CN109369916A - A kind of preparation method of superhigh temperature resistant silicone intermediate - Google Patents

A kind of preparation method of superhigh temperature resistant silicone intermediate Download PDF

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Publication number
CN109369916A
CN109369916A CN201811032364.2A CN201811032364A CN109369916A CN 109369916 A CN109369916 A CN 109369916A CN 201811032364 A CN201811032364 A CN 201811032364A CN 109369916 A CN109369916 A CN 109369916A
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China
Prior art keywords
temperature resistant
parts
minutes
preparation
superhigh temperature
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CN201811032364.2A
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江日新
肖杰
钟法往
林海滨
卢观庆
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Huizhou Reed New Materials Polytron Technologies Inc
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Huizhou Reed New Materials Polytron Technologies Inc
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Priority to CN201811032364.2A priority Critical patent/CN109369916A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • C08G77/06Preparatory processes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G77/00Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
    • C08G77/04Polysiloxanes
    • C08G77/06Preparatory processes
    • C08G77/08Preparatory processes characterised by the catalysts used

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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)
  • Catalysts (AREA)

Abstract

The invention discloses a kind of preparation methods of superhigh temperature resistant silicone intermediate, comprising the following steps: phenyltrimethoxysila,e, phenyidimethoxysilane, organosilicon linear body and methyltrimethoxysilane are uniformly mixed by S1., and water stirring is added;S2. the catalyst of 1% concentration is slowly added dropwise, after, it is warming up to 70-100 DEG C of reflux 120-240 minutes;S3. flow back after, be cooled to 40 DEG C hereinafter, be added neutralizer be neutralized to pH value be 8, with filter funnel stratification, take lower liquid;S4. performed polymer is warming up to 70 DEG C, vacuumizes distillation and organo-metallic catalyst is added after distillation to no liquid outflow, is warming up to 120 DEG C and flows back 120 minutes, redistillation 30 minutes, cooling discharge;Product of the present invention has superhigh temperature resistant effect.

