CN106433146A - Room-temperature vulcanization heat-resistant silicon rubber with active hydrogen based cage structure and preparation method thereof - Google Patents
Room-temperature vulcanization heat-resistant silicon rubber with active hydrogen based cage structure and preparation method thereof Download PDFInfo
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- CN106433146A CN106433146A CN201610809804.5A CN201610809804A CN106433146A CN 106433146 A CN106433146 A CN 106433146A CN 201610809804 A CN201610809804 A CN 201610809804A CN 106433146 A CN106433146 A CN 106433146A
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 46
- 239000001257 hydrogen Substances 0.000 title claims abstract description 20
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 20
- 238000004073 vulcanization Methods 0.000 title claims abstract description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 23
- 229920001971 elastomer Polymers 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 20
- 239000005060 rubber Substances 0.000 claims abstract description 18
- -1 vinylsiloxane Chemical class 0.000 claims abstract description 14
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 13
- 239000003112 inhibitor Substances 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 7
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 23
- 239000004945 silicone rubber Substances 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000011521 glass Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 229910052697 platinum Inorganic materials 0.000 claims description 11
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 8
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 239000013078 crystal Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims description 3
- 239000005052 trichlorosilane Substances 0.000 claims description 3
- 229910004721 HSiCl3 Inorganic materials 0.000 claims description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 2
- 238000006482 condensation reaction Methods 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 abstract 1
- 238000007259 addition reaction Methods 0.000 abstract 1
- 238000004132 cross linking Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 239000000806 elastomer Substances 0.000 description 5
- 150000002431 hydrogen Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229920002545 silicone oil Polymers 0.000 description 3
- ARLJCLKHRZGWGL-UHFFFAOYSA-N ethenylsilicon Chemical compound [Si]C=C ARLJCLKHRZGWGL-UHFFFAOYSA-N 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 0 C*(*N)O*=CN Chemical compound C*(*N)O*=CN 0.000 description 1
- 239000005046 Chlorosilane Substances 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- KOPOQZFJUQMUML-UHFFFAOYSA-N chlorosilane Chemical compound Cl[SiH3] KOPOQZFJUQMUML-UHFFFAOYSA-N 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 229920000260 silastic Polymers 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
Classifications
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/549—Silicon-containing compounds containing silicon in a ring
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic Table
- C07F7/02—Silicon compounds
- C07F7/21—Cyclic compounds having at least one ring containing silicon, but no carbon in the ring
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/244—Stepwise homogeneous crosslinking of one polymer with one crosslinking system, e.g. partial curing
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use 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; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses room-temperature vulcanization heat-resistant silicon rubber with an active hydrogen based cage structure and a preparation method thereof, and in particular relates to silicon rubber and a preparation method thereof. The silicon rubber is prepared from the raw materials of vinylsiloxane rubber, a crosslinking agent, a solvent, a Pt catalyst, and PC610 with the following percentages by weight: 60-70% of the vinylsiloxane rubber, 2-4% of the crosslinking agent,30-40% of cyclohexane, 0.3-0.5% of the Pt catalyst, and 0.01-0.02% of an inhibitor. Polyhedral oligomeric silsesquioxane (POSS) is added into a vinylsiloxane rubber system in a mode of chemical bonding, and under the action of the catalyst, the polyhedral oligomeric silsesquioxane and vinylsiloxane rubber are subjected to an addition reaction, so that the crosslinking density of the silicon rubber is improved, and POSS reinforced novel room-temperature vulcanization silicon rubber with good thermal stability and mechanical properties is prepared.
Description
Technical field
The present invention relates to a kind of silicone rubber and preparation method thereof, more particularly to a kind of with active hydrogen-based cage structure
Room temperature vulcanization heat-resistant silicon rubber and preparation method thereof.
Background technology
Silicone rubber is due to the characteristic such as its excellent resistant of high or low temperature, weatherability, ozone resistance and electric property, and adds phase
The filler that answers can make the conductive rubber of various uses, heat conductive rubber, thus in aerospace field, be mainly used as spacecraft table
Facestock material binders for coatings etc., it turns out that, severe spatial environmentss can destroy polymeric material, therefore improve the resistance to of silicone rubber
Hot have very important significance.
