CN102304282B - Flame-retardant silicone rubber and preparation method thereof - Google Patents
Flame-retardant silicone rubber and preparation method thereof Download PDFInfo
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- CN102304282B CN102304282B CN 201110009695 CN201110009695A CN102304282B CN 102304282 B CN102304282 B CN 102304282B CN 201110009695 CN201110009695 CN 201110009695 CN 201110009695 A CN201110009695 A CN 201110009695A CN 102304282 B CN102304282 B CN 102304282B
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Abstract
The invention discloses flame-retardant silicone rubber, which consists of polyether diols, isocyanate, an aminosilane crosslinking agent and a flame retardant in a certain ratio. A preparation method for the flame-retardant silicone rubber comprises the following steps of: performing heat treatment on the polyether diols in vacuum for 30 to 60 minutes, exhausting, adding the isocyanate, performing chemical reaction for 60 to 180 minutes; adding the aminosilane crosslinking agent, and continuously reacting for 30 to 60 minutes; and adding the flame retardant, fully dispersing, and dehydrating and extracting. The flame-retardant silicone rubber can be cured at room temperature without being heated, has the advantages of convenience for use, no smell or toxicity, oxidation ageing resistance, light ageing resistance, high temperature and severe cold resistance and the like, has good elasticity, strength, electric insulativity and excellent flame retardancy, and can be widely applied to the fields with high flame-retardant requirements, such as construction joint stopping, cable hole sealing, oil and gas pipeline plugging, telecommunication base stations, steel industry and the like.
Description
Technical field
The present invention relates to a kind of silicone rubber and preparation method thereof, specifically, relate to a kind of fire-proof silicone rubber and preparation method thereof, belong to building material technical field.
Background technology
In numerous synthetic rubber, silicone rubber is outstanding person wherein, and it has tasteless nontoxic, is not afraid of high temperature and the characteristics of resisting severe cold, and " keeping cool ", " remaining calm " when 300 degree Celsius and subzero 90 are spent are not still lost original intensity and elasticity.Silicone rubber also has good electrical insulating property, oxytolerant resistance to deterioration, fast light resistance to deterioration and mildew resistance, chemical stability etc., can be widely used in building the fields such as gap plugging, plugging cable hole, oil and gas pipes shutoff, telecomm base station, steel industry.But existing silicone rubber flame retardant properties is not good enough, is not suitable for the higher field of fire protection requirement.
Summary of the invention
The purpose of this invention is to provide a kind of fire-proof silicone rubber and preparation method thereof, to overcome the existing defects of prior art and deficiency, satisfy the demand of existing market.
For achieving the above object, the technical solution used in the present invention is as follows:
Fire-proof silicone rubber provided by the invention, its composition and composition and ratio are as follows:
Polyether Glycols 10～40 weight parts
Isocyanic ester 5～20 weight parts
Aminosilane linking agent 20～50 weight parts
Fire retardant 30～70 weight parts.
Described isocyanic ester is recommended as tolylene diisocyanate, diphenylmethanediisocyanate, hexa-methylene-1, any one or more than one the combination in the 6-vulcabond.
Described aminosilane linking agent is any one or more than one the combination in γ-aminopropyl triethoxysilane, phenylamino Union carbide A-162, γ-aminopropyltrimethoxysilane, the diaminoethyl aminopropyl trimethoxysilane.
Described fire retardant is recommended as any one or more than one the combination in ammonium polyphosphate, aluminium hydroxide, magnesium hydroxide, the zinc borate.
The preparation method of fire-proof silicone rubber of the present invention is as follows:
At first with the thermal treatment 30～60 minutes under vacuum of the polyether Glycols of 10～40 weight parts, the isocyanic ester that adds 5～20 weight parts after the venting carried out chemical reaction 60～180 minutes; The aminosilane linking agent that adds again 20～50 weight parts continues reaction 30～60 minutes; Then the fire retardant that adds 30～70 weight parts namely gets described fire-proof silicone rubber through the dehydration extraction after fully disperseing.
