CN108148545A - The production method of Halogen high-performance refractory silicone sealant - Google Patents

The production method of Halogen high-performance refractory silicone sealant Download PDF

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Publication number
CN108148545A
CN108148545A CN201611106034.4A CN201611106034A CN108148545A CN 108148545 A CN108148545 A CN 108148545A CN 201611106034 A CN201611106034 A CN 201611106034A CN 108148545 A CN108148545 A CN 108148545A
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China
Prior art keywords
parts
silicone sealant
methyl
performance refractory
silicone
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CN201611106034.4A
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Chinese (zh)
Inventor
蒋进生
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Weihai Cheng Jing Technology Co Ltd
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Weihai Cheng Jing Technology Co Ltd
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Priority to CN201611106034.4A priority Critical patent/CN108148545A/en
Publication of CN108148545A publication Critical patent/CN108148545A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives 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
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • 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
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • 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
    • C08L2201/22Halogen free composition
    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

A kind of Halogen high-performance refractory silicone sealant, by according to the methyl silicone rubber at room temperature cure of weight proportion, aluminium hydroxide, fumed silica, methyl tributanoximo silane, vinyl tributyl ketoximyl silane, N(B ammonia second)Y aminopropyl front threes(Second)Oxysilane, γ-aminopropyl triethoxysilane, dibutyl tin laurate, mill base are mixed with, wherein methyl silicone rubber at room temperature cure is support raw material, fumed silica, aluminium hydroxide are filling raw material, and mill base is used to adjust the color of silicone adhesive, other are functional aid.Present invention is generally directed to current halogen system flame-proof silicone sealant not environmentally, and largely it is added to the mechanical property of the silicone sealant of inorganic combustion inhibitor and the present situation of application that displacement capacity is had a greatly reduced quality, a kind of production method of Halogen high-performance refractory silicone sealant is provided, meet modern architecture is needed with glue.

