyltrisiloxane having the structure of formula iii was mixed with toluene to give a second mixture. In the invention, the mass ratio of the heptamethyltrisiloxane with the structure of formula III to toluene is preferably 0.8-1.2: 1.
after the first mixture and the second mixture are obtained, the second mixture is dropwise added into the first mixture at the temperature of 30-80 ℃ for reaction to obtain an intermediate product with a structure shown in formula IV.
In the invention, the time for the second mixture to react after being added dropwise into the first mixture is preferably 2.5-3.5 h, and more preferably 3 h. The temperature of the second mixture after dropwise adding into the first mixture is 30-80 ℃, preferably 65-75 ℃. The time for dripping the second mixture into the first mixture is preferably 2.5-3.5 h, and more preferably 3 h.
In a specific embodiment of the present invention, the intermediate product having the structure of formula iv is specifically represented by formula 301 or formula 302:
mixing an intermediate product with a structure shown in formula IV, a cyclosiloxane compound and a balancing catalyst, reacting at 30-70 ℃, and neutralizing to obtain a tackifier; the cyclosiloxane compound is selected from tetramethylcyclotetrasiloxane and/or methylphenylcyclotetrasiloxane.
The invention mixes the intermediate product with the structure of formula IV and the cyclosiloxane compound.
In the present invention, the equilibration catalyst in step c) is selected from one or more of concentrated sulfuric acid, trifluoromethanesulfonic acid, macroporous cation exchange resin and acid clay. In particular embodiments, the equilibration catalyst is selected from 98 wt% concentrated sulfuric acid. The mass ratio of the equilibration catalyst to the cyclosiloxane is 1: 1000-1: 100.
The invention preferably adopts sodium bicarbonate to neutralize; the mass of the sodium bicarbonate is 2-15 times of that of the equilibration catalyst. In the invention, the temperature of the equilibrium reaction is 30-70 ℃, preferably 40-60 ℃, and more preferably 45-55 ℃; in a specific example, the temperature of the equilibration reaction is 50 ℃. The time of the equilibrium reaction is preferably 6-9 h, and more preferably 7-8 h. After the completion of the equilibration reaction, it is preferably cooled to room temperature.
After neutralization, the neutralized product is preferably filtered and then toluene is removed to obtain the tackifier with the structure shown in the formula I. The temperature for removing the methylbenzene is 100 ℃; the pressure for removing toluene is preferably-0.95 MPa.
The invention provides a silicon rubber composition, which comprises silicon rubber and a tackifier;
the tackifier is the tackifier prepared by the technical scheme.
The mass ratio of the silicone rubber to the tackifier is 100: 1.
In the present invention, the silicone rubber can be prepared as follows:
to a dimethylvinylsiloxane-terminated dimethylpolysiloxane (viscosity 30000 mPas at 25 ℃ C., 65 parts) was added a trimethylsilanyl-terminated dimethylpolysiloxane having a vinyl group(vinyl value 0.096mmol/g, 5 parts), fumed silica (BET specific surface area 200 m)2(iv)/g, 25 parts, Ribendeshan QS-20), methylsilazane (6 parts), vinylsilazane (2.5 parts) and water (0.6 part), were uniformly mixed in a kneader/mixer and further heated and mixed at 150 ℃ for 3 hours to obtain a silicone rubber precursor. To the silicone rubber precursor, organohydrogenpolysiloxane (SiH content 7mmol/g, 1.8 parts), a tetramethyldivinylsiloxane solution of chloroplatinic acid (concentration 0.25 wt%, 0.5 part), and an ethanol solution of ethynylcyclohexanol (concentration 10 wt%, 0.8 part) were added, and after uniform mixing for 20min, silicone rubber was obtained.
The silicone rubber composition provided by the invention is tested for its adhesive strength and mold release properties according to the following methods:
100 parts of silicone rubber and 1 part of tackifier of formula (a) are mixed and stirred uniformly at room temperature to obtain the silicone rubber composition. The obtained silicone rubber composition was respectively molded with a glass fiber reinforced polyamide resin substrate (glass fiber PA), a polyetherimide resin (PEI) substrate, a polyphenylene sulfone resin (PPSU), and a polyethylene terephthalate (PC) substrate for 200s at a temperature of 120 ℃ and a pressure of 100MPa, and after cooling, the adhesive strength of the silicone rubber with various resin substrates and the releasability from a metal mold were tested.
In order to further illustrate the present invention, a tackifier, a method for preparing the same, and a silicone rubber composition according to the present invention will be described in detail with reference to examples, which should not be construed as limiting the scope of the present invention.
