CN106397775A - High temperature resistant silane cross-linking agent with L-POSS import and preparation method thereof - Google Patents
High temperature resistant silane cross-linking agent with L-POSS import and preparation method thereof Download PDFInfo
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- CN106397775A CN106397775A CN201610809803.0A CN201610809803A CN106397775A CN 106397775 A CN106397775 A CN 106397775A CN 201610809803 A CN201610809803 A CN 201610809803A CN 106397775 A CN106397775 A CN 106397775A
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- high temperature
- temperature resistant
- linking agent
- silane
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- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910000077 silane Inorganic materials 0.000 title claims abstract description 41
- 239000003431 cross linking reagent Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 230000008676 import Effects 0.000 title abstract 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 239000004342 Benzoyl peroxide Substances 0.000 claims abstract description 13
- 235000019400 benzoyl peroxide Nutrition 0.000 claims abstract description 13
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000047 product Substances 0.000 claims abstract description 12
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003999 initiator Substances 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000012467 final product Substances 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 238000006555 catalytic reaction Methods 0.000 claims abstract 2
- 239000004971 Cross linker Substances 0.000 claims description 25
- 238000010792 warming Methods 0.000 claims description 12
- 238000010992 reflux Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 230000004913 activation Effects 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 239000010413 mother solution Substances 0.000 claims description 6
- 239000000376 reactant Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- JLTDJTHDQAWBAV-UHFFFAOYSA-N N,N-dimethylaniline Chemical compound CN(C)C1=CC=CC=C1 JLTDJTHDQAWBAV-UHFFFAOYSA-N 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 4
- GGSUCNLOZRCGPQ-UHFFFAOYSA-N diethylaniline Chemical compound CCN(CC)C1=CC=CC=C1 GGSUCNLOZRCGPQ-UHFFFAOYSA-N 0.000 claims description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 4
- -1 silicon Alkane Chemical class 0.000 claims description 4
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 2
- DJEQZVQFEPKLOY-UHFFFAOYSA-N N,N-dimethylbutylamine Chemical compound CCCCN(C)C DJEQZVQFEPKLOY-UHFFFAOYSA-N 0.000 claims description 2
- SVYKKECYCPFKGB-UHFFFAOYSA-N N,N-dimethylcyclohexylamine Chemical compound CN(C)C1CCCCC1 SVYKKECYCPFKGB-UHFFFAOYSA-N 0.000 claims description 2
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 claims description 2
- 239000012267 brine Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 2
- CIXSDMKDSYXUMJ-UHFFFAOYSA-N n,n-diethylcyclohexanamine Chemical compound CCN(CC)C1CCCCC1 CIXSDMKDSYXUMJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052697 platinum Inorganic materials 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- IMFACGCPASFAPR-UHFFFAOYSA-N tributylamine Chemical compound CCCCN(CCCC)CCCC IMFACGCPASFAPR-UHFFFAOYSA-N 0.000 claims description 2
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 claims description 2
- YFTHZRPMJXBUME-UHFFFAOYSA-N tripropylamine Chemical compound CCCN(CCC)CCC YFTHZRPMJXBUME-UHFFFAOYSA-N 0.000 claims description 2
- 239000007822 coupling agent Substances 0.000 claims 1
- 229910052710 silicon Inorganic materials 0.000 claims 1
- 239000010703 silicon Substances 0.000 claims 1
- 229920002554 vinyl polymer Polymers 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 3
- 229920006351 engineering plastic Polymers 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 2
- 230000003213 activating effect Effects 0.000 abstract 1
- 229940023462 paste product Drugs 0.000 abstract 1
- 229920003023 plastic Polymers 0.000 abstract 1
- 239000004033 plastic Substances 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 239000011541 reaction mixture Substances 0.000 abstract 1
- 230000000284 resting effect Effects 0.000 abstract 1
- 150000004756 silanes Chemical class 0.000 abstract 1
- 238000005979 thermal decomposition reaction Methods 0.000 abstract 1
- 238000000354 decomposition reaction Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 241001597008 Nomeidae Species 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000010276 construction Methods 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- JGFZNNIVVJXRND-UHFFFAOYSA-N N,N-Diisopropylethylamine (DIPEA) Chemical compound CCN(C(C)C)C(C)C JGFZNNIVVJXRND-UHFFFAOYSA-N 0.000 description 2
- 229910018557 Si O Inorganic materials 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 1
- 229910018540 Si C Inorganic materials 0.000 description 1