Description

The production method of Halogen high-performance refractory silicone sealant
Technical field
The present invention relates to the production methods of Halogen high-performance refractory silicone sealant, and in particular to a kind of one-component Halogen is high The production method of performance flame-proof silicone sealant.
Background technology
Building fire has the characteristics that sprawling is fast, evacuating personnel is difficult, difficulty of putting out a fire to save life and property is big, especially skyscraper, once Fire occurs, loss is often very heavy.The fire protecting performance of building is improved, it not only will be from raising outer wall material particularly exterior wall The fire protecting performance of thermal insulation material considers, also to put forth effort to improve the anti-flammability of the silicone sealant of building joint sealing.With generation The raising that various countries of boundary require building fire protection rank and the concern to curtain wall fire protecting performance, the flame retardant property of silicone sealant are modified Also become focus of attention in industry.All it is by adding in fire retardant in formula because silicone adhesive itself does not have flame retardant type Method realize the flame retardant effect of silicone adhesive.The fire retardant being widely adopted at present mainly has halogenated flame retardant, inorganic fire-retarded Synergistic fire retardant that agent, a variety of fire retardants are used in mixed way etc..Halogenated flame retardant flame retardant effect is good, but because halogen system is fire-retardant Smoke amount is big when agent is burnt, and discharges toxic, pollution gas, is unfavorable for health and environmental protection.Inorganic combustion inhibitor is mainly hydrogen-oxygen Change aluminium, magnesium hydroxide and metal oxide, this based flame retardant has the function of fire-retardant, smoke elimination, filling etc., and flue gas in combustion process It is less.But since the additive amount of inorganic combustion inhibitor is big, the mechanical property for be easy to causeing silicone adhesive is affected, easily so that glue Body embrittlement is hardened, so as to which the resist displacement ability of silicone adhesive be caused to decline.The present invention exists for halogen containing flame-retardant and inorganic combustion inhibitor Major drawbacks present in silicone adhesive application, provide a kind of production method of Halogen high-performance refractory silicone sealant.The hair It is bright using the aluminium hydroxide that surface modification treatment is crossed as fire retardant, controlled by the selection of crosslinking agent and dosage, not only ensured The feature of environmental protection of silicone adhesive burning, while make the mechanical property of silicone adhesive and the displacement capacity unaffected again, it is ensured that silicone adhesive The applicability of building fire protection function.
Invention content
The purpose of the present invention is in view of the above shortcomings of the prior art, provide a kind of Halogen high-performance refractory silicone seal The production method of glue, solve halogen system flame-proof silicone sealant not environmentally makes silicone adhesive power with common inorganic flame-proof silicone sealant Learn the main problem of performance impairment.The invention is strong with environmental protection, low cigarette, flame retardant property protrusion, colloid high resiliency, resist displacement ability The advantages that, it is ensured that the applicability of silicone adhesive building fire protection function.
The present invention can be achieved by the following measures:
A kind of production method of Halogen high-performance refractory silicone sealant, it is characterised in that the silicone sealant is pressed by materials described below It is prepared according to weight proportion:
750-800 parts of 20000 viscosity (25 DEG C, mpa.s) methyl silicone rubber at room temperature cure
50-70 parts of 80000 viscosity (25 DEG C, mpa.s) methyl silicone rubber at room temperature cure
600-650 parts of aluminium hydroxide
30-35 parts of fumed silica
40-45 parts of methyl tributanoximo silane
3-5 parts of vinyl tributyl ketoximyl silane
3-4 parts of methyl mixing ketoxime crosslinking agent
N-(B- ammonia second)- Y- aminopropyl front threes(Second)2-3 parts of oxysilane
γ -2-3 parts of aminopropyl triethoxysilane
0.3-0.5 parts of dibutyl tin laurate
35-45 parts of mill base
Production stage is as follows:
(1)2000L kneaders put into methyl silicone rubber at room temperature cure after starting, stirring is warming up to 50 DEG C of input aluminium hydroxides, stirs It mixes and is warming up to 80 DEG C of input fumed silicas, wait that continuing stirring is warming up to 135-150 DEG C, and 100 DEG C or more lasting works The industry time reaches 3 hours, vacuum dehydration under -0.09Mpa states, output when being less than 0.3% using moisture teller detection moisture value Base-material;
