CN109694577A - A kind of permeability organosilicon material and preparation method thereof - Google Patents

A kind of permeability organosilicon material and preparation method thereof Download PDF

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Publication number
CN109694577A
CN109694577A CN201710985460.8A CN201710985460A CN109694577A CN 109694577 A CN109694577 A CN 109694577A CN 201710985460 A CN201710985460 A CN 201710985460A CN 109694577 A CN109694577 A CN 109694577A
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China
Prior art keywords
parts
silicone oil
permeability
organosilicon material
heat preservation
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CN201710985460.8A
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Chinese (zh)
Inventor
高川
余海艳
王煦怡
赵奕
刘咏梅
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China Bluestar Chengrand Research Institute of Chemical Industry Co Ltd
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China Bluestar Chengrand Research Institute of Chemical Industry Co Ltd
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Priority to CN201710985460.8A priority Critical patent/CN109694577A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J9/00Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
    • C08J9/04Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
    • C08J9/06Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
    • C08J9/08Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing carbon dioxide
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2203/00Foams characterized by the expanding agent
    • C08J2203/02CO2-releasing, e.g. NaHCO3 and citric acid
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2383/00Characterised 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
    • C08J2383/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2483/00Characterised 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
    • C08J2483/04Polysiloxanes
    • C08J2483/05Polysiloxanes containing silicon bound to hydrogen

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The present invention relates to a kind of permeability organosilicon materials and preparation method thereof, belong to organosilicon technical field.The organosilicon material includes following raw materials in parts by weight: 80-100 parts of hydroxy silicon oil, 5-10 parts of vinyl silicone oil, 15-20 parts of containing hydrogen silicone oil, 3-5 parts of dibutyl tin dilaurate, 3-5 parts of quaternary ammonium base, 10-15 parts of fume colloidal silica, 5-10 parts of nanometer calcium carbonate.Silicone foam of the invention has the process conditions of relatively optimization, and products obtained therefrom has excellent properties, uniform foam cell, fine and closely woven, elastic good and tool high-fire resistance.