- 241000826860 Trapezium Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 150000003961 organosilicon compounds Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical class [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- C08G77/38—Polysiloxanes modified by chemical after-treatment
- C08G77/382—Polysiloxanes modified by chemical after-treatment containing atoms other than carbon, hydrogen, oxygen or silicon
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Silicon Polymers (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
Provided is a high temperature resistant silane cross-linking agent with L-POSS import and preparation method thereof, relating to a cross-linking agent and preparation method thereof. The catalysis activity produced silane generated reactive point and L - POSS react to develop to polymerization then synthesize out new silane derivatives. The vinyltrimethoxysilane joins a three opening flasks, heating then stirring with catalyst triethylamine and initiator benzoyl peroxide in an agitator, and heating slowly, raising the temperature, placing the L-POSS in a constant pressure liquid dripping funnel and dripping slowly, at the same time stirring and reacting, taking out the reaction mixture and resting and activating, separating the mother liquid by a liquid separation funnel, and resulting in a sublayer thick paste product, placing the product in a vacuum drying cabinet to dry, and resulting in the final product. The L - POSS group is introduced on the basis of silane, due to the high temperature resistance of L-POSS. The thermal decomposition temperature of the cross-linking agent is raised, and the scope of application is wider. The high temperature resistant silane cross-linking agent with L-POSS import is mainly used in the field of special plastics and engineering plastics.
Description
Technical field
The present invention relates to a kind of cross-linking agent and preparation method thereof, more particularly to a kind of high temperature resistant crosslinkable silane containing L-POSS
Connection agent and preparation method thereof.
Background technology
Cross-linking agent is a kind of material making multiple linear molecules be bonded to cross-linked structure, and silane crosslinker is cross-linking agent
One of, it is the low molecule organo-silicon compound that a class has special construction, the silanol of each molecule of silane and inorganic particle
Hydroxyl reaction on particle surface, and mutual association oligomerisation forms network structure, possesses certain crosslinked action, synthesis technique and
Performance is ripe, but silane is as cross-linking agent, and the thermodynamic property that it possesses is not enough so as to the application in certain field is subject to
Limit, still can lift the deficiency of its thermodynamic property aspect using the derivant of silane.
Therefore we are concerned about L-POSS and possess superior performance, and it can form the derivant of silane with silane.L-POSS
Be the Si-O key larger containing bond energy and Si-C key and be made up of huge trapezium structure, be a kind of be inorganic interior with Si-O
Core, the larger macromole of intermolecular force, therefore there is the good performance such as high temperature resistant, pressure, L-POSS monomer structure
Novelty and Polymer Materials ' Structure turn to the novel L-POSS based high molecular of synthesis and provide wide space, in engineering plastic
The application in the fields such as material, liquid crystal material and dielectric materials is more and more extensive.
China Patent Publication No. is that the application for a patent for invention of CN103044614A employs with a kind of silane coupler modified
The preparation method of acrylate, it introduces silane coupler and is just used to serve as cross-linking agent, and the acrylate obtaining has excellent
Resistance to water and heat stability, but unsatisfactory in the effect of fundamentally its resistance to elevated temperatures, mechanical property and crosslinking, because
This is a kind of possess resistant to elevated temperatures cross-linking agent invention imperative.
Content of the invention
It is an object of the invention to provide a kind of high temperature resistant silane crosslinker containing L-POSS and preparation method thereof, the present invention
Cross-linking agent is the derivant that a kind of cross-linking agent with L-POSS structure also can be considered silane, and the thermostability of crosslinked with silicane can be with
The increase of L-POSS special construction in molecule and improve, the novel crosslinker therefore containing above material can improve common cross-linking agent
Decomposition temperature.
The purpose of the present invention is achieved through the following technical solutions：
A kind of high temperature resistant silane crosslinker containing L-POSS, the structural formula of described high temperature resistant silane crosslinker is as follows：
.