(2)SM405 three-roll grinders pass through step to being cooled to less than 50 DEG C(1)The base-material of output is ground, by two Secondary grinding, it is that 9-9.3 uncles step on to measure fineness with Hegman grind gage, consistency is measured with paste paint putty consistency analyzer;
(3)Step will be passed through(2)The storage tank deaeration under base-material input vacuum state, storage after grinding, holding state of temperature are 45-50℃;
(4)By methyl tributanoximo silane, vinyl tributyl ketoximyl silane, N-(B- ammonia second)- Y- aminopropyl front threes(Second) Oxysilane, γ-aminopropyl triethoxysilane, dibutyl tin laurate are stored in after the inferior weight of normal temperature state prepares It is for use in auxiliary tank;
(5)By step(3)The base-material of middle storage, step(4)The mixed aid of middle storage and mill base by synchronous valve control simultaneously, Enter after the reaction of JTH-3K static mixers with weight ratio and the closed storage of storage tank is inputted by pipeline;
(6)Through step(5)Finished product rubber cement after reaction inputs the condenser cooling temperature of 7 DEG C of ice water state of temperatures to 30-35 DEG C, It is dispensed by ZDG-300 hard tube automatic filling machines.
Above-mentioned fumed silica specific surface area is T200.
Above-mentioned aluminium hydroxide has been subjected to surface modification treatment.
Production process of the present invention operation under totally-enclosed state, rubber cement is without gel, skinning.
The present invention provides a kind of production methods of Halogen high-performance refractory silicone sealant, solve halogen system flame-proof silicone Fluid sealant not environmentally makes the main problem that silicone adhesive mechanical property is damaged with common inorganic flame-proof silicone sealant, which has The advantages that environmentally friendly, low cigarette, flame retardant property protrusion, colloid high resiliency, strong resist displacement ability, it is ensured that silicone adhesive building fire protection function Applicability.
Specific implementation method
A kind of production method of Halogen high-performance refractory silicone sealant, it is characterised in that the silicone sealant is pressed by materials described below It is prepared according to weight proportion:
750-800 parts of 20000 viscosity (25 DEG C, mpa.s) methyl silicone rubber at room temperature cure
50-70 parts of 80000 viscosity (25 DEG C, mpa.s) methyl silicone rubber at room temperature cure
600-650 parts of aluminium hydroxide
30-35 parts of fumed silica
40-45 parts of methyl tributanoximo silane
3-5 parts of vinyl tributyl ketoximyl silane
3-4 parts of methyl mixing ketoxime crosslinking agent
N-(B- ammonia second)- Y- aminopropyl front threes(Second)2-3 parts of oxysilane
γ -2-3 parts of aminopropyl triethoxysilane
0.3-0.5 parts of dibutyl tin laurate
35-45 parts of mill base.
Production stage is as follows:
(1)2000L kneaders put into methyl silicone rubber at room temperature cure after starting, stirring is warming up to 50 DEG C of input aluminium hydroxides, stirs It mixes and is warming up to 80 DEG C of input fumed silicas, wait that continuing stirring is warming up to 135-150 DEG C, and 100 DEG C or more lasting works The industry time reaches 3 hours, vacuum dehydration under -0.09Mpa states.Output when being less than 0.3% using moisture teller detection moisture value Base-material;
(2)SM405 three-roll grinders pass through step to being cooled to less than 50 DEG C(1)The base-material of output is ground, by two Secondary grinding, it is that 9-9.3 uncles step on to measure fineness with Hegman grind gage, consistency is measured with paste paint putty consistency analyzer;
(3)Step will be passed through(2)The storage tank deaeration under base-material input vacuum state, storage after grinding, holding state of temperature are 45-50℃;
(4)By methyl tributanoximo silane, vinyl tributyl ketoximyl silane, N-(B- ammonia second)- Y- aminopropyl front threes(Second) Oxysilane, γ-aminopropyl triethoxysilane, dibutyl tin laurate are stored in after the inferior weight of normal temperature state prepares It is for use in auxiliary tank;
(5)By step(3)The base-material of middle storage, step(4)The mixed aid of middle storage and mill base by synchronous valve control simultaneously, Enter after the reaction of JTH-3K static mixers with weight ratio and the closed storage of storage tank is inputted by pipeline;
(6)Through step(5)Finished product rubber cement after reaction inputs the condenser cooling temperature of 7 DEG C of ice water state of temperatures to 30-35 DEG C, It is dispensed by ZDG-300 hard tube automatic filling machines.
The present invention provides a kind of production methods of Halogen high-performance refractory silicone sealant, solve halogen system flame-proof silicone Fluid sealant not environmentally makes the main problem that silicone adhesive mechanical property is damaged with common inorganic flame-proof silicone sealant.The invention has The advantages that environmentally friendly, low cigarette, flame retardant property protrusion, colloid high resiliency, strong resist displacement ability, it is ensured that silicone adhesive building fire protection function Applicability.