The thermal treatment temp of described polyether Glycols is 40～105 ℃, and vacuum tightness is-0.1～0.05MPa.
Compared with prior art, the present invention has following advantage:
1, fire-proof silicone rubber provided by the invention is at room temperature curable, need not heating, has advantage easy to use.
2, fire-proof silicone rubber provided by the invention have tasteless nontoxic, oxytolerant resistance to deterioration, fast light resistance to deterioration, high temperature resistance and severe cold, and have good elasticity, intensity and electrical insulating property.
3, fire-proof silicone rubber provided by the invention also has excellent flame retardant properties, and flame retardant rating reaches FV-0 level (GB/T 2408).
Embodiment
Below in conjunction with embodiment the present invention is done further detailed, complete explanation, but the present invention is not limited in following embodiment.
Embodiment 1
At first with the polyether Glycols of 10 weight parts-0.005MPa, 65 ℃ of lower pre-treatment 30 minutes, the tolylene diisocyanate that adds 10 weight parts after the venting carried out chemical reaction 100 minutes; The phenylamino Union carbide A-162 that adds again 20 weight parts continues reaction 60 minutes; Then the magnesium hydroxide that adds 50 weight parts namely gets described fire-proof silicone rubber through the dehydration extraction after fully disperseing.
Embodiment 2
At first with the polyether Glycols of 20 weight parts-0.1Mpa, 45 ℃ of lower pre-treatment 40 minutes, the diphenylmethanediisocyanate that adds 5 weight parts after the venting carried out chemical reaction 120 minutes; The diaminoethyl aminopropyl trimethoxysilane that adds again 30 weight parts continues reaction 120 minutes; Then the ammonium polyphosphate that adds 60 weight parts namely gets described fire-proof silicone rubber through the dehydration extraction after fully disperseing.
Embodiment 3
At first with the polyether Glycols of 30 weight parts 0.05Mpa, 105 ℃ of lower pre-treatment 50 minutes, add the hexa-methylene-1 of 15 weight parts after the venting, the 6-vulcabond carried out chemical reaction 180 minutes; The γ-aminopropyltrimethoxysilane that adds again 40 weight parts continues reaction 110 minutes; Then the aluminium hydroxide that adds 30 weight parts namely gets described fire-proof silicone rubber through the dehydration extraction after fully disperseing.
Embodiment 4
At first with the polyethersiloxanediol of 40 weight parts-0.07Mpa, 60 ℃ of lower pre-treatment 60 minutes, add the hexa-methylene-1 of 20 weight parts after the venting, the 6-vulcabond carried out chemical reaction 130 minutes; The γ-aminopropyl triethoxysilane that adds again 40 weight parts continues reaction 140 minutes; Then the zinc borate that adds 70 weight parts namely gets described fire-proof silicone rubber through the dehydration extraction after fully disperseing.
Embodiment 5
At first with the polyether glycol of 15 weight parts-0.08Mpa, 50 ℃ of lower pre-treatment 45 minutes, the tolylene diisocyanate that adds 12 weight parts after the venting carried out chemical reaction 140 minutes; The phenylamino Union carbide A-162 that adds again 50 weight parts continues reaction 160 minutes; Then add the magnesium hydroxide of 45 weight parts and the ammonium polyphosphate of 15 weight parts, namely get described fire-proof silicone rubber through the dehydration extraction after fully disperseing.
Embodiment 6
At first with the polyether Glycols of 25 weight parts 0.01MPa, 85 ℃ of lower pre-treatment 35 minutes, the diphenylmethanediisocyanate that adds 6 weight parts after the venting carried out chemical reaction 110 minutes; The γ-aminopropyl triethoxysilane that adds again 40 weight parts continues reaction 100 minutes; Then the zinc borate that adds 40 weight parts namely gets described fire-proof silicone rubber through the dehydration extraction after fully disperseing.