Silastic elastomer is typically to adopt containing hydrogen silicone oil as cross-linking agent at present, but the silicon rubber heat-resisting temperature after solidification
Tend not to meet operation requirement, heat stability and mechanical property are poor.
Cage-type silsesquioxane (POSS), its general molecular formula is(RSiO3/2)n.It is that the organic-inorganic that latest development is got up is received
Nano composite material, with excellent thermal stability and mechanical property, is added in the middle of silicone rubber not only as cross-linking agent
The heat stability that silicone rubber can be improved can also improve its mechanical property.
Content of the invention
It is an object of the invention to provide a kind of room temperature vulcanization heat-resistant silicon rubber with active hydrogen-based cage structure and its
Preparation method, the octahydro base cage-type silsesquioxane for preparing is reacted with silicone rubber by the present invention as cross-linking agent, improves silicone rubber
Crosslink density, improve silicon rubber heat-resisting temperature while, improve silicone rubber heat stability and its mechanical property.
The purpose of the present invention is achieved through the following technical solutions:
A kind of room temperature vulcanization heat-resistant silicon rubber with active hydrogen-based cage structure, octahydro base cage-type silsesquioxane selected by raw material
(T8H8), it is by trichlorosilane, solvent, catalyst, and concentrated hydrochloric acid is obtained by hydrolysis-condensation reaction, and proportioning is as follows(Mass fraction):Three
Chlorosilane 7%-8%, solvent 75%-80%, catalyst 10%-15%, concentrated hydrochloric acid 4%-6%, react as follows:
A kind of described described room temperature vulcanization heat-resistant silicon rubber with active hydrogen-based cage structure, solvent is methanol, toluene,
Normal hexane, two or three of combination in petroleum ether.
A kind of described room temperature vulcanization heat-resistant silicon rubber with active hydrogen-based cagelike structure, catalyst is anhydrous tri-chlorination
One kind in aluminum or ferric chloride.
A kind of described room temperature vulcanization heat-resistant silicon rubber with active hydrogen-based cagelike structure, vinyl silicon selected by raw material
Rubber, cross-linking agent, solvent, Pt platinum catalyst, PC610, are prepared by following weight ratio (%):Vinylsiloxane rubber 60%-
70%, cross-linking agent 2%-4%, 0. 3%-0. 5% of hexamethylene 30%-40%, Pt catalyst, inhibitor 0.01%-0.02%, reactional equation
Formula is as follows:
A kind of described room temperature vulcanization heat-resistant silicon rubber with active hydrogen-based cage structure, described vinylsiloxane rubber, glues
Spend for 20000MPa.s;
A kind of room temperature vulcanization heat-resistant silicon rubber preparation method with active hydrogen-based cage structure, comprises the following steps:
(1)The preparation of octahydro base cage-type silsesquioxane
Catalyst and concentrated hydrochloric acid being added in there-necked flask, is subsequently added and solvent is also added in there-necked flask, stirs 30 min
By HSiCl3It is dissolved in solvent, is slowly dropped in 6h in flask, after completion of dropping, continues quick stirring 1h, course of reaction
Not higher than 60 DEG C of middle control system temperature, reacts in N2Carry out under gas shield, after completion of the reaction separately normal hexane layer, will band
The normal hexane layer for having a small amount of tan crystals is filtered, and filtrate adds anhydrous C aC l2And anhydrous K2CO3It is stirred overnight, filters;Will
The distillation of gained liquid pressure-reducing is filtered, crystal precipitation has been concentrated into, products therefrom has been collected, then is washed with solvent 2 times, obtain product
T8H8;
(2)The preparation of addition type room temperature vulcanized silicone rubber
Weigh cage modle octahydro base silsesquioxane(POSS)In beaker, hexamethylene is used as solvent so as to dissolve, and adds vinyl
Silicone rubber, makes its mixing with Glass rod stirring;Evacuation de-bubble in vacuum drying oven is put into, then, PC610 inhibitor is added,
Platinum catalyst is added after Glass rod stirring and evenly mixing, put into after stirring evenly under room temperature environment, until silicone rubber becomes to have the bullet of hardness
Gonosome.