A kind of described high temperature resistant silane crosslinker containing L-POSS, described cross-linking agent contains the resistance to of L-POSS by weight
High temperature silane crosslinker is made up of following components：
Silane：100 parts；
L—POSS：10 ~ 30 parts；
Catalyst：0. 2 ~ 0.3 part；
Initiator：0.2～0.6 part.
A kind of described high temperature resistant silane crosslinker containing L-POSS, described silane crosslinker is coupled for vinyl silanes
At least one in agent, preferred vinyl trimethoxy silane.
A kind of described high temperature resistant silane crosslinker containing L-POSS, described initiator is benzoyl peroxide（BPO）
And cumyl peroxide（DCP）In at least one, preferably benzoyl peroxide.
A kind of described high temperature resistant silane crosslinker containing L-POSS, described L POSS is the class in POSS is trapezoidal
Netted POSS, its architecture formula is as follows.
A kind of described high temperature resistant silane crosslinker containing L-POSS, described catalyst is that tertiary amine compounds include：Three
Ethamine, Tri-n-Propylamine, tri-n-butylamine, N, N- dimethyl butylamine, N, N- diisopropylethylamine, N, N- dimethylaniline, N, N-
Dimethyl cyclohexyl amine, N, N- diethyl cyclohexylamine or N, N- diethylaniline.Preferred catalyst is triethylamine.
A kind of high temperature resistant silane crosslinker preparation method containing L-POSS, methods described includes following preparation process：
It is to form raw material first, next to that introducing L POSS chemical reaction in silane active site to form new cross-linking agent；
（a）On the 250ml there-necked flask equipped with reflux condensing tube, agitator and constant pressure funnel, bath temperature controls
60 DEG C, brine ice reflux cooling, reaction bulb adds 20ml triethoxysilane, a certain amount of solvent and platinum catalyst, acetylene
Purification for gas adjusts flow after being dried and is slowly introducing, and obtains vinyltrimethoxy silane；
（b）Vinyltrimethoxy silane is added the 250ml tri- equipped with reflux condensing tube, agitator and constant pressure funnel
In mouthful flask, be warming up to 60 DEG C more same catalyst of triethylamine, initiator benzoyl peroxide in agitator (2000 turns of speed/
Min stirring 25min in), and be slowly heated, it is warming up to 95 DEG C, L-POSS is added constant pressure funnel and is slowly added dropwise,
It is stirred simultaneously, react 4h；Take out reactant mixture and stop activation 35min, with separatory funnel separation mother solution, obtain lower floor and stick
Thick shape product, this product is placed in 100 DEG C of vacuum drying ovens about 3h is dried, obtain final product.
Advantages of the present invention with effect is：
The novel crosslinker of the present invention is the derivant that a kind of cross-linking agent with L-POSS structure also can be considered silane, crosslinkable silane
The thermostability of connection can improve with the increase of L-POSS special construction in molecule, therefore contains the novel crosslinker of above material
The decomposition temperature of common cross-linking agent can be improved.
Brief description
Fig. 1 is the reaction equation of L-POSS and the high temperature resistant cross-linking agent of synthesis of vinyltrimethoxy silane.
Specific embodiment
With reference to embodiment, the present invention is described in detail.
Embodiment 1：
100 parts of vinyltrimethoxy silanes are added the 250ml equipped with reflux condensing tube, agitator and constant pressure funnel
In there-necked flask, be warming up to 60 DEG C again with 0.25 part of catalyst of triethylamine, 0.4 part of initiator benzoyl peroxide in agitator
Stirring 25min in (2000 turns/min of speed), and be slowly heated, it is warming up to 95 DEG C, 15 parts of L-POSS are added constant voltage to drip
Liquid funnel is simultaneously slowly added dropwise, and is stirred simultaneously, reacts 4h.Take out reactant mixture and stop activation 35min, use separatory funnel
Separate mother solution, obtain lower floor's sticky shape product, this product is placed in 100 DEG C of vacuum drying ovens about 3h is dried, obtain final product
1, its maximum decomposition temperature is 310 ~ 320.
