CN113956835A - Organosilicon sealant for U-shaped heating pipe and preparation method thereof - Google Patents

Abstract

The invention relates to the technical field of adhesives, in particular to an organosilicon sealant for a U-shaped heating pipe, which comprises the following components in percentage by mass: 100-150 parts of alpha, omega-dihydroxy polysiloxane, 10-20 parts of ketoxime crosslinking agent, 0-100 parts of filler, 1-5 parts of organic titanium catalyst, 1-3 parts of aminosilane coupling agent, 50-150 parts of vinyl silicone oil and 0.1-0.5 part of peroxide. By means of vinyl silicone oil and peroxide, on the basis of keeping the original heat resistance, the organic silicon sealant can be deeply cured through high temperature, and meanwhile, the mechanical property is greatly improved. The organosilicon sealant prepared by the invention has the advantages of single component, high temperature resistance, low manufacturing cost, suitability for U-shaped heating pipes and other parts with higher requirements on deep curing and temperature resistance, and wide application.

Description

Organosilicon sealant for U-shaped heating pipe and preparation method thereof

Technical Field

The invention relates to the technical field of adhesives, in particular to an organosilicon sealant for a U-shaped heating pipe and a preparation method thereof.

Background

The silicone rubber sealant is widely applied to the industries of automobiles, buildings, petrochemical industry, machine manufacturing and the like. In the household appliance industry, a large amount of organosilicon sealants are used for sealing, and are commonly used for sealing U-shaped heating pipes, induction cookers, ovens and the like. The U-shaped heating pipe has very strict requirements, requires high temperature resistance, insulation and low compression set, and needs deep encapsulation due to the manufacturing process problem. The organosilicon sealant takes hydroxyl-terminated polysiloxane as a basic polymer, and other auxiliary agents are added at the same time. The organosilicon sealant not only has weather resistance, heat resistance, cold resistance and adhesiveness, but also has the characteristics of low price, convenient operation and the like. 107 silicon rubber is taken as a main body, low-viscosity vinyl silicone oil is introduced, and secondary vulcanization is carried out under the high-temperature condition, so that the sealant with good high-temperature resistance, low compression set and insulation can be prepared. Chinese patent publication No. CN102093837B discloses a single-component high-temperature-resistant gasket-free sealant and a preparation method thereof, wherein the high-temperature resistance is increased by adding phenyl polysiloxane, but the cost is higher and deep curing cannot be carried out.

Based on the technical scheme, the invention designs the organic silicon sealant for the U-shaped heating pipe and the preparation method thereof, so as to solve the technical problems.

Disclosure of Invention

The invention aims to provide an organosilicon sealant for a U-shaped heating pipe and a preparation method thereof, which are used for solving the technical problems.

In order to achieve the purpose, the invention provides the following technical scheme: the organic silicon sealant for the U-shaped heating pipe comprises the following components in parts by weight

Preferably, the alpha, omega-dihydroxy polysiloxane (107 silicone rubber) is a polysiloxane mixture of one or more than two of fluid viscosity 1500-.

Preferably, the ketoxime cross-linking agent is one or a mixture of more than two of methyl tributyl ketoxime silane, vinyl tributyl ketoxime silane, phenyl tributyloxime silane, tetrabutoxime silane and methyl triacetone ketoxime silane.

Preferably, the filler is one or a mixture of more than two of gas-phase titanium dioxide, carbon black, white carbon black, ferroferric oxide, ferric oxide, cerium oxide and MQ silicon resin.

Preferably, the organic titanium catalyst is one or a mixture of more than two of acetylacetone titanate, ethyl acetoacetate titanate and isopropyl titanate.

Preferably, the aminosilane coupling agent is one or a mixture of more than two of gamma-aminopropyltrimethoxysilane (KH-540), gamma-aminopropyltriethoxysilane (KH-550) and N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane (KH-792), and the aminosilane coupling agent is a primary amine coupling agent or a secondary amine coupling agent.

Preferably, the vinyl silicone oil is one or a mixture of more than two terminal vinyl polydimethylsiloxanes with the fluid viscosity of 500-.

Preferably, the peroxide is one or a mixture of more than two of di-tert-butyl peroxide (DTBP) and dicumyl peroxide (DCP).