Description

A kind of permeability organosilicon material and preparation method thereof
Technical field
The present invention relates to a kind of organosilicon materials and preparation method thereof, it is more particularly related to which a kind of permeability has Machine silicon materials and preparation method thereof belong to organosilicon technical field.
Background technique
Flexible foams are a big verieties of foamed plastics, because soft, elasticity is good, be widely used in industry, agricultural, The fields such as communications and transportation, military affairs, building and daily necessities.Silicone foam is one of novel polymer soft foam Material, Silicone foam alternately forms main chain by silicon oxygen bond, inorganic by a kind of the half of silicon and organic group composition side chain High molecular material.Due to the particularity of its structure, therefore the excellent properties that cannot be provided simultaneously with many other materials, it is such as tall and erect High temperature resistant more and lower temperature resistance, it is excellent be electrically insulated with chemical stability, good resistance to ag(e)ing, surface-active outstanding, Hydrophobic is moisture-proof and physiological inertia etc..Usually as materials such as damping, sound insulation, damping, electrical isolation encapsulation, it is applied to aerospace and leads Lightweight, high temperature resistant, moisture repellent material of the domain as spacecraft, rocket etc..Also it can be used as the filling damping of propeller, wing, cabin The heat-insulating material of material and fiery wall.The 1950s, Dow corning company took the lead in developing Silicone foam, and High temperature resistant product is manufactured with it.After, the Bayer AG of Japanese company, SHIN-ETSU HANTOTAI, the General Electric in the U.S. and Germany Also start to be studied.China is since 20th century 30, the forties, no matter in terms of research also to the research of foamed material It is material production aspect, there are also no small gaps compared with foreign level.
State Intellectual Property Office discloses a Publication No. CN101802102A, entitled " condensation in 2010.08.11 The invention of the silicon foams of crosslinking ", the invention are related to method for producing silicon foams, reaction mixture and double groups Subsystem, wherein in one first reaction of the compound at least one Si -- H, in a kind of depositing for base catalyst Release hydrogen under, and in one second reaction reaction mixture in a kind of metallic catalyst in the presence of be crosslinked.
The above-mentioned silicon foams being prepared, abscess is uneven, fine and closely woven, and elasticity and heat resistance are poor.
Summary of the invention
Present invention seek to address that the problem of organosilicon material in the prior art, provide a kind of permeability organosilicon material, it should Organosilicon material has excellent properties, uniform foam cell, fine and closely woven, elastic good and tool high-fire resistance.
In order to achieve the above-mentioned object of the invention, specific technical solution is as follows:
A kind of permeability organosilicon material, it is characterised in that: including following raw materials in parts by weight:
80-100 parts of hydroxy silicon oil
5-10 parts of vinyl silicone oil
15-20 parts of containing hydrogen silicone oil
3-5 parts of dibutyl tin dilaurate
3-5 parts of quaternary ammonium base
10-15 parts of fume colloidal silica
5-10 parts of nanometer calcium carbonate.
Currently preferred, O.015-0.20Pas the viscosity of the hydroxy silicon oil is.
Currently preferred, the viscosity of the vinyl silicone oil is 0.5-1.0Pas, contents of ethylene >=9%.
It is currently preferred, reactive hydrogen mass fraction >=1.6% of the containing hydrogen silicone oil.
A kind of preparation method of permeability organosilicon material, it is characterised in that: comprise the following steps that:
A, have in electric stirring, feed opening and condensation pipe reactor in one and hydroxy silicon oil is added according to recipe requirements;Addition is urged Agent dibutyl tin dilaurate, the pre-polymerization 1.5-2.0h at 130-150 DEG C obtain pre- silicone oil, spare;
B, the pre- silicone oil for obtaining step A mixes simultaneously with vinyl silicone oil, fume colloidal silica and nanometer calcium carbonate, quaternary ammonium base It stirs evenly;Containing hydrogen silicone oil is added, reaction system is warming up to 170-175 DEG C after mixing evenly, makes reaction system in normal pressure item It independently foams under part;The foaming body for completing to obtain after foaming is taken out and keeps it completely cooling at room temperature;
C, foaming body after cooling is placed within baking oven;It is warming up to 95-100 DEG C in 0.5-1.0h, keeps the temperature 1-2h;125- 130 DEG C of heat preservation 1-2h;155-160 DEG C of heat preservation 1-2h;170-180 DEG C of heat preservation 1-2h;190-200 DEG C of heat preservation 2-3h is up to product.
Bring advantageous effects of the present invention:
The present invention is matched and formula appropriate and work according to the preparation principle of Silicone foam using low viscosity hydroxy silicon oil Skill, is prepared for Silicone foam, and Silicone foam of the invention has the process conditions of relatively optimization, products obtained therefrom tool There are excellent properties, uniform foam cell, fine and closely woven, elastic good and tool high-fire resistance.
Specific embodiment
Embodiment 1