Embodiment 2：
100 parts of vinyltrimethoxy silanes are added the 250ml equipped with reflux condensing tube, agitator and constant pressure funnel
In there-necked flask, be warming up to 60 DEG C again with 0.25 part of catalyst of triethylamine, 0.4 part of initiator benzoyl peroxide in agitator
Stirring 25min in (2000 turns/min of speed), and be slowly heated, it is warming up to 95 DEG C, 20 parts of L-POSS are added constant voltage to drip
Liquid funnel is simultaneously slowly added dropwise, and is stirred simultaneously, reacts 4h.Take out reactant mixture and stop activation 35min, use separatory funnel
Separate mother solution, obtain lower floor's sticky shape product, this product is placed in 100 DEG C of vacuum drying ovens about 3h is dried, obtain final product
2, its maximum decomposition temperature is 320 ~ 330
Embodiment 3：
100 parts of vinyltrimethoxy silanes are added the 250ml equipped with reflux condensing tube, agitator and constant pressure funnel
In there-necked flask, be warming up to 60 DEG C again with 0.25 part of catalyst of triethylamine, 0.4 part of initiator benzoyl peroxide in agitator
Stirring 25min in (2000 turns/min of speed), and be slowly heated, it is warming up to 95 DEG C, 25 parts of L-POSS are added constant voltage to drip
Liquid funnel is simultaneously slowly added dropwise, and is stirred simultaneously, reacts 4h.Take out reactant mixture and stop activation 35min, use separatory funnel
Separate mother solution, obtain lower floor's sticky shape product, this product is placed in 100 DEG C of vacuum drying ovens about 3h is dried, obtain final product
3, its maximum decomposition temperature is 330 ~ 340.
Embodiment 4：
100 parts of vinyltrimethoxy silanes are added the 250ml equipped with reflux condensing tube, agitator and constant pressure funnel
In there-necked flask, be warming up to 60 DEG C again with 0.25 part of catalyst of triethylamine, 0.4 part of initiator benzoyl peroxide in agitator
Stirring 25min in (2000 turns/min of speed), and be slowly heated, it is warming up to 95 DEG C, 30 parts of L-POSS are added constant voltage to drip
Liquid funnel is simultaneously slowly added dropwise, and is stirred simultaneously, reacts 4h.Take out reactant mixture and stop activation 35min, use separatory funnel
Separate mother solution, obtain lower floor's sticky shape product, this product is placed in 100 DEG C of vacuum drying ovens about 3h is dried, obtain final product
4, its maximum decomposition temperature is 340 ~ 350.
During above-mentioned testing result can be seen that this cross-linking agent, reaction condition is gentle, and synthesis technique is simple, and
Understand：Introduce L POSS group on the basis of silane, so that the resistance to heat decomposition temperature of this cross-linking agent is improved, applicable elements model
Enclose bigger.
Above by specific embodiment, the present invention is further illustrated, but these embodiments are only exemplary
, any restriction is not constituted to protection scope of the present invention.It will be appreciated by those skilled in the art that in the spirit without departing from the present invention
In the case of protection domain, technical solutions and their implementation methods of the present invention can be carried out multiple equivalencings, modification or
Improve, these all should fall within the scope of protection of the present invention.Protection scope of the present invention is defined by appended claim.
Claims (7)
1. a kind of high temperature resistant silane crosslinker containing L-POSS it is characterised in that the structural formula of described high temperature resistant silane crosslinker such as
Under：
.
2. a kind of high temperature resistant silane crosslinker containing L-POSS according to claim 1 is it is characterised in that described cross-linking agent
The high temperature resistant silane crosslinker containing L-POSS by weight is made up of following components：
Silane：100 parts；
L—POSS：10 ~ 30 parts；
Catalyst：0. 2 ~ 0.3 part；
Initiator：0.2～0.6 part.
3. a kind of high temperature resistant silane crosslinker containing L-POSS according to claim 1 and 2 is it is characterised in that described silicon
Alkane cross-linking agent is at least one in vinyl silicane coupling agent, preferred vinyl trimethoxy silane.
4. a kind of high temperature resistant silane crosslinker containing L-POSS according to claim 1 and 2 is it is characterised in that described draws
Sending out agent is benzoyl peroxide（BPO）And cumyl peroxide（DCP）In at least one, preferably benzoyl peroxide.
