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Tackifier as well as synthesis method and application thereof

A synthesis method and tackifier technology, which are applied in the direction of adhesives, polymer adhesive additives, adhesive additives, etc., can solve the problems of affecting Si-H content, poor compatibility, and inability to remove Pt.

Active Publication Date: 2021-06-11
ZHEJIANG XINAN CHEM INDAL GROUP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation of tackifier molecules by hydrosilylation has the following disadvantages: 1) The hydrosilylation reaction requires the use of a Pt catalyst, and Pt cannot be completely removed from the system after the reaction
When the tackifier containing Pt is added to the addition-type liquid silicone rubber, it will have a certain impact on the storage stability of the rubber; 2) The hydrosilicon addition reaction is an exothermic reaction. If the tackifier molecule is not properly controlled during the synthesis process, The reaction system is violently exothermic, and there is a certain risk, and the process stability is poor; 3) The Si-H bond-containing substances are simultaneously dehydrogenated under the catalysis of Pt, releasing hydrogen gas, thereby affecting the Si-H content and affecting the hydrosilylation process. Yield; 4) In some tackifier synthetic raw materials, there are multiple reaction sites (containing more than two Si-H bonds and double bonds) in the molecular structure, which leads to the formation of polymers and polymers during the synthesis process and storage process of the reaction substances. Poor compatibility with small molecules, resulting in precipitation, showing storage stability
Patent CN 111417687 discloses a tackifier prepared by hydrogen-containing cyclic body and allyl terephthalate through hydrosilicon addition. In the actual synthesis process, there is polymerization, which leads to precipitation and continuous precipitation during storage. White precipitate, which eventually leads to poor storage stability and affects the transparency of the compound after being added to the compound

Method used

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  • Tackifier as well as synthesis method and application thereof
  • Tackifier as well as synthesis method and application thereof
  • Tackifier as well as synthesis method and application thereof

Examples

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preparation example Construction

[0056] The present invention also provides a kind of synthetic method of tackifier, comprises the following steps:

[0057] Mixing the silicone oil with the structure shown in formula (i) and the polar compound, heating and reacting to obtain the tackifier;

[0058]

[0059] In the synthetic method provided by the invention, in formula (i), R 0 for NH 2 -(CH 2 ) n - and / or SH-(CH 2 ) n -, n is an integer ≥ 0, specifically 0, 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10.

[0060] In the synthetic method provided by the invention, in formula (i), R 2 , R 4 , R 5 , R 6 , R 7 and R 8 Both are based on R’-(CH 2 ) x - represents the same or different groups. Among them, R' is methyl, hydrogen, amino, mercapto, carboxyl, halogen, phenyl, trifluoropropyl, epoxy, vinyl, piperazinyl, N-(β-aminoethyl)-γ- Aminopropyl, one or more of γ-glycidyl etheroxypropyl and γ-methacryloyloxy, preferably one of vinyl, methyl, phenyl, trifluoropropyl and hydrogen atom or more, more preferably met...

Embodiment 1

[0080] Synthesize tackifier according to the reaction route shown in the following formula:

[0081]

[0082] Concrete synthetic steps include:

[0083] Add vinyl-terminated amino silicone oil and methyl acrylate into a glass reactor at a molar ratio of amino group to methyl acrylate of 1:2.5; at 50°C, mechanically stir (speed 100r / min) for 6 hours; The viscosity is 0.09MPa, and the thickener is obtained by distillation under reduced pressure at 60°C;

[0084] Wherein, the vinyl-terminated amino silicone oil is prepared according to the following steps:

[0085] Vinyl terminated simethicone (10 g), aminopropylmethyldiethoxysilane (100 g, 0.524 mol), water (18.9 g, 0.105 mol), KOH (0.0980 g, 0.00175 mol) and DMSO ( 1.0g) was added to a 250mL three-neck flask, equipped with a spherical condenser and a mechanical stirrer; the mixture was gradually heated to 100°C under heating in an oil bath, and stirred at reflux for 4 hours for hydrolysis prepolymerization; the mixture was...

Embodiment 2

[0088] Synthesize tackifier according to the reaction route shown in the following formula:

[0089]

[0090] Concrete synthetic steps include:

[0091] Add vinyl-terminated amino silicone oil and methyl methacrylate into a glass reactor at a molar ratio of 1:2 between amino groups and methyl methacrylate; at 100°C, mechanically stir (speed 100r / min) for 4 hours; vacuum distillation at 0.09MPa at 80°C to obtain a tackifier;

[0092] Wherein, the vinyl-terminated amino silicone oil is prepared according to the following steps:

[0093] Vinyl-terminated phenylmethyl silicone oil (10 g), aminopropylmethyldiethoxysilane (100 g, 0.524 mol), water (18.9 g, 0.105 mol), KOH (0.0980 g, 0.00175 mol) and DMSO ( 1.0g) was added to a 250mL three-neck flask, equipped with a spherical condenser and a mechanical stirrer; the mixture was gradually heated to 100°C under heating in an oil bath, and stirred at reflux for 4 hours for hydrolysis prepolymerization; the mixture was cooled to roo...

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Abstract

The invention belongs to the field of organic silicon materials, and particularly relates to a tackifier as well as a synthesis method and application thereof. The tackifier provided by the invention has a chemical structure as shown in a formula (I); and in the formula (I), R3, R9 and R10 are independently selected from alkyl, vinyl or a hydrogen atom, and at least one of R3, R9 and R10 is vinyl or a hydrogen atom. Vinyl or Si-H bonds are reserved in the tackifier structure, so that the tackifier can participate in liquid silicone rubber to jointly form a chemical crosslinking structure, and the bonding force of the self-adhesive organic liquid silicone rubber and a base material is improved; and the structural main body is polysiloxane, so that the compatibility with silicon rubber is relatively high. The tackifier provided by the invention has selective adhesion to different substrates, specifically, the tackifier has good adhesion to polycarbonate (PC) and glass, has no adhesion to polyphenylene sulfone resin (PPSU) and stainless steel, and is very suitable for injection molding of composite products such as plastics.

Description

technical field [0001] The invention belongs to the field of organosilicon materials, and in particular relates to a tackifier and its synthesis method and application. Background technique [0002] With the promotion of the application of silicone materials, more and more composite products of silicone rubber and other materials have attracted the attention of the market. There is a high demand for bonding in the compounding of addition-type liquid silicone rubber and other materials. [0003] Due to its own inertia, silicone rubber has poor adhesion to most substrates, so the bonding of silicone rubber to substrates has become a key factor in the development of silicone rubber composites. From a physical and chemical point of view, in order to form a perfect bond between the compound and the substrate, the interface between the two must have good wetting. For liquid silicone rubber with polymethylsiloxane as the main structure, at 20°C, its surface tension is about 20×10...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/388C08G77/392C08G77/20C08G77/12C09J11/08C09J183/04
CPCC08G77/388C08G77/392C08G77/20C08G77/12C09J11/08C09J183/04C08L2205/02C08L2205/035C08L2205/025C08L83/08
Inventor 卢杭袁振乐陈丽云徐旋
Owner ZHEJIANG XINAN CHEM INDAL GROUP