CN112940672B - Preparation method of organosilicon foam material with high foaming performance - Google Patents

Preparation method of organosilicon foam material with high foaming performance Download PDF

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CN112940672B
CN112940672B CN202110237880.4A CN202110237880A CN112940672B CN 112940672 B CN112940672 B CN 112940672B CN 202110237880 A CN202110237880 A CN 202110237880A CN 112940672 B CN112940672 B CN 112940672B
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foam material
silicone oil
preparing
high foaming
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CN112940672A (en
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罗伟奇
李志敏
骆海华
刘羽婷
夏国江
朱航天
周佳怡
俞丁
张建新
宋江航
汤继俊
孟春凤
王宇鑫
乔岩欣
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Jiangsu University of Science and Technology
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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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • 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
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • 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
    • C09J171/00—Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2371/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2383/00—Characterised by the use of 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; Derivatives of such polymers
    • C08J2383/04—Polysiloxanes
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00—Characterised by the use of 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; Derivatives of such polymers
    • C08J2483/04—Polysiloxanes
    • C08J2483/05—Polysiloxanes containing silicon bound to hydrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00—Characterised by the use of 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; Derivatives of such polymers
    • C08J2483/04—Polysiloxanes
    • C08J2483/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
    • C—CHEMISTRY; METALLURGY
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    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
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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
    • 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
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Abstract

A preparation method of an organic silicon foam material with high foaming performance belongs to the technical field of organic silicon foam materials, and specifically comprises the following steps: 1) 45-55 parts of vinyl silicone oil, 40-70 parts of alpha-omega-dihydroxy polysiloxane, 20-40 parts of siloxane modified polyether resin, 0.5-1.5 parts of platinum catalyst and filler are uniformly mixed; 2) adding 20-45 parts of hydrogen-containing silicone oil, and stirring to uniformly mix; 3) and smearing the mixture to a construction position. The invention has the beneficial effects that: the siloxane modified polyether resin is creatively added, and the low viscosity of the siloxane modified polyether resin enables the siloxane modified polyether resin to be added with more flame retardant and thixotropic auxiliary agent, so that the silicone foam material prepared by the method has better flame retardant property and thixotropic property, and the manufacturing cost is effectively reduced.