A preparation method of an organosilicon sealant for a U-shaped heating pipe comprises the following process steps:

s1, adding alpha, omega-dihydroxy polysiloxane and filler into a power mixer according to the mass part ratio, stirring for 20min, heating to 120 ℃, vacuumizing and stirring for 3 hours;

s2, naturally cooling to room temperature, adding the ketoxime cross-linking agent, and stirring for 20min in vacuum;

and S3, adding an aminosilane coupling agent, a titanium catalyst, vinyl silicone oil and peroxide, and stirring for 20min in vacuum to obtain the uniform, fine and flowable single-component organosilicon sealant.

Compared with the prior art, the invention has the beneficial effects that: by means of vinyl silicone oil and peroxide, on the basis of keeping the original heat resistance, the organic silicon sealant can be deeply cured through high temperature, and meanwhile, the mechanical property is greatly improved. The organosilicon sealant prepared by the invention has the advantages of single component, high temperature resistance, low manufacturing cost, suitability for U-shaped heating pipes and other parts with higher requirements on deep curing and temperature resistance, and wide application.

Detailed Description

The present invention will be further described with reference to the following examples, which are intended to illustrate only some, but not all, of the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

The organic silicon sealant for the U-shaped heating pipe comprises the following components in percentage by mass:

wherein the fluid viscosity of the alpha, omega-dihydroxy polysiloxane is 1500cps, and the fluid viscosity of the vinyl silicone oil is 500 cps.

The preparation method comprises the following steps:

s1, adding 100 parts of alpha, omega-dihydroxy polysiloxane, 10 parts of R-974 white carbon black and 10 parts of ferroferric oxide into a power mixer, stirring for 20min, heating to 120 ℃, vacuumizing and stirring for 3 hours;

s2, naturally cooling to room temperature, adding 10 parts of methyl tributyl ketoxime silane and 5 parts of vinyl tributyl ketoxime silane, and stirring for 20min in vacuum;

and S3, adding 1 part of gamma-aminopropyltriethoxysilane, 2 parts of acetylacetone titanate, 50 parts of vinyl silicone oil and 0.1 part of di-tert-butyl peroxide, and stirring for 20min under vacuum to obtain the uniform, fine and flowable one-component organosilicon sealant.

Example 2

The organic silicon sealant for the U-shaped heating pipe comprises the following components in percentage by mass:

wherein the fluid viscosity of the alpha, omega-dihydroxy polysiloxane is 1500cps, and the fluid viscosity of the vinyl silicone oil is 500 cps.

The preparation method comprises the following steps:

s1, adding 100 parts of alpha, omega-dihydroxy polysiloxane, 10 parts of R-974 white carbon black and 10 parts of ferroferric oxide into a power mixer, stirring for 20min, heating to 120 ℃, vacuumizing and stirring for 3 hours;

s2, naturally cooling to room temperature, adding 10 parts of methyl tributyl ketoxime silane and 5 parts of vinyl tributyl ketoxime silane, and stirring for 20min in vacuum;

and S3, adding 1 part of gamma-aminopropyltriethoxysilane, 2 parts of acetylacetone titanate, 100 parts of vinyl silicone oil and 0.2 part of di-tert-butyl peroxide, and stirring for 20min under vacuum to obtain the uniform, fine and flowable one-component organosilicon sealant.

Example 3

The organic silicon sealant for the U-shaped heating pipe comprises the following components in percentage by mass:

wherein the fluid viscosity of the alpha, omega-dihydroxy polysiloxane is 1500cps, and the fluid viscosity of the vinyl silicone oil is 500 cps.

The preparation method comprises the following steps:

s1, adding 100 parts of alpha, omega-dihydroxy polysiloxane, 10 parts of R-974 white carbon black and 10 parts of ferroferric oxide into a power mixer, stirring for 20min, heating to 120 ℃, vacuumizing and stirring for 3 hours;

s2, naturally cooling to room temperature, adding 10 parts of methyl tributyl ketoxime silane and 5 parts of vinyl tributyl ketoxime silane, and stirring for 20min in vacuum;

and S3, adding 1 part of gamma-aminopropyltriethoxysilane, 2 parts of acetylacetone titanate, 200 parts of vinyl silicone oil and 0.4 part of di-tert-butyl peroxide, and stirring for 20min under vacuum to obtain the uniform, fine and flowable one-component organosilicon sealant.