Embodiment 7
At first with the polyether Glycols of 35 weight parts-0.03pa, 70 ℃ of lower pre-treatment 30 minutes, add the hexa-methylene-1 of 8 weight parts after the venting, the 6-vulcabond carried out chemical reaction 60 minutes; The diaminoethyl aminopropyl trimethoxysilane that adds again 30 weight parts continues reaction 180 minutes; Then the ammonium polyphosphate that adds 30 weight parts namely gets described fire-proof silicone rubber through the dehydration extraction after fully disperseing.
Fire-proof silicone rubber of the present invention is shown in Table 1 by the performance test results that GB/T5574-2008 and GB/T2408-1996 carry out.
The performance test results of table 1 fire-proof silicone rubber of the present invention
| Test item | Test result | Test item | Test result |
| Outward appearance | The black Hookean body | Thermal conductivity (J/msK) | 5.1×10 -4 |
| Proportion (g/cm 3) | 1.40 | Volume resistivity (Ω cm) | 3.4×10 13 |
| Hardness (Shao Shi A) | 40 | Shearing resistance (MPa) | 0.49 |
| Elongation at break (%) | 200 | Combustionproperty | Meet the FV-0 rank |
By the performance test results of table 1 as seen: fire-proof silicone rubber proportion provided by the invention is lighter, have favorable elasticity and, heat insulation, insulation and flame retardant properties, can be widely used in building the higher fields of fire protection requirement such as gap plugging, plugging cable hole, oil and gas pipes shutoff, telecomm base station, steel industry.
Claims (7)
1. the preparation method of a fire-proof silicone rubber is characterized in that :-0.005MPa, 65 ℃ of lower pre-treatment 30 minutes, the tolylene diisocyanate that adds 10 weight parts after the venting carried out chemical reaction 100 minutes with the polyether Glycols of 10 weight parts; The phenylamino Union carbide A-162 that adds again 20 weight parts continues reaction 60 minutes; Then the magnesium hydroxide that adds 50 weight parts namely gets described fire-proof silicone rubber through the dehydration extraction after fully disperseing.
2. the preparation method of a fire-proof silicone rubber is characterized in that :-0.1Mpa, 45 ℃ of lower pre-treatment 40 minutes, the diphenylmethanediisocyanate that adds 5 weight parts after the venting carried out chemical reaction 120 minutes with the polyether Glycols of 20 weight parts; The diaminoethyl aminopropyl trimethoxysilane that adds again 30 weight parts continues reaction 120 minutes; Then the ammonium polyphosphate that adds 60 weight parts namely gets described fire-proof silicone rubber through the dehydration extraction after fully disperseing.
3. the preparation method of a fire-proof silicone rubber is characterized in that: the polyether Glycols of 30 weight parts 0.05Mpa, 105 ℃ of lower pre-treatment 50 minutes, is added the hexa-methylene-1 of 15 weight parts after the venting, the 6-vulcabond carried out chemical reaction 180 minutes; The γ-aminopropyltrimethoxysilane that adds again 40 weight parts continues reaction 110 minutes; Then the aluminium hydroxide that adds 30 weight parts namely gets described fire-proof silicone rubber through the dehydration extraction after fully disperseing.
4. the preparation method of a fire-proof silicone rubber, it is characterized in that: with the polyethersiloxanediol of 40 weight parts-0.07Mpa, 60 ℃ of lower pre-treatment 60 minutes, add the hexa-methylene-1 of 20 weight parts after the venting, the 6-vulcabond carried out chemical reaction 130 minutes; The γ-aminopropyl triethoxysilane that adds again 40 weight parts continues reaction 140 minutes; Then the zinc borate that adds 70 weight parts namely gets described fire-proof silicone rubber through the dehydration extraction after fully disperseing.
