CN109694688A - A kind of appropriateness tough organosilicon sealant and preparation method thereof - Google Patents

A kind of appropriateness tough organosilicon sealant and preparation method thereof Download PDF

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Publication number
CN109694688A
CN109694688A CN201710986129.8A CN201710986129A CN109694688A CN 109694688 A CN109694688 A CN 109694688A CN 201710986129 A CN201710986129 A CN 201710986129A CN 109694688 A CN109694688 A CN 109694688A
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CN
China
Prior art keywords
parts
silane
organosilicon sealant
viscosity
tough
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Pending
Application number
CN201710986129.8A
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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 CN201710986129.8A priority Critical patent/CN109694688A/en
Publication of CN109694688A publication Critical patent/CN109694688A/en
Pending legal-status Critical Current

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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
    • C09J183/06—Polysiloxanes containing silicon bound to oxygen-containing groups
    • 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
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • 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
    • C09J11/08—Macromolecular additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • 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
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • 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
    • C08K3/24—Acids; Salts thereof
    • C08K3/26—Carbonates; Bicarbonates
    • C08K2003/265—Calcium, strontium or barium carbonate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • C08L2203/206—Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts
    • 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

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

Abstract

The present invention relates to a kind of appropriate tough organosilicon sealants and preparation method thereof, belong to organosilicon sealant technical field.The organosilicon sealant includes medium viscosity α, alpha, omega-dihydroxy polydimethyl siloxane, low viscosity α, alpha, omega-dihydroxy polydimethyl siloxane, dimethicone, two butanone oximino silane of dimethyl, polyethylene glycol, fumed titanium dioxide, nanometer grade calcium carbonate, methyl triacetoxysilane, ditert-butyldiacetyl oxygen-base silane, dioctyl tin cinnamic acid tin, stannous octoate, aminomethyl phenyl two (N- methylacetamido) silane.The organosilicon sealant is having the appropriate toughness in controlled range.

