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 PDFInfo
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- 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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- temperature resistant
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- preparation
- superhigh temperature
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- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 238000004821 distillation Methods 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000010792 warming Methods 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000003863 metallic catalyst Substances 0.000 claims abstract description 12
- 125000002524 organometallic group Chemical group 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 10
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229920000642 polymer Polymers 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000010992 reflux Methods 0.000 claims abstract description 6
- 238000013517 stratification Methods 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 239000010936 titanium Substances 0.000 claims description 5
- 239000011701 zinc Substances 0.000 claims description 5
- 229910052725 zinc Inorganic materials 0.000 claims description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 4
- 239000000908 ammonium hydroxide Substances 0.000 claims description 4
- 230000000694 effects Effects 0.000 abstract description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000013329 compounding Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- YQGOWXYZDLJBFL-UHFFFAOYSA-N dimethoxysilane Chemical compound CO[SiH2]OC YQGOWXYZDLJBFL-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
- C08G77/08—Preparatory processes characterised by the catalysts used
Landscapes
- 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
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.
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Citations (4)
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 |
-
2018
- 2018-09-05 CN CN201811032364.2A patent/CN109369916A/en active Pending
Patent Citations (4)
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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