Claims (4)

1. a kind of production method of Halogen high-performance refractory silicone sealant, it is characterised in that the silicone sealant is by materials described below It is prepared according to weight proportion:
750-800 parts of 20000 viscosity (25 DEG C, mpa.s) methyl silicone rubber at room temperature cure
50-70 parts of 80000 viscosity (25 DEG C, mpa.s) methyl silicone rubber at room temperature cure
600-650 parts of aluminium hydroxide
30-35 parts of fumed silica
40-45 parts of methyl tributanoximo silane
3-5 parts of vinyl tributyl ketoximyl silane
3-4 parts of methyl mixing ketoxime crosslinking agent
N-(B- ammonia second)- Y- aminopropyl front threes(Second)2-3 parts of oxysilane
γ -2-3 parts of aminopropyl triethoxysilane
0.3-0.5 parts of dibutyl tin laurate
35-45 parts of mill base
The preparation method of the Halogen high-performance refractory silicone sealant is as follows:
(1)2000L kneaders put into methyl silicone rubber at room temperature cure after starting, stirring is warming up to 50 DEG C of input aluminium hydroxides, stirs It mixes and is warming up to 80 DEG C of input fumed silicas, wait that continuing stirring is warming up to 135-150 DEG C, and 100 DEG C or more lasting works The industry time reaches 3 hours, vacuum dehydration under -0.09Mpa states, output when being less than 0.3% using moisture teller detection moisture value Base-material;
(2)SM405 three-roll grinders pass through step to being cooled to less than 50 DEG C(1)The base-material of output is ground, by two Secondary grinding, it is that 9-9.3 uncles step on to measure fineness with Hegman grind gage, consistency is measured with paste paint putty consistency analyzer;
(3)Step will be passed through(2)The storage tank deaeration under base-material input vacuum state, storage after grinding, holding state of temperature are 45-50℃;
(4)By methyl tributanoximo silane, vinyl tributyl ketoximyl silane, N-(B- ammonia second)- Y- aminopropyl front threes(Second) Oxysilane, γ-aminopropyl triethoxysilane, dibutyl tin laurate are stored in after the inferior weight of normal temperature state prepares It is for use in auxiliary tank;
(5)By step(3)The base-material of middle storage, step(4)The mixed aid of middle storage and mill base by synchronous valve control simultaneously, Enter after the reaction of JTH-3K static mixers with weight ratio and the closed storage of storage tank is inputted by pipeline;
(6)Through step(5)Finished product rubber cement after reaction inputs the condenser cooling temperature of 7 DEG C of ice water state of temperatures to 30-35 DEG C, It is dispensed by ZDG-300 hard tube automatic filling machines.
2. Halogen high-performance refractory silicone sealant according to claim 1, it is characterised in that:Step(5), step(6) Operation under totally-enclosed state, rubber cement is without gel, skinning.
3. Halogen high-performance refractory silicone sealant according to claim 1, it is characterised in that:Fumed silica ratio Surface area is T200.
4. Halogen high-performance refractory silicone sealant according to claim 1, it is characterised in that:Aluminium hydroxide has been subjected to table Face modification.
CN201611106034.4A 2016-12-06 2016-12-06 The production method of Halogen high-performance refractory silicone sealant Pending CN108148545A (en)

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Application Number Priority Date Filing Date Title
CN201611106034.4A CN108148545A (en) 2016-12-06 2016-12-06 The production method of Halogen high-performance refractory silicone sealant

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111876124A (en) * 2020-08-26 2020-11-03 重庆天旗实业有限公司 Novel flame-retardant sealant and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103289636A (en) * 2013-05-30 2013-09-11 河南硅宝能源科技有限公司 Silicone weather-proof sealant and preparation method thereof
CN104232013A (en) * 2014-10-14 2014-12-24 泸州北方化学工业有限公司 Silicone sealant and preparation method thereof
CN105419721A (en) * 2015-12-15 2016-03-23 河南硅宝能源科技有限公司 Special flow type silicone sealant for road

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103289636A (en) * 2013-05-30 2013-09-11 河南硅宝能源科技有限公司 Silicone weather-proof sealant and preparation method thereof
CN104232013A (en) * 2014-10-14 2014-12-24 泸州北方化学工业有限公司 Silicone sealant and preparation method thereof
CN105419721A (en) * 2015-12-15 2016-03-23 河南硅宝能源科技有限公司 Special flow type silicone sealant for road

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111876124A (en) * 2020-08-26 2020-11-03 重庆天旗实业有限公司 Novel flame-retardant sealant and preparation method thereof

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Application publication date: 20180612

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