Description

Preparation method of organosilicon foam material with high foaming performance
Technical Field
The invention belongs to the technical field of organic silicon foam materials, and particularly relates to a preparation method of an organic silicon foam material with high foaming performance.
Background art:
the fireproof plugging material is often applied to the fields of nuclear power, rail transit, building fireproof plugging, cable through-wall flame-retardant sealing and the like. For example, in the case of an unexpected fire in a rail transit vehicle, holes and gaps formed when cable ducts, pipes, etc. penetrate are a main path for causing a large-area fire to spread, and a great fire loss is caused. The sealing putty plugging material widely used in vehicle holes at present is often poor in cohesiveness with the material surface, can fall off after being used for a long time, can corrode vehicle cables and cable sleeves, and is not provided with vibration resistance and noise reduction performance.
Disclosure of Invention
In order to solve the technical problems, the invention innovatively adopts alpha-omega-dihydroxy polysiloxane, straight-chain vinyl silicone oil, branched-chain vinyl silicone oil and siloxane modified polyether resin as raw materials, and a filler and a platinum catalyst are added to prepare the high-performance organic silicon foam material, wherein the parts mentioned in the application are parts by mass, and the preparation method comprises the following steps:
1) uniformly mixing 45-55 parts of vinyl silicone oil, 40-70 parts of alpha-omega-dihydroxy polysiloxane, 20-40 parts of siloxane modified polyether resin, 20-45 parts of hydrogen-containing silicone oil and a filler;
2) adding 0.5-1.5% of platinum catalyst, and stirring to mix uniformly;
3) and smearing the mixture to a construction position.
Preferably, the vinyl silicone oil in the step 1) comprises a branched vinyl silicone oil and a straight vinyl silicone oil which are mixed according to a ratio of 1: 1 and mixing.
Preferably, 0-0.3 part of colorant and 0-0.9 part of polymerization inhibitor are also added in the step 1).
Preferably, the polymerization inhibitor is any one of 3-phenyl-1-butyn-3-ol, 3-methyl-1-butyn-3-ol, 3-propyl-1-butyn-3-ol, 1-dimethylsilyloxy-1-ethynyl-cyclohexane or 1-ethynylcyclohexanol, or a combination thereof.
Preferably, the filler in step 1) is any one of a flame retardant or a thixotropic aid or a combination thereof.
Preferably, the flame retardant is aluminum hydroxide, and the thixotropic auxiliary agent is white carbon black.
Preferably, the amount of aluminum hydroxide added is 80 to 120 parts.
Preferably, the mass ratio of the alpha-omega-dihydroxy polysiloxane to the siloxane modified polyether resin is 1: 1 and mixing.
Preferably, the addition amount of the white carbon black accounts for 0.5-5% of the total mass.
Preferably, the platinum catalyst is one or a combination of chloroplatinic acid vinyl siloxane complex, chloroplatinic acid isopropanol complex, chloroplatinic acid diethyl phthalate complex, chloroplatinic acid dibutyl maleate complex or chloroplatinic acid tetrahydrofuran complex.
The beneficial effects of the invention are as follows:
the organic silicon foam sealing material has the characteristics of no halogen, no toxicity and the like, and has good cohesiveness with the surface of the material; and has excellent air tightness, water tightness, radiation resistance, aging resistance, decontamination and the like. The silicone modified polyether resin is creatively added, so that more flame retardant and thixotropic auxiliary agent can be added due to the low viscosity characteristic of the silicone modified polyether resin, the viscosity of a common silicone foaming material is higher, and the auxiliary agent with the high proportion cannot be contained, so that the silicone foam material prepared by the silicone modified polyether resin has better flame retardant property and thixotropic property, and the manufacturing cost is effectively reduced.
Description of the drawings:
fig. 1 is a compression force-displacement curve of the first embodiment.
The specific implementation mode is as follows:
the first implementation mode comprises the following steps:
at room temperature, uniformly mixing 30 parts (the following parts are all parts by mass) of vinyl silicone oil, 20 parts of siloxane modified polyether resin, 70 parts of alpha-omega-dihydroxy polysiloxane and 80 parts of aluminum hydroxide, adding 2 parts of white carbon black, 0.5 part of colorant and 0.9 part of 3-phenyl-1-butyn-3-ol, and uniformly stirring;
adding 45 parts of hydrogen-containing silicone oil and 0.5 part of platinum catalyst, and uniformly stirring; and (3) coating the mixture on the surface to be constructed, and forming the material after the reaction is completed.
The starting materials of the present application are primarily involved in the following two types of reactions:
one is the reaction of straight-chain vinyl silicone oil containing hydrogen silicone oil, namely:
Figure BDA0002959892530000031
Figure BDA0002959892530000041
the second is branched vinyl silicone oil and hydrogen-containing silicone oil, namely:
Figure BDA0002959892530000042
it can be seen from the above reaction formula that the platinum catalyst and the hydrogen-containing silicone oil can be respectively placed in different pre-formulations when in use, and the platinum catalyst and the hydrogen-containing silicone oil are mixed when in use, so that the use is convenient. The thixotropy of the mixture before the reaction can be well improved by adding the white carbon black, the polymerization reaction time is adjusted by adjusting the adding amount of the polymerization inhibitor, and the construction of the organosilicon foam material is more convenient and quick by adding the white carbon black and the polymerization inhibitor, and the improvement of the construction quality is facilitated.
Second embodiment
At room temperature, evenly mixing 25 parts of vinyl silicone oil, namely fifty percent of each of branched vinyl silicone oil and straight-chain vinyl silicone oil, 25 parts of siloxane modified polyether resin, 60 parts of alpha-omega-dihydroxy polysiloxane and 90 parts of aluminum hydroxide, adding 3 parts of white carbon black, 0.4 part of colorant and 0.7 part of 3-phenyl-1-butyn-3-ol, and uniformly stirring;
adding 40 parts of hydrogen-containing silicone oil and 0.8 part of platinum catalyst, and uniformly stirring; and (3) coating the mixture on the surface to be constructed, and forming the material after the reaction is completed.
The third embodiment is as follows:
at room temperature, 20 parts of vinyl silicone oil, namely fifty percent of each of branched vinyl silicone oil and straight-chain vinyl silicone oil, 30 parts of siloxane modified polyether resin, 50 parts of alpha-omega-dihydroxy polysiloxane and 110 parts of aluminum hydroxide are uniformly mixed, 4 parts of white carbon black, 0.2 part of colorant and 0.5 part of 3-phenyl-1-butyn-3-ol are added, and the mixture is uniformly stirred;
adding 30 parts of hydrogen-containing silicone oil and 1.2 parts of platinum catalyst, and uniformly stirring; and (3) coating the mixture on the surface to be constructed, and forming the material after the reaction is completed.
The fourth embodiment:
at room temperature, evenly mixing 10 parts of vinyl silicone oil, namely fifty percent of each of branched vinyl silicone oil and straight vinyl silicone oil, 40 parts of siloxane modified polyether resin, 40 parts of alpha-omega-dihydroxy polysiloxane and 120 parts of aluminum hydroxide, adding 5 parts of white carbon black, and uniformly stirring;
adding 45 parts of hydrogen-containing silicone oil and 1.5 parts of platinum catalyst, and uniformly stirring; and (3) coating the mixture on the surface to be constructed, and forming the material after the reaction is completed.
The following table shows some important parameters of the silicone foams produced in examples one to four:
Figure BDA0002959892530000061
for the organosilicon foam materials prepared by the embodiments 1-4, the foaming time is adjustable and controllable, the foaming multiplying power is close to 2.8 times, the flame retardance accords with the standard of UL-94-V-0, is far superior to similar products on the market, the high and low temperature resistance and the aging resistance of the organosilicon foam materials are also far higher than the existing products on the market, the service life is more than sixty years, and the service temperature range after curing is as follows: the temperature of-50 ℃ to 270 ℃ is very excellent in electrical insulation and chemical stability. In addition, the material has the advantages of no toxicity, moisture resistance, ultraviolet resistance, chemical corrosion resistance, difficult deformation and the like.
The silicone foam material described in example one was prepared into a 50mm diameter test specimen, which was subjected to a compression test according to the method of GB/T1041-92, and the test data are shown in the following table and attached FIG. 1:
Figure BDA0002959892530000071
the comprehensive data show that the foam material prepared by the invention has good compression performance,
the foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, and such changes and modifications are within the scope of the invention as claimed.