A kind of permeability organosilicon material, including following raw materials in parts by weight:
80 parts of hydroxy silicon oil
5 parts of vinyl silicone oil
15 parts of containing hydrogen silicone oil
3 parts of dibutyl tin dilaurate
3 parts of quaternary ammonium base
10 parts of fume colloidal silica
5 parts of nanometer calcium carbonate.
Embodiment 2
A kind of permeability organosilicon material, including following raw materials in parts by weight:
100 parts of hydroxy silicon oil
10 parts of vinyl silicone oil
20 parts of containing hydrogen silicone oil
5 parts of dibutyl tin dilaurate
5 parts of quaternary ammonium base
15 parts of fume colloidal silica
10 parts of nanometer calcium carbonate.
Embodiment 3
A kind of permeability organosilicon material, including following raw materials in parts by weight:
90 parts of hydroxy silicon oil
7.5 parts of vinyl silicone oil
17.5 parts of containing hydrogen silicone oil
4 parts of dibutyl tin dilaurate
4 parts of quaternary ammonium base
12.5 parts of fume colloidal silica
7.5 parts of nanometer calcium carbonate.
Embodiment 4
A kind of permeability organosilicon material, including following raw materials in parts by weight:
88 parts of hydroxy silicon oil
6 parts of vinyl silicone oil
19 parts of containing hydrogen silicone oil
3.3 parts of dibutyl tin dilaurate
3.2 parts of quaternary ammonium base
11 parts of fume colloidal silica
8 parts of nanometer calcium carbonate.
Embodiment 5
A, have in electric stirring, feed opening and condensation pipe reactor in one and hydroxy silicon oil is added according to recipe requirements;Addition is urged Agent dibutyl tin dilaurate, the pre-polymerization 1.5h at 130 DEG C obtain pre- silicone oil, spare;
B, the pre- silicone oil for obtaining step A mixes simultaneously with vinyl silicone oil, fume colloidal silica and nanometer calcium carbonate, quaternary ammonium base It stirs evenly;Containing hydrogen silicone oil is added, reaction system is warming up to 170 DEG C after mixing evenly, makes reaction system in atmospheric conditions Autonomous foaming;The foaming body for completing to obtain after foaming is taken out and keeps it completely cooling at room temperature;
C, foaming body after cooling is placed within baking oven;It is warming up to 95 DEG C in 0.5h, keeps the temperature 1h;125 DEG C of heat preservation 1h;155 DEG C heat preservation 1h;170 DEG C of heat preservation 1h;190 DEG C of heat preservation 2h are up to product.
Embodiment 6
A, have in electric stirring, feed opening and condensation pipe reactor in one and hydroxy silicon oil is added according to recipe requirements;Addition is urged Agent dibutyl tin dilaurate, the pre-polymerization 2.0h at 150 DEG C obtain pre- silicone oil, spare;
B, the pre- silicone oil for obtaining step A mixes simultaneously with vinyl silicone oil, fume colloidal silica and nanometer calcium carbonate, quaternary ammonium base It stirs evenly;Containing hydrogen silicone oil is added, reaction system is warming up to 175 DEG C after mixing evenly, makes reaction system in atmospheric conditions Autonomous foaming;The foaming body for completing to obtain after foaming is taken out and keeps it completely cooling at room temperature;
C, foaming body after cooling is placed within baking oven;It is warming up to 100 DEG C in 1.0h, keeps the temperature 2h;130 DEG C of heat preservation 2h;160 DEG C heat preservation 2h;180 DEG C of heat preservation 2h;200 DEG C of heat preservation 3h are up to product.
Embodiment 7
A, have in electric stirring, feed opening and condensation pipe reactor in one and hydroxy silicon oil is added according to recipe requirements;Addition is urged Agent dibutyl tin dilaurate, the pre-polymerization 1.75h at 140 DEG C obtain pre- silicone oil, spare;
B, the pre- silicone oil for obtaining step A mixes simultaneously with vinyl silicone oil, fume colloidal silica and nanometer calcium carbonate, quaternary ammonium base It stirs evenly;Containing hydrogen silicone oil is added, reaction system is warming up to 172.5 DEG C after mixing evenly, makes reaction system in condition of normal pressure Lower autonomous foaming;The foaming body for completing to obtain after foaming is taken out and keeps it completely cooling at room temperature;
C, foaming body after cooling is placed within baking oven;It is warming up to 97.5 DEG C in 0.75h, keeps the temperature 1.5h;127.5 DEG C of heat preservations 1.5h;157.5 DEG C heat preservation 1.5h;175 DEG C of heat preservation 1.5h;195 DEG C of heat preservation 2.5h are up to product.
Embodiment 8
A, have in electric stirring, feed opening and condensation pipe reactor in one and hydroxy silicon oil is added according to recipe requirements;Addition is urged Agent dibutyl tin dilaurate, the pre-polymerization 1.8h at 132 DEG C obtain pre- silicone oil, spare;
B, the pre- silicone oil for obtaining step A mixes simultaneously with vinyl silicone oil, fume colloidal silica and nanometer calcium carbonate, quaternary ammonium base It stirs evenly;Containing hydrogen silicone oil is added, reaction system is warming up to 171 DEG C after mixing evenly, makes reaction system in atmospheric conditions Autonomous foaming;The foaming body for completing to obtain after foaming is taken out and keeps it completely cooling at room temperature;
C, foaming body after cooling is placed within baking oven;It is warming up to 99 DEG C in 0.8h, keeps the temperature 1.25h;126 DEG C of heat preservations 1.26h;156 DEG C of heat preservation 1.9h;179 heat preservation 1.6h;192 DEG C of heat preservation 2.2h are up to product.