Comparative example 1

The organic silicon sealant comprises the following components in percentage by mass:

wherein the fluid viscosity of the alpha, omega-dihydroxy polysiloxane is 1500cps, and the fluid viscosity of the methyl silicone oil is 500 cps.

After the organosilicon sealant is prepared, the organosilicon sealant is treated in a polytetrafluoroethylene mold according to GB/T2941, and is cured for 168 hours at the temperature of 23 +/-2 ℃.

The performance of the organosilicon sealant is tested by the following method:

(1) and (3) testing tensile stress strain performance: tensile stress strain testing was performed according to GB/T528.

(2) And (3) testing heat resistance: the material is subjected to a heat resistance test according to GB/T3512, and the aging temperature is 250 ℃, and the aging time is 168 h.

(3) And (3) testing the hardness of the sealant: and (4) carrying out a hardness test on the sealant according to GB/T531.2.

The results of the room temperature standing property test are shown in the following table:

	example 1	Example 2	Example 3	Comparative example 1
					Tensile strength (Mpa)	1.87	1.61	1.39	1.92
Elongation at Break (%)	456	430	418	460
					Hardness (A)	33	27	22	32

The results of the heat resistance test-related performance test are shown in the following table:

	example 1	Example 2	Example 3	Comparative example 1
					Tensile strength (Mpa)	2.41	2.82	3.36	1.75
Elongation at Break (%)	187	207	198	210
					Hardness (A)	37	41	47	35

As shown in the table, the heat resistance of the organosilicon sealant is greatly improved through secondary vulcanization of the vinyl silicone oil at high temperature, and the tensile strength is greatly improved after high temperature. Other different fillers can be added in the formula, so that the sealant has other properties.

The organosilicon sealant prepared by the invention has the advantages of single component, good heat resistance, capability of solving deep curing, low manufacturing cost, suitability for U-shaped heating pipes and other parts with higher requirements on deep curing and temperature resistance, and wide application.

In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims (9)

1. The organic silicon sealant for the U-shaped heating pipe is characterized in that: the organosilicon sealant comprises the following components in parts by weight

2. The silicone sealant for the U-shaped heating tube as claimed in claim 1, wherein: the alpha, omega-dihydroxy polysiloxane is one or more of polysiloxane mixture with fluid viscosity of 1500-20000 cps.

3. The silicone sealant for the U-shaped heating tube as claimed in claim 1, wherein: the ketoxime cross-linking agent is one or a mixture of more than two of methyl tributyl ketoxime silane, vinyl tributyl ketoxime silane, phenyl tributyl ketoxime silane, tetrabutoxime silane and methyl triacetone ketoxime silane.

4. The silicone sealant for the U-shaped heating tube as claimed in claim 1, wherein: the filler is one or a mixture of more than two of gas-phase titanium dioxide, carbon black, white carbon black, ferroferric oxide, ferric oxide, cerium oxide and MQ silicon resin.

5. The silicone sealant for the U-shaped heating tube as claimed in claim 1, wherein: the organic titanium catalyst is one or a mixture of more than two of acetylacetone titanate, ethyl acetoacetate titanate and isopropyl titanate.

6. The silicone sealant for the U-shaped heating tube as claimed in claim 1, wherein: the amino silane coupling agent is one or a mixture of more than two of gamma-aminopropyl trimethoxy silane, gamma-aminopropyl triethoxy silane and N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy silane.

7. The silicone sealant for the U-shaped heating tube as claimed in claim 1, wherein: the vinyl silicone oil is one or a mixture of more than two terminal vinyl polydimethylsiloxanes with the fluid viscosity of 500-.

8. The silicone sealant for the U-shaped heating tube as claimed in claim 1, wherein: the peroxide is one or a mixture of more than two of di-tert-butyl peroxide and dicumyl peroxide.

9. The preparation method of the silicone sealant for the U-shaped heating pipe as claimed in any one of claims 1 to 8, characterized in that: the method comprises the following process steps:

s1, adding alpha, omega-dihydroxy polysiloxane and filler into a power mixer according to the mass part ratio, stirring for 20min, heating to 120 ℃, vacuumizing and stirring for 3 hours;

s2, naturally cooling to room temperature, adding the ketoxime cross-linking agent, and stirring for 20min in vacuum;

and S3, adding an aminosilane coupling agent, a titanium catalyst, vinyl silicone oil and peroxide, and stirring for 20min in vacuum to obtain the uniform, fine and flowable single-component organosilicon sealant.