5. the preparation method of a fire-proof silicone rubber is characterized in that :-0.08Mpa, 50 ℃ of lower pre-treatment 45 minutes, the tolylene diisocyanate that adds 12 weight parts after the venting carried out chemical reaction 140 minutes with the polyether glycol of 15 weight parts; The phenylamino Union carbide A-162 that adds again 50 weight parts continues reaction 160 minutes; Then add the magnesium hydroxide of 45 weight parts and the ammonium polyphosphate of 15 weight parts, namely get described fire-proof silicone rubber through the dehydration extraction after fully disperseing.
6. the preparation method of a fire-proof silicone rubber is characterized in that: 0.01MPa, 85 ℃ of lower pre-treatment 35 minutes, the diphenylmethanediisocyanate that adds 6 weight parts after the venting carried out chemical reaction 110 minutes with the polyether Glycols of 25 weight parts; The γ-aminopropyl triethoxysilane that adds again 40 weight parts continues reaction 100 minutes; Then the zinc borate that adds 40 weight parts namely gets described fire-proof silicone rubber through the dehydration extraction after fully disperseing.
7. the preparation method of a fire-proof silicone rubber is characterized in that: the polyether Glycols of 35 weight parts-0.03pa, 70 ℃ of lower pre-treatment 30 minutes, is added the hexa-methylene-1 of 8 weight parts after the venting, the 6-vulcabond carried out chemical reaction 60 minutes; The diaminoethyl aminopropyl trimethoxysilane that adds again 30 weight parts continues reaction 180 minutes; Then the ammonium polyphosphate that adds 30 weight parts namely gets described fire-proof silicone rubber through the dehydration extraction after fully disperseing.
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| CN102181148A (en) * | 2011-01-27 | 2011-09-14 | 海龙核材科技（江苏）有限公司 | Fire-proof silicone rubber and preparation method thereof |
| CN105175685A (en) * | 2015-08-27 | 2015-12-23 | 江苏海龙核科技股份有限公司 | Modified silicone rubber and preparation process therefor |
| CN106243734A (en) * | 2016-07-28 | 2016-12-21 | 江苏昌悦重工科技有限公司 | A kind of Defend salt fog container |
| CN108047725A (en) * | 2017-12-11 | 2018-05-18 | 江苏海龙核科技股份有限公司 | A kind of nuclear power fire-proof silicone rubber and preparation method thereof |
| CN113527886A (en) * | 2021-06-08 | 2021-10-22 | 江苏海龙核科技股份有限公司 | Nuclear-grade dense electrical hole plugging material and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6750309B1 (en) * | 2002-05-17 | 2004-06-15 | Henkel Corporation | Methacrylated polyurethane copolymers with silicone segments containing alkoxysilyl groups |
| CN101245145A (en) * | 2008-03-25 | 2008-08-20 | 张广强 | Modified silicone rubber and preparation technique |
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| US8193293B2 (en) * | 2008-03-17 | 2012-06-05 | Ppg Industries Ohio, Inc. | Low temperature curable coating compositions and related methods |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6750309B1 (en) * | 2002-05-17 | 2004-06-15 | Henkel Corporation | Methacrylated polyurethane copolymers with silicone segments containing alkoxysilyl groups |
| CN101245145A (en) * | 2008-03-25 | 2008-08-20 | 张广强 | Modified silicone rubber and preparation technique |
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Denomination of invention: Fire-proof silicone rubber and preparation method thereof Effective date of registration: 20131126 Granted publication date: 20130109 Pledgee: Jiangsu Zhenjiang Rural Commercial Bank branch Dingmao Limited by Share Ltd Pledgor: Hailong nuclear material technology (Jiangsu) Co., Ltd. Registration number: 2013990000900 |
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Address after: Jian Xin Lu 212009 Zhenjiang province Jiangsu City Jingkou Industrial Park No. 36 Patentee after: JIANGSU ENTC NUCLEAR TECHNOLOGY JOINT STOCK CO., LTD. Address before: 212009 Zhenjiang City, Jiangsu Province Economic Development Zone eight road No. 17 Patentee before: Hailong nuclear material technology (Jiangsu) Co., Ltd. |