CN108047725A - A kind of nuclear power fire-proof silicone rubber and preparation method thereof - Google Patents

A kind of nuclear power fire-proof silicone rubber and preparation method thereof Download PDF

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Publication number
CN108047725A
CN108047725A CN201711303245.1A CN201711303245A CN108047725A CN 108047725 A CN108047725 A CN 108047725A CN 201711303245 A CN201711303245 A CN 201711303245A CN 108047725 A CN108047725 A CN 108047725A
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China
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component
parts
nuclear power
silicone rubber
preparation
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CN201711303245.1A
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Chinese (zh)
Inventor
严玉
邓晓阳
黄阁
兰才胜
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JIANGSU ENTC NUCLEAR TECHNOLOGY JOINT STOCK Co Ltd
China Nuclear Power Engineering Co Ltd
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JIANGSU ENTC NUCLEAR TECHNOLOGY JOINT STOCK Co Ltd
China Nuclear Power Engineering Co Ltd
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Priority to CN201711303245.1A priority Critical patent/CN108047725A/en
Publication of CN108047725A publication Critical patent/CN108047725A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions 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; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/322Ammonium phosphate
    • C08K2003/323Ammonium polyphosphate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

A kind of nuclear power fire-proof silicone rubber of the present invention, a kind of nuclear power fire-proof silicone rubber, by 1: 1 mixing by volume of A, B component, cure in 15~40 DEG C, the component A ingredient is made of dihydroxy sealing end dimethyl silicone polymer, polyether diols, isocyanates, tin catalyst, precipitated silica, ammonium polyphosphate;The B component ingredient is made of ethenyl blocking dimethyl silicone polymer, organic siliconresin, containing hydrogen silicone oil, hydroxy silicon oil, glycerin monostearate, chlorinated paraffin, mixed fillers.Silicone rubber produced by the present invention is tasteless nontoxic, has good electrical insulating property, oxytolerant ageing resistance, fast light ageing resistance.