Advantages of the present invention with effect is:
In the present invention, octahydro base cage-type silsesquioxane is added in vinylsiloxane rubber as cross-linking agent.Its heat resisting temperature can
More than 400 DEG C are reached, the heat stability of silicone rubber compared with the cross-linking agent such as containing hydrogen silicone oil, is not only substantially increased, is also improved
The combination properties such as its mechanical property, expand the range of application of cage-type silsesquioxane.
Specific embodiment
With reference to embodiment, the present invention is described in detail.
Do not do in following instance illustrate refer both to mass percent.
In embodiment, raw material removes specified otherwise, is commercial.
Implement raw materials used:
Vinylsiloxane rubber
Cross-linking agent is homemade octahydro base cage-type silsesquioxane
Catalyst is Pt platinum catalyst
Inhibitor is PC610
Solvent is hexamethylene
Embodiment 1
Weigh the cage modle octahydro base silsesquioxane that mass fraction is 2.5%(POSS)In beaker, 35% hexamethylene is used as molten
Agent so as to dissolve.64.2% vinylsiloxane rubber is added, and its mixing is made with Glass rod stirring.It is put in vacuum drying oven and takes out very
Empty de-bubble.Then, 0.02%PC610 inhibitor being added, 0.45% platinum catalyst is added after Glass rod stirring and evenly mixing, is put after stirring evenly
Under entering to room temperature environment, a period of time is placed, until silicone rubber becomes the elastomer for having certain degree of hardness.
Embodiment 2
Weigh the cage modle octahydro base silsesquioxane that mass fraction is 3%(POSS)In beaker, 35% hexamethylene as solvent,
Make its dissolving.64.2% vinylsiloxane rubber is added, and its mixing is made with Glass rod stirring.It is put into evacuation in vacuum drying oven
De-bubble.Then, 0.02%PC610 inhibitor being added, 0.45% platinum catalyst is added after Glass rod stirring and evenly mixing, is put into after stirring evenly
To under room temperature environment, a period of time is placed, until silicone rubber becomes the elastomer for having certain degree of hardness.
Embodiment 3
Weigh the cage modle octahydro base silsesquioxane that mass fraction is 4%(POSS)In beaker, 35% hexamethylene as solvent,
Make its dissolving.64.2% vinylsiloxane rubber is added, and its mixing is made with Glass rod stirring.It is put into evacuation in vacuum drying oven
De-bubble.Then, 0.02%PC610 inhibitor being added, 0.45% platinum catalyst is added after Glass rod stirring and evenly mixing, is put into after stirring evenly
To under room temperature environment, a period of time is placed, until silicone rubber becomes the elastomer for having certain degree of hardness.
Comparative example
Weigh mass fraction be 3% containing hydrogen silicone oil in beaker, add 64.2% vinyl silicon 2%PC610 inhibitor, glass
0.45% platinum catalyst being added after rod stirring and evenly mixing, is put under room temperature environment after stirring evenly, places a period of time, until silicon rubber
Glue becomes the elastomer for having certain degree of hardness.
.
Can be seen that in embodiment 1-3 by data in form adds octahydro base cage-type silsesquioxane to add as cross-linking agent
Enter in the middle of vinylsiloxane rubber, due to eight summits of cage-type silsesquioxane be respectively connected with double in Si -- H bond and silicone rubber
There is hydrosilylation in key, improve the crosslink density of silicone rubber, and then improve the heat stability of silicone rubber, cage model sesquialter
Siloxane structure characteristic, can function as reinforcing agent, improve the mechanical property of silicone rubber.
Claims (6)
1. a kind of room temperature vulcanization heat-resistant silicon rubber with active hydrogen-based cage structure, it is characterised in that octahydro base cage selected by raw material
Type silsesquioxane(T8H8), it is by trichlorosilane, solvent, catalyst, and concentrated hydrochloric acid is obtained by hydrolysis-condensation reaction, and proportioning is as follows
(Mass fraction):Trichlorosilane 7%-8%, solvent 75%-80%, catalyst 10%-15%, concentrated hydrochloric acid 4%-6%, react as follows:
.
2. described a kind of room temperature vulcanization heat-resistant silicon rubber with active hydrogen-based cage structure according to claim 1,
It is characterized in that solvent is methanol, toluene, and normal hexane, two or three of combination in petroleum ether.