Claims (5)

1. a kind of permeability organosilicon material, it is characterised in that: including following raw materials in parts by weight:
80-100 parts of hydroxy silicon oil
5-10 parts of vinyl silicone oil
15-20 parts of containing hydrogen silicone oil
3-5 parts of dibutyl tin dilaurate
3-5 parts of quaternary ammonium base
10-15 parts of fume colloidal silica
5-10 parts of nanometer calcium carbonate.
2. a kind of permeability organosilicon material according to claim 1, it is characterised in that: the viscosity of the hydroxy silicon oil is O.015-0.20Pa·s。
3. a kind of permeability organosilicon material according to claim 1, it is characterised in that: the viscosity of the vinyl silicone oil is 0.5-1.0Pas, contents of ethylene >=9%.
4. a kind of permeability organosilicon material according to claim 1, it is characterised in that: the reactive hydrogen matter of the containing hydrogen silicone oil Measure score >=1.6%.
5. a kind of preparation method of permeability organosilicon material according to claim 1, it is characterised in that: including following technique Step:
A, have in electric stirring, feed opening and condensation pipe reactor in one and hydroxy silicon oil is added according to recipe requirements;Addition is urged Agent dibutyl tin dilaurate, the pre-polymerization 1.5-2.0h at 130-150 DEG C obtain pre- silicone oil, spare;
B, the pre- silicone oil for obtaining step A mixes simultaneously with vinyl silicone oil, fume colloidal silica and nanometer calcium carbonate, quaternary ammonium base It stirs evenly;Containing hydrogen silicone oil is added, reaction system is warming up to 170-175 DEG C after mixing evenly, makes reaction system in normal pressure item It independently foams under part;The foaming body for completing to obtain after foaming is taken out and keeps it completely cooling at room temperature;
C, foaming body after cooling is placed within baking oven;It is warming up to 95-100 DEG C in 0.5-1.0h, keeps the temperature 1-2h;125- 130 DEG C of heat preservation 1-2h;155-160 DEG C of heat preservation 1-2h;170-180 DEG C of heat preservation 1-2h;190-200 DEG C of heat preservation 2-3h is up to product.
CN201710985460.8A 2017-10-20 2017-10-20 A kind of permeability organosilicon material and preparation method thereof Pending CN109694577A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110819116A (en) * 2019-11-28 2020-02-21 广东聚航新材料研究院有限公司 Novel organic silicon rubber foam material and preparation method thereof
CN111675910A (en) * 2020-06-23 2020-09-18 哈尔滨工程大学 Preparation method and product of flame-retardant organic silicon foam material
CN112574567A (en) * 2020-12-14 2021-03-30 漳州普瑞邦节能科技有限公司 High-strength organic silicon foam plastic and preparation method thereof
CN114085531A (en) * 2021-11-30 2022-02-25 江西伟普科技有限公司 High-flame-retardant organic silicon foam material and preparation method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101280112A (en) * 2008-05-16 2008-10-08 卢儒 Foamed silastic
CN106633902A (en) * 2016-10-20 2017-05-10 中蓝晨光化工研究设计院有限公司 Foaming organic silicon material and preparation method thereof

Patent Citations (2)

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Publication number Priority date Publication date Assignee Title
CN101280112A (en) * 2008-05-16 2008-10-08 卢儒 Foamed silastic
CN106633902A (en) * 2016-10-20 2017-05-10 中蓝晨光化工研究设计院有限公司 Foaming organic silicon material and preparation method thereof

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110819116A (en) * 2019-11-28 2020-02-21 广东聚航新材料研究院有限公司 Novel organic silicon rubber foam material and preparation method thereof
CN111675910A (en) * 2020-06-23 2020-09-18 哈尔滨工程大学 Preparation method and product of flame-retardant organic silicon foam material
CN112574567A (en) * 2020-12-14 2021-03-30 漳州普瑞邦节能科技有限公司 High-strength organic silicon foam plastic and preparation method thereof
CN114085531A (en) * 2021-11-30 2022-02-25 江西伟普科技有限公司 High-flame-retardant organic silicon foam material and preparation method thereof

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Application publication date: 20190430