Description

A kind of nuclear power fire-proof silicone rubber and preparation method thereof
Technical field
The present invention relates to a kind of nuclear power fire-proof silicone rubbers and preparation method thereof.
Background technology
The purpose of nuclear power plant's fire-proof curtain is that, around a certain space passive border of offer, this barrier should have the ability to bear With contain estimated fire and do not allow this fire spread to the non-fire side of fire-proof curtain material or items or do not make these Direct or indirect damage occurs for material and items, and requires fulfiling for these functions that can be acted in no any fire extinguishing system Under conditions of complete.Fireproof blocking be using fire-proof sealing material to being spaced apart mouth, perforated holes, building gap etc. are sealed and Filling makes it cooperate in defined fire resistance period with respective members, to prevent heat, flame and fire and smoke spread diffusion A kind of technical measures.
The commonly used fire-proof sealing material of nuclear power plant has inorganic fire-proof cement, silicone foam and silicone rubber.Inorganic fire Although cement was once widely used because cheap, due to high strength after curing so that is applied when replacing or increasing penetration piece Work is inconvenient and easily damages penetration piece, and quality is also not sufficiently stable, thus at present in the nuclear power of the nuclear powers big country such as the U.S., France It is not used already in factory, domestic nuclear power grassroot project also has the trend for abandoning this material.Based on this, silicone material, which becomes, works as The optimal selection of preceding nuclear power plant's hole fireproof blocking.
The content of the invention
The present invention proposes a kind of nuclear power fire-proof silicone rubber and preparation method thereof regarding to the issue above.
Specific technical solution is as follows:
A kind of nuclear power fire-proof silicone rubber by 1: 1 mixing by volume of A, B component, cures in 15~40 DEG C, special Sign is,
The component A ingredient is counted as follows in parts by weight:
Dihydroxy blocks 15~25 parts of dimethyl silicone polymer
12~16 parts of polyether diols
10~12 parts of isocyanates
0.1~1 part of tin catalyst
10~35 parts of precipitated silica
5~25 parts of ammonium polyphosphate
The B component ingredient is counted as follows in parts by weight:
40~55 parts of ethenyl blocking dimethyl silicone polymer
10~15 parts of organic siliconresin
10~20 parts of containing hydrogen silicone oil
3~12 parts of hydroxy silicon oil
3~5 parts of glycerin monostearate
1~3.5 part of chlorinated paraffin
5~30 parts of mixed fillers.
Further, the dihydroxy sealing end dimethyl silicone polymer viscosity is 10000~15000mPa.
Further, the ethenyl blocking dimethyl silicone polymer viscosity is 1000~5000mPa.
Further, the mixed fillers in the A, B component are gas-phase silica, wollastonite in powder and silicon powder with 2:3:4 The mixture that mixes of mass ratio.
Further, for the range of viscosities of the containing hydrogen silicone oil in 20~40cp, hydrogen content is 1.0~2.5%.
A kind of preparation method of nuclear power fire-proof silicone rubber, which is characterized in that include the following steps:
A) mixed fillers are prepared, by gas-phase silica, wollastonite in powder and silicon powder with 2:3:4 mass ratio mixing, incorporation time 10-30min obtains mixed fillers after mixing;
B) each constitutive material is weighed according to the compositing formula of component A and B component respectively;
C) dihydroxy sealing end dimethyl silicone polymer and the polyether diols in component A are added in reaction kettle, 20~70 DEG C, 10~30min is mixed under vacuum degree (- 0.1~-0.05MPa), then isocyanates, tin catalysis are added in into solution mixed above Agent, precipitated silica are stirred 30~60min with high-speed emulsifying machine, add ammonium polyphosphate and are stirred, vacuum outgas 10~20min;It is filling with the filtering net pressure filter of 120 mesh, component A is made;
D) ethenyl blocking dimethyl silicone polymer, organic siliconresin, hydroxy silicon oil and the containing hydrogen silicone oil in B component are added in anti- It answers in kettle, 10~30min is stirred at 20~70 DEG C, then glycerin monostearate, chlorinated paraffin are added in into solution mixed above And mixed fillers, 30~60min is stirred with high-speed emulsifying machine, then 30~60min of vacuum outgas;With the strainer of 150 mesh Press filtration, it is filling, B component is made;
E) by 1: 1 mixing by volume of the component A of preparation and B component, cure in 15~40 DEG C to get finished product.
Beneficial effects of the present invention are:
1st, preparation process is simple, easy for construction, is readily disassembled replacement;
2nd, density is big, high mechanical strength, and radiation resistance is good;
3rd, it is tasteless nontoxic, there is good electrical insulating property, oxytolerant ageing resistance, fast light ageing resistance;
4th, flame retardant property is good, and fire retardant performance reaches the FV-0 ranks of GB/T2408-1996;
5th, the products application after the present invention cures is lasting, resistant to damage, the easy decontamination in surface.
Specific embodiment
For technical scheme is made to become apparent from clearly, below the present invention is described further, it is any to this The technical characteristic of inventive technique scheme carries out the scheme that equivalencing is drawn with conventional reasoning and each falls within the scope of the present invention.