Example 1
A) A2000 mL four-necked flask equipped with a reflux condenser, thermometer, dropping funnel and mechanical stirrer was charged with (110g) toluene and the compound shown in the following figure: (0.5mol)1, 6-hexanediol diacrylate
And 15ppm of Karstedt catalyst throughout the reaction system;
B) heating to 70 ℃, dropwise adding (1mol) heptamethyltrisiloxane and (110g) toluene in 3h, and reacting at constant temperature of 80 ℃ for 3h to obtain an intermediate reaction product.
Stirring and cooling the reaction product to 50 ℃ (0.3mol) of 1,3,5, 7-tetramethylcyclotetrasiloxane, (1g) 98% concentrated sulfuric acid, stirring for 8h, cooling to room temperature, adding (5g) sodium bicarbonate to neutralize for 2h, filtering, removing low molecules at 110 ℃ (0.95 Mpa) to obtain the tackifier A with the structure of formula 101;
FIG. 1 is an infrared test chart of tackifier A of formula 101 prepared in example 1 of the present invention.
The adhesion effect of the obtained tackifier (a) was tested by the following method: 100 parts of silicone rubber and 1 part of tackifier of formula (a) are mixed and stirred uniformly at room temperature to obtain the silicone rubber composition. The obtained silicone rubber composition was molded with a glass fiber reinforced polyamide resin substrate (glass fiber PA), a polyetherimide resin (PEI) substrate, a polyphenylene sulfone resin (PPSU), and a polyethylene terephthalate (PC) substrate for 200 seconds at a temperature of 120 ℃ and a pressure of 100MPa, respectively, and after cooling, the adhesion strength of the silicone rubber to various resin substrates and the releasability from a metal mold were tested, and the results are shown in table 1.
The silicone rubber can be prepared by the following method: to a dimethylpolysiloxane capped with dimethylvinylmethylsiloxane (viscosity of 30000 mPas at 25 ℃ C., 65 parts) were added a dimethylpolysiloxane capped with trimethylsiloxy group having a vinyl group (vinyl value 0.096mmol/g, 5 parts), fumed silica (BET specific surface area 200 m)2(iv)/g, 25 parts, Ribendeshan QS-20), methylsilazane (6 parts), vinylsilazane (2.5 parts) and water (0.6 part), were uniformly mixed in a kneader/mixer and further heated and mixed at 150 ℃ for 3 hours to obtain a silicone rubber precursor. To the direction ofOrganic hydrogen polysiloxane (SiH content 7mmol/g, 1.8 parts), a tetramethyldivinylsiloxane solution of chloroplatinic acid (concentration 0.25 wt%, 0.5 part) and an ethanol solution of ethynylcyclohexanol (concentration 10 wt%, 0.8 part) were added to the silicone rubber precursor, and uniformly mixed for 20min to obtain silicone rubber.
Example 2
A) A2000 mL four-necked flask equipped with a reflux condenser, thermometer, dropping funnel and mechanical stirrer was charged with (110g) toluene and the compound shown in the following figure: (0.5mol)1, 9-hexanediol diacrylate
And Speier catalyst at 15ppm throughout the reaction system;
B) heating to 70 ℃, dropwise adding (1mol) heptamethyltrisiloxane and (110g) toluene in 3h, and reacting at constant temperature of 80 ℃ for 3h to obtain an intermediate reaction product.
Stirring and cooling the reaction product to 50 ℃ (0.3mol) of 1,3,5, 7-tetramethylcyclotetrasiloxane, (1g) 98% concentrated sulfuric acid, stirring for 8h, cooling to room temperature, adding (5g) sodium bicarbonate to neutralize for 2h, filtering, removing low molecules at 110 ℃ (0.95 MPa), and obtaining the tackifier B with the structure of formula 102;
the adhesion effect of the tackifier of formula (b) on the silicone rubber and the resin base material less likely to be tacky and the releasability from the metal mold were tested in the same manner as in example 1, and the results are shown in Table 1.
Example 3
A) A2000 mL four-necked flask equipped with a reflux condenser, thermometer, dropping funnel and mechanical stirrer was charged with (110g) toluene and the compounds shown below: (0.5mol)1, 6-hexanediol diacrylate
And 15ppm of a Karster catalyst in the whole reaction system;
B) heating to 70 ℃, dropwise adding (1mol) heptamethyltrisiloxane and (110g) toluene in 3h, and reacting at constant temperature of 80 ℃ for 3h to obtain an intermediate reaction product.