3. a kind of room temperature vulcanization heat-resistant silicon rubber with active hydrogen-based cagelike structure according to claim 1, its feature
It is catalyst for the one kind in aluminum trichloride (anhydrous) or ferric chloride.
4. a kind of room temperature vulcanization heat-resistant silicon rubber with active hydrogen-based cagelike structure according to claim 1, its feature
It is that raw material, from vinylsiloxane rubber, cross-linking agent, solvent, Pt platinum catalyst, PC610, is joined by following weight ratio (%)
System:Vinylsiloxane rubber 60%-70%, cross-linking agent 2%-4%, 0. 3%-0. 5% of hexamethylene 30%-40%, Pt catalyst, inhibitor
0.01%-0.02%, reaction equation is as follows:
.
5. a kind of room temperature vulcanization heat-resistant silicon rubber with active hydrogen-based cage structure according to claim 4, its feature
It is described vinylsiloxane rubber, viscosity is 20000MPa.s.
6. a kind of room temperature vulcanization heat-resistant silicon rubber preparation method with active hydrogen-based cage structure, it is characterised in that including following
Step:
The preparation of octahydro base cage-type silsesquioxane
Catalyst and concentrated hydrochloric acid being added in there-necked flask, is subsequently added and solvent is also added in there-necked flask, stirs 30 min
By HSiCl3It is dissolved in solvent, is slowly dropped in 6h in flask, after completion of dropping, continues quick stirring 1h, course of reaction
Not higher than 60 DEG C of middle control system temperature, reacts in N2Carry out under gas shield, after completion of the reaction separately normal hexane layer, will band
The normal hexane layer for having a small amount of tan crystals is filtered, and filtrate adds anhydrous C aC l2And anhydrous K2CO3It is stirred overnight, filters;Will
The distillation of gained liquid pressure-reducing is filtered, crystal precipitation has been concentrated into, products therefrom has been collected, then is washed with solvent 2 times, obtain product
T8H8;
The preparation of addition type room temperature vulcanized silicone rubber
Weigh cage modle octahydro base silsesquioxane(POSS)In beaker, hexamethylene is used as solvent so as to dissolve, and adds vinyl
Silicone rubber, makes its mixing with Glass rod stirring;Evacuation de-bubble in vacuum drying oven is put into, then, PC610 inhibitor is added,
Platinum catalyst is added after Glass rod stirring and evenly mixing, put into after stirring evenly under room temperature environment, until silicone rubber becomes to have the bullet of hardness
Gonosome.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109749083A (en) * | 2018-12-10 | 2019-05-14 | 沈阳化工大学 | Eight (trimethoxy silica ethyl) poss silicone rubber crosslinking agent |
CN110016297A (en) * | 2019-02-25 | 2019-07-16 | 陈琪峰 | A kind of conductive adhesive film and preparation method thereof |
CN111253860A (en) * | 2020-02-09 | 2020-06-09 | 西北工业大学 | Ablation-resistant organic silicon resin coating material and preparation method thereof |
CN114437355A (en) * | 2021-12-31 | 2022-05-06 | 山东省科学院新材料研究所 | Polymer cross-linking agent based on cage-type silsesquioxane structure |
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CN102181159A (en) * | 2011-03-15 | 2011-09-14 | 杭州师范大学 | Polysilsesquioxane reinforced light emitting diode (LED) encapsulation organic silicon rubber and preparation method thereof |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109749083A (en) * | 2018-12-10 | 2019-05-14 | 沈阳化工大学 | Eight (trimethoxy silica ethyl) poss silicone rubber crosslinking agent |
CN110016297A (en) * | 2019-02-25 | 2019-07-16 | 陈琪峰 | A kind of conductive adhesive film and preparation method thereof |
CN111253860A (en) * | 2020-02-09 | 2020-06-09 | 西北工业大学 | Ablation-resistant organic silicon resin coating material and preparation method thereof |
CN114437355A (en) * | 2021-12-31 | 2022-05-06 | 山东省科学院新材料研究所 | Polymer cross-linking agent based on cage-type silsesquioxane structure |
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