Embodiment 1
A kind of preparation method of nuclear power fire-proof silicone rubber, which is characterized in that include the following steps:
A) mixed fillers are prepared, by gas-phase silica, wollastonite in powder and silicon powder with 2:3:4 mass ratio mixing, incorporation time 10min obtains mixed fillers after mixing;
B) each constitutive material is weighed according to the compositing formula of component A and B component respectively;
C) 15 parts of dihydroxy sealing end dimethyl silicone polymer in component A and 12 parts of polyether diols are added in reaction kettle, 20 DEG C, 10min is mixed under vacuum degree (- 0.1MPa), then add in 10 parts of isocyanates into solution mixed above, 0.1 part of tin is urged Agent, 10 parts of precipitated silicas, 30min is stirred with high-speed emulsifying machine, is added 5 parts of ammonium polyphosphate and is stirred, very Sky degassing 10min;It is filling with the filtering net pressure filter of 120 mesh, component A is made;
D) by 40 parts of ethenyl blocking dimethyl silicone polymers, 10 parts of organic siliconresins, the 3 parts of hydroxy silicon oils and 10 in B component Part containing hydrogen silicone oil is added in reaction kettle, and 10min are stirred at 20 DEG C, then 3 parts of glycerol monostearates are added in into solution mixed above Ester, 1 part of chlorinated paraffin and 5 parts of mixed fillers, are stirred 30min, then vacuum outgas 30min with high-speed emulsifying machine;With The filtering net pressure filter of 150 mesh, it is filling, B component is made;
E) by 1: 1 mixing by volume of the component A of preparation and B component, cure in 15 DEG C to get finished product.
Embodiment 2
A kind of preparation method of nuclear power fire-proof silicone rubber, which is characterized in that include the following steps:
A) mixed fillers are prepared, by gas-phase silica, wollastonite in powder and silicon powder with 2:3:4 mass ratio mixing, incorporation time 30min obtains mixed fillers after mixing;
B) each constitutive material is weighed according to the compositing formula of component A and B component respectively;
C) 25 parts of dihydroxy sealing end dimethyl silicone polymer in component A and 16 parts of polyether diols are added in reaction kettle, 70 DEG C, 30min is mixed under vacuum degree (- 0.05MPa), then 12 parts of isocyanates, 1 part of tin catalysis are added in into solution mixed above Agent, 35 parts of precipitated silicas, 60min is stirred with high-speed emulsifying machine, is added 25 parts of ammonium polyphosphate and is stirred, vacuum Deaerate 20min;It is filling with the filtering net pressure filter of 120 mesh, component A is made;
D) by 55 parts of ethenyl blocking dimethyl silicone polymers, 15 parts of organic siliconresins, the 12 parts of hydroxy silicon oils and 20 in B component Part containing hydrogen silicone oil is added in reaction kettle, and 30min are stirred at 70 DEG C, then 5 parts of glycerol monostearates are added in into solution mixed above Ester, 3.5 parts of chlorinated paraffins and 30 parts of mixed fillers, are stirred 60min, then vacuum outgas 60min with high-speed emulsifying machine; It is filling with the filtering net pressure filter of 150 mesh, B component is made;
E) by 1: 1 mixing by volume of the component A of preparation and B component, cure in 40 DEG C to get finished product.
Embodiment 3
A kind of preparation method of nuclear power fire-proof silicone rubber, which is characterized in that include the following steps:
A) mixed fillers are prepared, by gas-phase silica, wollastonite in powder and silicon powder with 2:3:4 mass ratio mixing, incorporation time 20min obtains mixed fillers after mixing;
B) each constitutive material is weighed according to the compositing formula of component A and B component respectively;
C) 20 parts of dihydroxy sealing end dimethyl silicone polymer in component A and 13 parts of polyether diols are added in reaction kettle, 40 DEG C, 20min is mixed under vacuum degree (- 0.06MPa), then add in 11 parts of isocyanates into solution mixed above, 0.6 part of tin is urged Agent, 22 parts of precipitated silicas, 40min is stirred with high-speed emulsifying machine, is added 15 parts of ammonium polyphosphate and is stirred, very Sky degassing 16min;It is filling with the filtering net pressure filter of 120 mesh, component A is made;
D) by 49 parts of ethenyl blocking dimethyl silicone polymers, 13 parts of organic siliconresins, the 8 parts of hydroxy silicon oils and 16 in B component Part containing hydrogen silicone oil is added in reaction kettle, and 20min are stirred at 50 DEG C, then 4 parts of glycerol monostearates are added in into solution mixed above Ester, 2.5 parts of chlorinated paraffins and 18 parts of mixed fillers, are stirred 40min, then vacuum outgas 40min with high-speed emulsifying machine;With The filtering net pressure filter of 150 mesh, it is filling, B component is made;
E) by 1: 1 mixing by volume of the component A of preparation and B component, cure in 30 DEG C to get finished product.
Beneficial effects of the present invention are:
1st, preparation process is simple, easy for construction, is readily disassembled replacement;
2nd, density is big, high mechanical strength, and radiation resistance is good;
3rd, it is tasteless nontoxic, there is good electrical insulating property, oxytolerant ageing resistance, fast light ageing resistance;
4th, flame retardant property is good, and fire retardant performance reaches the FV-0 ranks of GB/T2408-1996;
5th, the products application after the present invention cures is lasting, resistant to damage, the easy decontamination in surface.