Description

A kind of appropriateness tough organosilicon sealant and preparation method thereof
Technical field
The present invention relates to a kind of sealants and preparation method thereof, it is more particularly related to which a kind of appropriateness toughness has Machine silicone sealant and preparation method thereof belongs to organosilicon sealant technical field.
Background technique
In the encapsulation of certain electronic products or other products, it is often required that organosilicon sealing material is with certain submissive While property, also require it with certain toughness, it is normal under some special environment conditions to meet the electronic product It uses.Has the mechanical property of certain modulus and high-elongation after solidifying this requires sealing material.Simultaneously, it is desirable that produced after solidification Product will have certain shape stability, deformation resistance.Therefore, such novel organosilicon sealing material becomes people's research hotspot.
State Intellectual Property Office discloses a Publication No. CN103756627A, entitled " resistance to storage in 2014.04.30 Deposit the fast cured silicone sealant of weather-proof dealcoholized type " invention, a kind of disclosure of the invention weather-proof dealcoholized type of shelf-stable solidifies fastly Organosilicon sealant, including following parts by weight of component: alkoxy end-capped α, 100 parts of alpha, omega-dihydroxy polydimethyl siloxane, plasticising 15~20 parts of agent, 15~18 parts of coupling agent of mixing, 100~120 parts of filler, 5~10 parts of precipitated silica, crosslinking agent 8 ~10 parts, 5~30 parts of function additive.The present invention passes through raw material using the alkoxy end-capped polysiloxanes prepared as polymer Reasonable selection and proportion, the alkoxy end-capped dealcoholized type organosilicon sealant prepared have curing rate fast, high mechanical strength, The advantages that good weatherability, long period of storage, faster curing rate and deeper cured thickness can effectively increase sizing The effective rate of utilization of working efficiency and sizing material.
Although above-mentioned organosilicon sealant curing rate is fast, so that work efficiency is high, cannot have certain modulus While with high-elongation, product has certain shape stability, deformation resistance after solidification.
Summary of the invention
Present invention seek to address that in the prior art organosilicon sealant the problem of, a kind of appropriate tough organosilicon sealing is provided Glue, the organosilicon sealant while having certain modulus and high-elongation, after solidification product have certain shape stability, Deformation resistance.
In order to achieve the above-mentioned object of the invention, specific technical solution is as follows:
A kind of appropriateness tough organosilicon sealant, it is characterised in that: including following raw materials in parts by weight:
Medium viscosity α, 65-70 parts of alpha, omega-dihydroxy polydimethyl siloxane
Low viscosity α, 30-35 parts of alpha, omega-dihydroxy polydimethyl siloxane
5-10 parts of dimethicone
5-10 parts of two butanone oximino silane of dimethyl
3-5 parts of polyethylene glycol
10-15 parts of fumed titanium dioxide
20-30 parts of nanometer grade calcium carbonate
5-10 parts of methyl triacetoxysilane
5-10 parts of ditert-butyldiacetyl oxygen-base silane
0.5-1.0 parts of dioctyl tin cinnamic acid tin
0.3-0.5 parts of stannous octoate
8-12 parts of silane of aminomethyl phenyl two (N- methylacetamido).
It is currently preferred, the medium viscosity α, viscosity >=50000mPas of alpha, omega-dihydroxy polydimethyl siloxane.
It is currently preferred, the low viscosity α, viscosity >=500mPas of alpha, omega-dihydroxy polydimethyl siloxane
A kind of preparation method of appropriateness tough organosilicon sealant, it is characterised in that: comprise the following steps that:
A, medium viscosity dialkyl polydimethylsiloxane, low viscosity dialkyl polydimethylsiloxane, dimethicone are weighed, is stirred It mixes uniformly mixed；In high speed agitator, 2h, vacuum dehydration are stirred；
B, fumed titanium dioxide, nanometer grade calcium carbonate, polyethylene glycol, methyl triacetoxysilane is added, continues to stir 1h, Vacuum dehydration；
C, ditert-butyldiacetyl oxygen-base silane, two butanone oximino silane of dimethyl is added, continues to stir 0.5-1.0h；It is added Aminomethyl phenyl two (N- methylacetamido) silane continues to stir 0.5-1.0h；Stannous octoate, dioctyl tin cinnamic acid is added Tin continues to stir 1h；1h is vacuumized, continues to be dehydrated；Discharging, packaging.
Bring advantageous effects of the present invention:
The present invention uses certain chain length chain extender, hands over organosilicon sealing material its increased polymer while crosslinking Chain length between connection point molecule can control in a certain range, and be unlikely to keep cure silicone rubber excessively soft, to destroy The shape stability of its cured product.This requires other than selecting the chain extender of appropriate chain length to keep being crosslinked in network structure Outside density, to obtain appropriate modulus, keep also making prepared sealing material that there is lower mould outside product shape stability Amount, the performance of high-elongation, meet the requirement of such material under given conditions.
Specific embodiment
Embodiment 1
A kind of appropriateness tough organosilicon sealant, including following raw materials in parts by weight:
Medium viscosity α, 65 parts of alpha, omega-dihydroxy polydimethyl siloxane
Low viscosity α, 30 parts of alpha, omega-dihydroxy polydimethyl siloxane
5 parts of dimethicone
5 parts of two butanone oximino silane of dimethyl
3 parts of polyethylene glycol
10 parts of fumed titanium dioxide
20 parts of nanometer grade calcium carbonate
5 parts of methyl triacetoxysilane
5 parts of ditert-butyldiacetyl oxygen-base silane
0.5 part of dioctyl tin cinnamic acid tin
0.3 part of stannous octoate
8 parts of silane of aminomethyl phenyl two (N- methylacetamido).
Embodiment 2
A kind of appropriateness tough organosilicon sealant, including following raw materials in parts by weight:
Medium viscosity α, 70 parts of alpha, omega-dihydroxy polydimethyl siloxane
Low viscosity α, 35 parts of alpha, omega-dihydroxy polydimethyl siloxane
10 parts of dimethicone
10 parts of two butanone oximino silane of dimethyl
5 parts of polyethylene glycol
15 parts of fumed titanium dioxide
30 parts of nanometer grade calcium carbonate
10 parts of methyl triacetoxysilane
10 parts of ditert-butyldiacetyl oxygen-base silane
1.0 parts of dioctyl tin cinnamic acid tin
0.5 part of stannous octoate
12 parts of silane of aminomethyl phenyl two (N- methylacetamido).
Embodiment 3
A kind of appropriateness tough organosilicon sealant, including following raw materials in parts by weight:
Medium viscosity α, 67.5 parts of alpha, omega-dihydroxy polydimethyl siloxane
Low viscosity α, 32.5 parts of alpha, omega-dihydroxy polydimethyl siloxane
7.5 parts of dimethicone
7.5 parts of two butanone oximino silane of dimethyl
4 parts of polyethylene glycol
12.5 parts of fumed titanium dioxide
25 parts of nanometer grade calcium carbonate
7.5 parts of methyl triacetoxysilane
7.5 parts of ditert-butyldiacetyl oxygen-base silane
0.75 part of dioctyl tin cinnamic acid tin
0.4 part of stannous octoate
10 parts of silane of aminomethyl phenyl two (N- methylacetamido).
Embodiment 4
A kind of appropriateness tough organosilicon sealant, including following raw materials in parts by weight:
Medium viscosity α, 66 parts of alpha, omega-dihydroxy polydimethyl siloxane
Low viscosity α, 32 parts of alpha, omega-dihydroxy polydimethyl siloxane
9 parts of dimethicone
6.5 parts of two butanone oximino silane of dimethyl
4.5 parts of polyethylene glycol
11 parts of fumed titanium dioxide
21 parts of nanometer grade calcium carbonate
8 parts of methyl triacetoxysilane
9 parts of ditert-butyldiacetyl oxygen-base silane
0.9 part of dioctyl tin cinnamic acid tin
0.45 part of stannous octoate
11 parts of silane of aminomethyl phenyl two (N- methylacetamido).