5. a kind of high temperature resistant silane crosslinker containing L-POSS according to claim 1 and 2 is it is characterised in that described L
POSS is the class in POSS is trapezoidal netted POSS, and its architecture formula is as follows.
6. a kind of high temperature resistant silane crosslinker containing L-POSS according to claim 1 and 2 is it is characterised in that described catalysis
Agent is that tertiary amine compounds include：Triethylamine, Tri-n-Propylamine, tri-n-butylamine, N, N- dimethyl butylamine, N, N- diisopropyl second
Amine, N, N- dimethylaniline, N, N- dimethyl cyclohexyl amine, N, N- diethyl cyclohexylamine or N, N- diethylaniline；Preferably
Catalyst is triethylamine.
7. a kind of high temperature resistant silane crosslinker preparation method containing L-POSS is it is characterised in that methods described includes preparing as follows
Journey：
It is to form raw material first, next to that introducing L POSS chemical reaction in silane active site to form new cross-linking agent；
On the 250ml there-necked flask equipped with reflux condensing tube, agitator and constant pressure funnel, bath temperature controls 60
DEG C, brine ice reflux cooling, reaction bulb adds 20ml triethoxysilane, a certain amount of solvent and platinum catalyst, acetylene gas
Body purification adjusts flow after being dried and is slowly introducing, and obtains vinyltrimethoxy silane；
Vinyltrimethoxy silane is added the tri- mouthfuls of burnings of 250ml equipped with reflux condensing tube, agitator and constant pressure funnel
Bottle in, be warming up to 60 DEG C more same catalyst of triethylamine, initiator benzoyl peroxide in agitator (2000 turns/min of speed)
Middle stirring 25min, and be slowly heated, it is warming up to 95 DEG C, L-POSS is added constant pressure funnel and is slowly added dropwise, enter simultaneously
Row stirring, reacts 4h；Take out reactant mixture and stop activation 35min, with separatory funnel separation mother solution, obtain the sticky shape of lower floor and produce
Thing, this product is placed in 100 DEG C of vacuum drying ovens about 3h is dried, obtain final product.
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| CN201610809803.0A CN106397775B (en) | 2016-09-08 | 2016-09-08 | A kind of high temperature resistant silane crosslinker and preparation method thereof containing L-POSS |
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| CN201610809803.0A CN106397775B (en) | 2016-09-08 | 2016-09-08 | A kind of high temperature resistant silane crosslinker and preparation method thereof containing L-POSS |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109749128A (en) * | 2018-12-10 | 2019-05-14 | 沈阳化工大学 | A kind of high temperature resistant silane crosslinker and preparation method thereof containing triphenylphosphonium chloride |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08325455A (en) * | 1995-05-31 | 1996-12-10 | Nec Corp | Silicon-containing polymer compound and photosensitive resin composition |
| JP3115928B2 (en) * | 1992-02-10 | 2000-12-11 | 旭化成工業株式会社 | Silicone compound, vinyl copolymer thereof, and coating composition using the same |
-
2016
- 2016-09-08 CN CN201610809803.0A patent/CN106397775B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3115928B2 (en) * | 1992-02-10 | 2000-12-11 | 旭化成工業株式会社 | Silicone compound, vinyl copolymer thereof, and coating composition using the same |
| JPH08325455A (en) * | 1995-05-31 | 1996-12-10 | Nec Corp | Silicon-containing polymer compound and photosensitive resin composition |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109749128A (en) * | 2018-12-10 | 2019-05-14 | 沈阳化工大学 | A kind of high temperature resistant silane crosslinker and preparation method thereof containing triphenylphosphonium chloride |
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Application publication date: 20170215 Assignee: SHENYANG XINFEIYU RUBBER PRODUCTS CO.,LTD. Assignor: SHENYANG University OF CHEMICAL TECHNOLOGY Contract record no.: X2023210000283 Denomination of invention: A high-temperature resistant silane crosslinking agent containing L-POSS and its preparation method Granted publication date: 20190621 License type: Common License Record date: 20231205 |
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