Description

A kind of preparation method of superhigh temperature resistant silicone intermediate
Technical field
The present invention relates to adhesive tape production fields, and in particular to a kind of preparation method of superhigh temperature resistant silicone intermediate.
Background technique
Superhigh temperature resistant silicone intermediate is that one kind can improve other materials temperature tolerance, adhesive force, gloss with reactive grafting Etc. performances synthetic intermediate material.This silicone intermediate, can be direct in the case where not needing any other additive More than 600 DEG C high temperature are resistant to, and can be worked under the conditions of 400 DEG C for a long time, it is roasting in non-stick pan coating, powdery paints, high temperature resistant The industries such as paint are widely used.
But the existing resistance to temp effect of silicone intermediate be not it is highly desirable, since it is desired that more catalyst, cost Higher, moreover, the prior art needs to realize high temperature resistant by the scheme of compounding inorganic matter, the poor medium-sized and small enterprises of some technologies are real Now get up relatively difficult.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of preparation method of superhigh temperature resistant silicone intermediate, the present invention is produced After product first pass through hydrolytie polycondensation synthesis performed polymer, then by temperature, catalyst adjusting molecular structure, so that product is with fabulous Resistance to temp effect.Moreover, compared with prior art, the prior art needs to realize high temperature resistant by the scheme of compounding inorganic matter, and originally Invention carries out molecular regulation by more complex design technology, and a large amount of molecular radicals fabulous using this heatproof of phenyl are realized The superhigh temperature resistant effect of organic matter.
In order to solve the above technical problems, the technical scheme is that a kind of preparation of superhigh temperature resistant silicone intermediate Method, comprising the following steps:
S1. phenyltrimethoxysila,e, phenyidimethoxysilane, organosilicon linear body and methyltrimethoxysilane are mixed Uniformly, water stirring is added;
S2. the catalyst of 1% concentration is slowly added dropwise, after, it is warming up to 70-100 DEG C of reflux 120-240 minutes;
S3. after flowing back, 40 DEG C are cooled to hereinafter, it is 8 that neutralizer, which is added, to be neutralized to pH value, with filter funnel stratification, Take lower liquid;
S4. performed polymer is warming up to 70 DEG C, vacuumizes distillation and organo-metallic catalyst is added after distillation to no liquid outflow, rises Temperature to 120 DEG C flow back 120 minutes, redistillation 30 minutes, cooling discharge.
Preferably, phenyltrimethoxysila,e described in step S1, phenyidimethoxysilane, organosilicon linear body, first Base trimethoxy silane, water parts by weight component be followed successively by 0-50 parts, 0-50 parts, 0-30 parts, 0-10 parts, 0-100 parts, and add Enter water stirring to carry out at normal temperature, mixing time is 30-60 minutes.
Preferably, catalyst described in step S2 is hydrochloric acid or sulfuric acid.
Preferably, neutralizer described in step S3 is ammonium hydroxide or ethylenediamine or sodium hydroxide.
Preferably, the vacuum degree that distillation is vacuumized described in step S4 is 0.06-0.08.
Preferably, organo-metallic catalyst described in step S4 is organic zinc or organotin or organic titanium.
It is that the present invention realizes the utility model has the advantages that product of the present invention first pass through hydrolytie polycondensation synthesis performed polymer after, then by temperature, Catalyst adjusts molecular structure, so that product has fabulous resistance to temp effect.Moreover, compared with prior art, the prior art needs High temperature resistant is realized by compounding the scheme of inorganic matter, and the present invention carries out molecular regulation by more complex design technology, greatly The amount molecular radical fabulous using this heatproof of phenyl, realizes the superhigh temperature resistant effect of organic matter.
Specific embodiment
In order to facilitate the understanding of those skilled in the art, further being retouched in detail below in conjunction with embodiment to the present invention It states.
The preparation method of superhigh temperature resistant silicone intermediate, comprising the following steps:
S1. phenyltrimethoxysila,e, phenyidimethoxysilane, organosilicon linear body and methyltrimethoxysilane are mixed Uniformly, water stirring is added;
S2. the catalyst of 1% concentration is slowly added dropwise, after, it is warming up to 70-100 DEG C of reflux 120-240 minutes;
S3. after flowing back, 40 DEG C are cooled to hereinafter, it is 8 that neutralizer, which is added, to be neutralized to pH value, with filter funnel stratification, Take lower liquid;
S4. performed polymer is warming up to 70 DEG C, vacuumizes distillation and organo-metallic catalyst is added after distillation to no liquid outflow, rises Temperature to 120 DEG C flow back 120 minutes, redistillation 30 minutes, cooling discharge.
Specifically, phenyltrimethoxysila,e described in step S1, phenyidimethoxysilane, organosilicon linear body, first Base trimethoxy silane, water parts by weight component be followed successively by 0-50 parts, 0-50 parts, 0-30 parts, 0-10 parts, 0-100 parts, and add Enter water stirring to carry out at normal temperature, mixing time is 30-60 minutes.
Specifically, catalyst described in step S2 is hydrochloric acid or sulfuric acid.
Specifically, neutralizer described in step S3 is ammonium hydroxide or ethylenediamine or sodium hydroxide.
Specifically, the vacuum degree for vacuumizing distillation described in step S4 is 0.06-0.08.
Specifically, organo-metallic catalyst described in step S4 is organic zinc or organotin or organic titanium.
Embodiment one
The preparation method of superhigh temperature resistant silicone intermediate above-mentioned is combined into specific way in reality, does corresponding elaboration, It is specific as follows: the preparation method of superhigh temperature resistant silicone intermediate, comprising the following steps:
S1. phenyltrimethoxysila,e, phenyidimethoxysilane, organosilicon linear body and methyltrimethoxysilane are mixed Uniformly, water stirring is added;
S2. the catalyst of 1% concentration is slowly added dropwise, after, it is warming up to 70-100 DEG C of reflux 120-240 minutes;
S3. after flowing back, 40 DEG C are cooled to hereinafter, it is 8 that neutralizer, which is added, to be neutralized to pH value, with filter funnel stratification, Take lower liquid;
S4. performed polymer is warming up to 70 DEG C, vacuumizes distillation and organo-metallic catalyst is added after distillation to no liquid outflow, rises Temperature to 120 DEG C flow back 120 minutes, redistillation 30 minutes, cooling discharge.
Specifically, phenyltrimethoxysila,e described in step S1, phenyidimethoxysilane, organosilicon linear body, first Base trimethoxy silane, water parts by weight component be followed successively by 0-50 parts, 0-50 parts, 0-30 parts, 0-10 parts, 0-100 parts, and add Enter water stirring to carry out at normal temperature, mixing time is 30-60 minutes.
Specifically, catalyst described in step S2 is hydrochloric acid or sulfuric acid.
Specifically, neutralizer described in step S3 is ammonium hydroxide or ethylenediamine or sodium hydroxide.
Specifically, the vacuum degree for vacuumizing distillation described in step S4 is 0.06-0.08.
Specifically, organo-metallic catalyst described in step S4 is organic zinc or organotin or organic titanium.
In the present embodiment: being specially by 25 parts of phenyltrimethoxysila,e, 25 parts of phenyidimethoxysilane, organosilicon line Property 15 parts of body, methyltrimethoxysilane be uniformly mixed.80 parts of water is added, is stirred 60 minutes under room temperature.It is dense to be slowly added dropwise 1% The hydrochloric acid of degree, after, it is warming up to 100 DEG C and flows back 240 minutes.After reflux, 40 DEG C are cooled to hereinafter, neutralizer ammonia is added It is 8 that water, which is neutralized to pH value, with filter funnel stratification, takes lower liquid (performed polymer).Performed polymer is warming up to 70 DEG C, is taken out true Organo-metallic catalyst organic zinc is added after distillation to no liquid outflow in sky distillation, vacuum degree 0.06, is warming up to 120 DEG C and returns Stream 120 minutes, redistillation 30 minutes, cooling discharge.Test data are as follows: appearance: yellowish;Index of refraction: 1.472;Hydroxyl value: 0.8%; Heatproof (500 DEG C, 30 minutes): OK;Surface tension: 26.
Embodiment two
As embodiment one with two basic setup of embodiment is, primary difference is that: the present embodiment is used phenyl trimethoxy 15 parts of base silane, 35 parts of phenyidimethoxysilane, 15 parts of organosilicon linear body, methyltrimethoxysilane are uniformly mixed.It takes out Vacuum distillation, vacuum degree 0.08.Organo-metallic catalyst is organotin.Test data are as follows: appearance: yellowish;Index of refraction: 1.475;Hydroxyl value: 0.8%;Heatproof (500 DEG C, 30 minutes): OK;Surface tension: 24.
Embodiment three
As embodiment three with one basic setup of embodiment is, primary difference is that: by 15 parts of phenyltrimethoxysila,e, benzene 25 parts of base dimethoxysilane, 20 parts of organosilicon linear body, methyltrimethoxysilane are uniformly mixed.Vacuumize distillation, vacuum Degree is 0.07.Addition organo-metallic catalyst is organic titanium.Test data are as follows: appearance: yellowish;Index of refraction: 1.473;Hydroxyl value: 0.8%;Heatproof (500 DEG C, 30 minutes): OK;Surface tension: 23.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair The restriction of embodiments of the present invention.For those of ordinary skill in the art, may be used also on the basis of the above description To make other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all this Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within the spirit and principle of invention Protection scope within.