Claims (4)

1. a kind of appropriateness tough organosilicon sealant, it is characterised in that: including following raw materials in parts by weight:
Medium viscosity α, 65-70 parts of alpha, omega-dihydroxy polydimethyl siloxane
Low viscosity α, 30-35 parts of alpha, omega-dihydroxy polydimethyl siloxane
5-10 parts of dimethicone
5-10 parts of two butanone oximino silane of dimethyl
3-5 parts of polyethylene glycol
10-15 parts of fumed titanium dioxide
20-30 parts of nanometer grade calcium carbonate
5-10 parts of methyl triacetoxysilane
5-10 parts of ditert-butyldiacetyl oxygen-base silane
0.5-1.0 parts of dioctyl tin cinnamic acid tin
0.3-0.5 parts of stannous octoate
8-12 parts of silane of aminomethyl phenyl two (N- methylacetamido).
2. a kind of appropriate tough organosilicon sealant according to claim 1, it is characterised in that: the medium viscosity α, ω- Viscosity >=50000mPas of dialkyl polydimethylsiloxane.
3. a kind of appropriate tough organosilicon sealant according to claim 1, it is characterised in that: the low viscosity α, ω- Viscosity >=500mPas of dialkyl polydimethylsiloxane.
4. a kind of preparation method of appropriate tough organosilicon sealant according to claim 1, it is characterised in that: including following technique Step:
A, medium viscosity dialkyl polydimethylsiloxane, low viscosity dialkyl polydimethylsiloxane, dimethicone are weighed, is stirred It mixes uniformly mixed；In high speed agitator, 2h, vacuum dehydration are stirred；
B, fumed titanium dioxide, nanometer grade calcium carbonate, polyethylene glycol, methyl triacetoxysilane is added, continues to stir 1h, Vacuum dehydration；
C, ditert-butyldiacetyl oxygen-base silane, two butanone oximino silane of dimethyl is added, continues to stir 0.5-1.0h；It is added Aminomethyl phenyl two (N- methylacetamido) silane continues to stir 0.5-1.0h；Stannous octoate, dioctyl tin cinnamic acid is added Tin continues to stir 1h；1h is vacuumized, continues to be dehydrated；Discharging, packaging.
CN201710986129.8A 2017-10-20 2017-10-20 A kind of appropriateness tough organosilicon sealant and preparation method thereof Pending CN109694688A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19832687A1 (en) * 1998-07-21 2000-02-03 Heidelberger Bauchemie Gmbh Accelerated acetate-curing silicone masses
CN102746486A (en) * 2012-07-13 2012-10-24 上海拓引数码技术有限公司 Single-component bonding sealing type silicone adhesive for solar battery assembly
CN105086926A (en) * 2015-09-09 2015-11-25 蓝星（成都）新材料有限公司 Flexible organosilicone sealant for LED package and preparation method thereof
CN105385408A (en) * 2015-12-17 2016-03-09 广西华纳新材料科技有限公司 Fatigue-resistant ultraviolet-resistant one-component dealcoholization type silicone structure sealant and preparation method thereof
CN105820579A (en) * 2016-03-23 2016-08-03 航天材料及工艺研究所 One-component room temperature vulcanization conductive shielding and sealing material and preparing method and application thereof
CN107142074A (en) * 2017-05-09 2017-09-08 江苏天辰新材料股份有限公司 A kind of preparation method of de-oxime type one component room temperature fluid sealant

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE19832687A1 (en) * 1998-07-21 2000-02-03 Heidelberger Bauchemie Gmbh Accelerated acetate-curing silicone masses
CN102746486A (en) * 2012-07-13 2012-10-24 上海拓引数码技术有限公司 Single-component bonding sealing type silicone adhesive for solar battery assembly
CN105086926A (en) * 2015-09-09 2015-11-25 蓝星（成都）新材料有限公司 Flexible organosilicone sealant for LED package and preparation method thereof
CN105385408A (en) * 2015-12-17 2016-03-09 广西华纳新材料科技有限公司 Fatigue-resistant ultraviolet-resistant one-component dealcoholization type silicone structure sealant and preparation method thereof
CN105820579A (en) * 2016-03-23 2016-08-03 航天材料及工艺研究所 One-component room temperature vulcanization conductive shielding and sealing material and preparing method and application thereof
CN107142074A (en) * 2017-05-09 2017-09-08 江苏天辰新材料股份有限公司 A kind of preparation method of de-oxime type one component room temperature fluid sealant

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
任春华等: "功能化有机硅密封胶的研究进展 ", 《弹性体》 *
黄文润编著: "《液体硅橡胶》", 30 June 2009, 四川科学技术出版社 *

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