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Preparation method of deacidification type organic silicon adhesive

A silicone adhesive, deacidification technology, applied in the direction of adhesives, non-polymer adhesive additives, adhesive additives, etc., can solve the problem of acetic acid having a pungent odor, unsuitable for electronic appliances, and unsuitable for cement bonding, etc. Achieve excellent hydrophobic properties, improved shelf life, and improved chemical resistance

Active Publication Date: 2022-01-04
广东巨马新材料有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It is widely used, but its biggest disadvantage is that the by-product of the curing process, acetic acid, has a pungent odor and is corrosive to metals, so it is not suitable for applications in the electrical and electronic industries; A layer of chalk is formed between them and loses the bonding force, so it is not suitable for bonding between cement

Method used

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  • Preparation method of deacidification type organic silicon adhesive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Preparation of acetic acid type crosslinker:

[0028] Step S11. Add sulfuric acid solution to 2-hydroxy-3-methoxybenzaldehyde in an ice-water bath. After adding, stir and react for 50 minutes at 15°C, and then dropwise add α, α, α -Trifluoroacetophenone, heated up to 60°C, stirred for 16 hours, after the reaction, mixed with an equal volume of 50°C deionized water, filtered while hot, and dried the obtained filter cake to obtain intermediate 1; wherein, The mass fraction of sulfuric acid solution is 80%, and the dosage ratio of 2-hydroxy-3-methoxybenzaldehyde, sulfuric acid solution and α,α,α-trifluoroacetophenone is 1.5g:5mL:1.7g;

[0029] Step S12, mixing absolute ethanol and intermediate 1, adding glacial acetic acid, adding an ethanol solution in which amino monomers are dissolved, and heating under reflux at 80°C for 12 hours. After the reaction, the solvent is removed by rotary evaporation to obtain Schiff Alkaline compound; wherein, the amino monomer is aniline;...

Embodiment 2

[0033] Preparation of acetic acid type crosslinker:

[0034] Step S11. Add sulfuric acid solution to 2-hydroxy-3-methoxybenzaldehyde in an ice-water bath. After adding, stir and react for 50 minutes at 15°C, and then dropwise add α, α, α -Trifluoroacetophenone, heated up to 60°C, stirred for 16 hours, after the reaction, mixed with an equal volume of 50°C deionized water, filtered while hot, and dried the obtained filter cake to obtain intermediate 1; wherein, The mass fraction of sulfuric acid solution is 80%, and the dosage ratio of 2-hydroxy-3-methoxybenzaldehyde, sulfuric acid solution and α,α,α-trifluoroacetophenone is 1.5g:5mL:1.7g;

[0035] Step S12, mixing absolute ethanol and intermediate 1, adding glacial acetic acid, adding an ethanol solution in which amino monomers are dissolved, and heating under reflux at 80°C for 12 hours. After the reaction, the solvent is removed by rotary evaporation to obtain Schiff Alkaline compound; wherein, the amino monomer is aniline;...

Embodiment 3

[0039] Preparation of modified fillers:

[0040]Dry the precipitated white carbon black at 150°C for 24 hours, then mix the dried precipitated white carbon black and glycidyl methacrylate according to a certain ratio, and ball mill for 4 hours in a ball mill with a rotating speed of 500r / min. After finishing, wash with acetone, filter, and dry the filter cake at 80° C. to a constant weight to obtain a modified filler. Wherein, the mass ratio of dried precipitated silica to glycidyl methacrylate is 5:2.1.

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Abstract

The invention relates to a preparation method of a deacidification type organic silicon adhesive, and belongs to the technical field of adhesives. The preparation method comprises the steps of adding alpha, omega-dihydroxy polydimethylsiloxane, white oil and an acetic acid type cross-linking agent into a planetary stirrer, and uniformly mixing under a vacuum condition; and adding the modified filler, finally adding the dibutyltin dilaurate, and mixing and stirring to obtain the deacidification type organic silicon adhesive. The principle of the invention is as follows: fluorine-containing groups are introduced into the structure of the acetic acid type cross-linking agent, and fluorine atoms can reduce the surface energy of silicon rubber and reduce the surface activity, so that the organic silicon adhesive has excellent hydrophobic performance. Meanwhile, fluorine atoms have very strong electronegativity, negative electricity shielding is formed around a rubber molecular chain, attack of a nucleophilic reagent can be blocked, and then the chemical resistance of the silicon adhesive is effectively improved through introduction of the fluorine atoms.

Description

technical field [0001] The invention belongs to the technical field of adhesives, and in particular relates to a method for preparing a deacidified silicone adhesive. Background technique [0002] Silicone adhesives are widely used in three systems: deoximation type, dealcoholization type and deacidification type using different crosslinking agents. [0003] Deoxime type and dealcohol type silicone adhesives are mainly used in construction, electronic appliances, new energy and other industries. However, the de-oxime type has general adhesion, and the by-product oxime will corrode copper metals and some plastics; the de-alcoholized type is difficult to preserve and has a slow curing speed. The deacidified type is a one-component room temperature curing silicone adhesive. It is widely used, but its biggest disadvantage is that the by-product of the curing process, acetic acid, has a pungent odor and is corrosive to metals, so it is not suitable for applications in the elect...

Claims

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Application Information

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IPC IPC(8): C09J183/04C09J11/04C09J11/06
CPCC09J183/04C09J11/04C09J11/06C08K9/04C08K7/26C08K5/5465
Inventor 王彬罗伟邓戈陈海东黎春湄陈艳清梁倩映侯星平戴海英
Owner 广东巨马新材料有限公司