Claims (6)

1. a kind of preparation method of superhigh temperature resistant silicone intermediate, which comprises the following steps:
S1. phenyltrimethoxysila,e, phenyidimethoxysilane, organosilicon linear body and methyltrimethoxysilane are mixed Uniformly, water stirring is added;
S2. the catalyst of 1% concentration is slowly added dropwise, after, it is warming up to 70-100 DEG C of reflux 120-240 minutes;
S3. after flowing back, 40 DEG C are cooled to hereinafter, it is 8 that neutralizer, which is added, to be neutralized to pH value, with filter funnel stratification, Take lower liquid;
S4. performed polymer is warming up to 70 DEG C, vacuumizes distillation and organo-metallic catalyst is added after distillation to no liquid outflow, rises Temperature to 120 DEG C flow back 120 minutes, redistillation 30 minutes, cooling discharge.
2. the preparation method of superhigh temperature resistant silicone intermediate according to claim 1, it is characterised in that: institute in step S1 State phenyltrimethoxysila,e, phenyidimethoxysilane, organosilicon linear body, methyltrimethoxysilane, the parts by weight of water Array point is followed successively by 0-50 parts, 0-50 parts, 0-30 parts, 0-10 parts, 0-100 parts, and water stirring is added and carries out at normal temperature, stirs Time is 30-60 minutes.
3. the preparation method of superhigh temperature resistant silicone intermediate according to claim 1, it is characterised in that: institute in step S2 The catalyst stated is hydrochloric acid or sulfuric acid.
4. the preparation method of superhigh temperature resistant silicone intermediate according to claim 1, it is characterised in that: institute in step S3 The neutralizer stated is ammonium hydroxide or ethylenediamine or sodium hydroxide.
5. the preparation method of superhigh temperature resistant silicone intermediate according to claim 1, it is characterised in that: institute in step S4 The vacuum degree for vacuumizing distillation stated is 0.06-0.08.
6. the preparation method of superhigh temperature resistant silicone intermediate according to claim 1, it is characterised in that: institute in step S4 Stating organo-metallic catalyst is organic zinc or organotin or organic titanium.
CN201811032364.2A 2018-09-05 2018-09-05 A kind of preparation method of superhigh temperature resistant silicone intermediate Pending CN109369916A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101857674A (en) * 2010-05-27 2010-10-13 大连交通大学 Method for synthesizing high-temperature resistant organic silicon resin
CN104974349A (en) * 2014-04-07 2015-10-14 马凤国 Preparation method of silicone resin
WO2016082287A1 (en) * 2014-11-27 2016-06-02 深圳市森日有机硅材料有限公司 Mdq phenyl vinyl silicone resin and preparation method therefor
CN106750312A (en) * 2017-03-27 2017-05-31 成都硅宝科技股份有限公司 Phenyl DT silicones and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101857674A (en) * 2010-05-27 2010-10-13 大连交通大学 Method for synthesizing high-temperature resistant organic silicon resin
CN104974349A (en) * 2014-04-07 2015-10-14 马凤国 Preparation method of silicone resin
WO2016082287A1 (en) * 2014-11-27 2016-06-02 深圳市森日有机硅材料有限公司 Mdq phenyl vinyl silicone resin and preparation method therefor
CN106750312A (en) * 2017-03-27 2017-05-31 成都硅宝科技股份有限公司 Phenyl DT silicones and preparation method thereof

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Application publication date: 20190222

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