Claims (6)

1. a kind of nuclear power fire-proof silicone rubber by 1: 1 mixing by volume of A, B component, cures in 15~40 DEG C, It is characterized in that,
The component A ingredient is counted as follows in parts by weight:
Dihydroxy blocks 15~25 parts of dimethyl silicone polymer
12~16 parts of polyether diols
10~12 parts of isocyanates
0.1~1 part of tin catalyst
10~35 parts of precipitated silica
5~25 parts of ammonium polyphosphate
The B component ingredient is counted as follows in parts by weight:
40~55 parts of ethenyl blocking dimethyl silicone polymer
10~15 parts of organic siliconresin
10~20 parts of containing hydrogen silicone oil
3~12 parts of hydroxy silicon oil
3~5 parts of glycerin monostearate
1~3.5 part of chlorinated paraffin
5~30 parts of mixed fillers.
2. a kind of nuclear power fire-proof silicone rubber as claimed in claim 1 and preparation method thereof, it is characterized in that, the dihydroxy sealing end Dimethyl silicone polymer viscosity is 10000~15000mPa.
3. a kind of nuclear power fire-proof silicone rubber as claimed in claim 1 and preparation method thereof, it is characterized in that, the ethenyl blocking Dimethyl silicone polymer viscosity is 1000~5000mPa.
4. a kind of nuclear power fire-proof silicone rubber as claimed in claim 1 and preparation method thereof, it is characterized in that, in the A, B component Mixed fillers for gas-phase silica, wollastonite in powder and silicon powder with 2:3:The mixture that 4 mass ratio mixes.
5. a kind of nuclear power fire-proof silicone rubber as claimed in claim 1 and preparation method thereof, it is characterized in that, the containing hydrogen silicone oil For range of viscosities in 20~40cp, hydrogen content is 1.0~2.5%.
6. a kind of preparation method of nuclear power fire-proof silicone rubber, which is characterized in that include the following steps:
A) mixed fillers are prepared, by gas-phase silica, wollastonite in powder and silicon powder with 2:3:4 mass ratio mixing, incorporation time 10-30min obtains mixed fillers after mixing;
B) each constitutive material is weighed according to the compositing formula of component A and B component respectively;
C) dihydroxy sealing end dimethyl silicone polymer and the polyether diols in component A are added in reaction kettle, 20~70 DEG C, 10~30min is mixed under vacuum degree (- 0.1~-0.05MPa), then isocyanates, tin catalysis are added in into solution mixed above Agent, precipitated silica are stirred 30~60min with high-speed emulsifying machine, add ammonium polyphosphate and are stirred, vacuum outgas 10~20min;It is filling with the filtering net pressure filter of 120 mesh, component A is made;
D) ethenyl blocking dimethyl silicone polymer, organic siliconresin, hydroxy silicon oil and the containing hydrogen silicone oil in B component are added in anti- It answers in kettle, 10~30min is stirred at 20~70 DEG C, then glycerin monostearate, chlorinated paraffin are added in into solution mixed above And mixed fillers, 30~60min is stirred with high-speed emulsifying machine, then 30~60min of vacuum outgas;With the strainer of 150 mesh Press filtration, it is filling, B component is made;
E) by 1: 1 mixing by volume of the component A of preparation and B component, cure in 15~40 DEG C to get finished product.
CN201711303245.1A 2017-12-11 2017-12-11 A kind of nuclear power fire-proof silicone rubber and preparation method thereof Pending CN108047725A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109628044A (en) * 2018-12-06 2019-04-16 成都硅宝科技股份有限公司 A kind of environmental protection dual-component silicane modified polyether glue 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 (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102304282A (en) * 2011-01-17 2012-01-04 海龙核材科技(江苏)有限公司 Flame-retardant silicone rubber and preparation method thereof
CN102504545A (en) * 2011-12-02 2012-06-20 海龙核材科技(江苏)有限公司 High-density fire-proof silicone rubber and preparation method thereof
CN102504544A (en) * 2011-12-02 2012-06-20 海龙核材科技(江苏)有限公司 Biological shielding type liquid silicone rubber and preparation method thereof
CN103665891A (en) * 2013-12-10 2014-03-26 海龙核材科技(江苏)有限公司 Double-component fireproof silicone foamed material with ultra-low density and preparation technology thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102304282A (en) * 2011-01-17 2012-01-04 海龙核材科技(江苏)有限公司 Flame-retardant silicone rubber and preparation method thereof
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
CN102504545A (en) * 2011-12-02 2012-06-20 海龙核材科技(江苏)有限公司 High-density fire-proof silicone rubber and preparation method thereof
CN102504544A (en) * 2011-12-02 2012-06-20 海龙核材科技(江苏)有限公司 Biological shielding type liquid silicone rubber and preparation method thereof
CN103665891A (en) * 2013-12-10 2014-03-26 海龙核材科技(江苏)有限公司 Double-component fireproof silicone foamed material with ultra-low density and preparation technology thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109628044A (en) * 2018-12-06 2019-04-16 成都硅宝科技股份有限公司 A kind of environmental protection dual-component silicane modified polyether glue 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

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Application publication date: 20180518