Stirring and cooling the reaction product to 50 ℃ (0.3mol)1,3,5, 7-tetramethyl-1, 3,5, 7-tetraphenylcyclotetrasiloxane, (0.3mol)1,3,5, 7-tetramethylcyclotetrasiloxane, (1g) 98% concentrated sulfuric acid, stirring for 8h, cooling to room temperature, adding (5g) sodium bicarbonate to neutralize for 2h, filtering, and removing low molecules at 110 ℃ and-0.95 MPa to obtain the tackifier C with the structure of formula 103.
FIG. 2 is an infrared test chart of tackifier C of formula 103 prepared in example 3 of the present invention.
The tackifier of formula (C) was tested for its adhesive effect between silicone rubber and a resin base material which is hardly adhesive and for mold releasability in accordance with the method of example 1.
TABLE 1 bonding Effect of the tackifiers according to examples 1 to 3 of the present application
| Base material | Example 1 | Example 2 | Example 3 |
| Glass fiber PA | ++++ | ++++ | ++++ |
| PEI | ++++ | ++++ | ++++ |
| PPSU | ++++ | ++++ | ++++ |
| PC | ++++ | ++++ | ++++ |
| Stainless steel | × | × | × |
| Aluminium sheet | × | × | × |
Wherein, each symbol means as follows:
x: cohesive failure 0% (peel);
+: 30 percent or more than 0 percent of cohesive failure;
++: 60% or more than 30% of cohesive failure;
+++: 90% or more than 60% of cohesive failure;
++++: cohesive failure > 90%.
The embodiment shows that the tackifier provided by the invention can obviously improve the bonding effect between the silicone rubber and the resin base material difficult to bond, so that the silicone rubber and the resin base material difficult to bond are fully bonded, and the tackifier has good metal stripping property and good industrial application prospect.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. An adhesion promoter having the structure of formula i:
wherein Me is methyl, and R is selected from methyl, ethyl or phenyl;
x is more than or equal to 1, Y is more than or equal to 0, X + Y is more than or equal to 1 and less than or equal to 20, and X is more than or equal to Y;
2≤n≤20。
2. the adhesion promoter of claim 1, wherein n is 4 to 10; x is 7-9; and Y is 7-9.
3. The adhesion promoter of claim 1, wherein n is 6 to 9; x is 8; and Y is 8.
4. A method for preparing the tackifier according to any one of claims 1 to 3, comprising the steps of:
a) mixing a compound with a structure shown in a formula II with toluene and a platinum catalyst to obtain a first mixture; the mass ratio of the compound with the structure shown in the formula II to the methylbenzene is 1.8-2.3: 3;
mixing heptamethyltrisiloxane with a structure of formula III and toluene to obtain a second mixture; the mass ratio of the heptamethyltrisiloxane with the structure of the formula III to the toluene is 0.8-1.2: 1;
b) dropwise adding the second mixture into the first mixture at the temperature of 30-80 ℃ for reaction to obtain an intermediate product with a structure shown in the formula IV;
c) mixing the intermediate product with the structure shown in the formula IV, a cyclosiloxane compound and a balancing catalyst, and carrying out a balancing reaction at 30-70 ℃ to neutralize to obtain the tackifier with the structure shown in the formula I; the cyclosiloxane compound is selected from tetramethylcyclotetrasiloxane and/or methylphenylcyclotetrasiloxane; the equilibration catalyst is selected from one or more of concentrated sulfuric acid, trifluoromethanesulfonic acid, macroporous cation exchange resin and acid clay; the mass ratio of the equilibration catalyst to the cyclosiloxane compound is 1: 1000-1: 100.
5. The method according to claim 4, wherein the temperature of the reaction in the step b) is 65 to 75 ℃.
6. The preparation method according to claim 4, wherein the platinum catalyst in step a) is selected from one or more of Speier catalyst, Karstedt catalyst and Lamoreaux catalyst;
the platinum catalyst accounts for 5-30 ppm of the total mass of all the raw materials.
7. A silicone rubber composition comprising a silicone rubber and an adhesion promoter;
the tackifier is prepared by the preparation method of any one of claims 1 to 3 or any one of claims 4 to 6.
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| CN105482120A (en) * | 2015-12-18 | 2016-04-13 | 杭州福斯特光伏材料股份有限公司 | Preparation method of tackifier for addition type liquid silicone rubber |
| CN106010423B (en) * | 2016-05-24 | 2019-02-05 | 浙江凌志新材料有限公司 | A kind of preparation method of addition-type silicon rubber adhesion promoters |
| CN106496565B (en) * | 2016-12-08 | 2019-08-30 | 东莞市贝特利新材料有限公司 | A kind of tackifier, preparation method and silicone rubber compound |
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