Claims (9)

1. A preparation method of a high-foaming-performance organic silicon foam material is characterized by comprising the following steps:
1) 45-55 parts of vinyl silicone oil, 40-70 parts of alpha-omega-dihydroxy polysiloxane, 20-40 parts of siloxane modified polyether resin, 0.5-1.5 parts of platinum catalyst and filler are uniformly mixed; the vinyl silicone oil comprises branched vinyl silicone oil and straight-chain vinyl silicone oil, wherein the weight ratio of the branched vinyl silicone oil to the straight-chain vinyl silicone oil is 1: 1, mixing;
2) adding 20-45 parts of hydrogen-containing silicone oil, and stirring to uniformly mix;
3) and smearing the mixture to a construction position.
2. The method for preparing a high foaming silicone foam material according to claim 1, wherein 0-0.3 part of colorant and 0-0.9 part of polymerization inhibitor are added in step 1).
3. The method for preparing a high foaming silicone foam material according to claim 2, wherein the polymerization inhibitor is any one of 3-phenyl-1-butyn-3-ol, 3-methyl-1-butyn-3-ol, 3-propyl-1-butyn-3-ol, 1-dimethylsilyloxy-1-ethynyl-cyclohexane or 1-ethynylcyclohexanol, or a combination thereof.
4. The method for preparing a high foaming silicone foam material according to claim 1, wherein the filler in step 1) is a flame retardant or a thixotropic aid or a combination thereof.
5. The method for preparing the silicone foam material with high foaming performance according to claim 4, wherein the flame retardant is aluminum hydroxide, and the thixotropic auxiliary agent is white carbon black.
6. The method for preparing a high foaming silicone foam material as recited in claim 5, wherein the amount of aluminum hydroxide added is 80-120 parts.
7. The method for preparing the silicone foam material with high foaming performance according to claim 1, wherein the mass ratio of the alpha-omega-dihydroxy polysiloxane to the siloxane modified polyether resin is 1: 1 and mixing.
8. The preparation method of the high-foaming-performance silicone foam material according to claim 5, characterized in that the addition amount of the white carbon black accounts for 0.5-5% of the total mass.
9. The method for preparing a high foaming silicone foam material according to any one of claims 1 to 8, wherein the platinum catalyst is one or a combination of a chloroplatinic acid vinyl siloxane complex, a chloroplatinic acid isopropanol complex, a chloroplatinic acid diethyl phthalate complex, a chloroplatinic acid dibutyl maleate complex, or a chloroplatinic acid tetrahydrofuran complex.
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Citations (3)

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Publication number Priority date Publication date Assignee Title
CN106589954A (en) * 2017-02-13 2017-04-26 成都硅宝科技股份有限公司 Low viscosity flame-retardant room temperature vulcanized foam silicone rubber and preparation method thereof
CN106832956A (en) * 2017-02-10 2017-06-13 深圳市森日有机硅材料股份有限公司 A kind of preparation method of flame retardant type cold curing foaming liquid silicon rubber
CN111057378A (en) * 2019-12-26 2020-04-24 肇庆皓明有机硅材料有限公司 Foamed silicone rubber foam and preparation method and application thereof

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JPH09316335A (en) * 1996-05-24 1997-12-09 Toray Dow Corning Silicone Co Ltd Liquid silicone rubber composition and preparation thereof
CN103265813B (en) * 2013-05-30 2015-04-01 成都拓利化工实业有限公司 Foaming type encapsulating silica gel composition
CN106566255A (en) * 2016-10-27 2017-04-19 深圳市乐普泰科技股份有限公司 Conductive silicone rubber and preparation method
CN109161205A (en) * 2018-09-04 2019-01-08 杭州之江新材料有限公司 A kind of flame-retardant expanded silicon rubber and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN106832956A (en) * 2017-02-10 2017-06-13 深圳市森日有机硅材料股份有限公司 A kind of preparation method of flame retardant type cold curing foaming liquid silicon rubber
CN106589954A (en) * 2017-02-13 2017-04-26 成都硅宝科技股份有限公司 Low viscosity flame-retardant room temperature vulcanized foam silicone rubber and preparation method thereof
CN111057378A (en) * 2019-12-26 2020-04-24 肇庆皓明有机硅材料有限公司 Foamed silicone rubber foam and preparation method and application thereof

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