CN103834172B - Low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber and preparation method thereof - Google Patents
Low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber and preparation method thereof Download PDFInfo
- Publication number
- CN103834172B CN103834172B CN201410066445.XA CN201410066445A CN103834172B CN 103834172 B CN103834172 B CN 103834172B CN 201410066445 A CN201410066445 A CN 201410066445A CN 103834172 B CN103834172 B CN 103834172B
- Authority
- CN
- China
- Prior art keywords
- alpha
- parts
- low
- room temperature
- modification
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to a kind of low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber and preparation method thereof, this silicon rubber is made up of the component of following mass fraction: the α of modification, 100 parts of alpha, omega-dihydroxy polydimethyl siloxanes; 10 ~ 40 parts of Alpha-hydroxy-ω-methyl dimethyl silicone polymers of modification; 10 ~ 20 parts of inorganic functional fillers; 3 ~ 10 parts of fume colloidal silicas; 0.5 ~ 2 part of carbon black; 1 ~ 5 part of fumed titanium dioxide; 1 ~ 15 part of crosslinking agent; 1 ~ 10 part of titanate catalyst; 0 ~ 5 part of silane coupler; The present invention has improved processing characteristics, the storge quality of titanate esters catalyst system and catalyzing, can prepare low viscous silicon rubber; Filler and silicon rubber Miscibility, color homogeneity and storage stability and electrical property are improved; Realize UL94-V0 rank fire-retardant, when burning, do not discharge any toxic gas; Lower, the viscosity adjustable extent of silicon rubber density of preparation is wider, cost is lower, corrosion-free to contact material, meets the requirement of electronic enterprises.
Description
Technical field
The present invention relates to high molecule sealing materials field, especially relate to the one-component titanate esters catalysis room temperature of halogen-free flameproofSulphurated siliastic and preparation method thereof.
Background technology
The vulcanization reaction of single-component room-temperature vulcanized silicone rubber is by having an effect and be sulfided into elasticity with airborne moistureBody. Along with the difference of crosslinking agent, can be divided into depickling type, de-oxime type, dealcoholized type, de-amine type, de amide type and deacetone etc. perhapsMany kinds. Different with additive according to the filler adding, there is different density, viscosity, mobility and thixotropy, show notWith property as heat-resisting, heat conduction, resistance to ablation, fire-retardant, conduction etc., thereby be applied to different industry fields.
Wherein, at electronic enterprises, with the raising of its development and environmental requirement, to for the protection of certain of electric appliance and electronicA little organic silicon sealant performance requirements are further strict: first silicon rubber does not have to components and parts such as electronic apparatus the valency that burn into is lowerLattice and excellent ageing properties; Next require UL94-V0 rank fire-retardant and not halogen-containing, require compared with low-density and sticky simultaneouslyDegree; Finally, European Union has put into effect the following organotin use of some regulation limitations. Integration requirement and following developments, adopt titaniumThe separating methanol system of acid esters catalysis, can meet the restriction such as price, European Union's regulation requirement. And currently available technology realizes Halogen resistanceCombustion generally has following mode: 1) nitrogen-phosphorus expansion sex flame retardant is as polyphosphate, APP, red phosphorus, melamine, phosphorous acidEsters etc., can affect storage characteristics but be applied in single-component room temperature vulcanized silicon rubber; 2) platinum element/carbon black based flame retardant, can urgeEnter into carbon, and form insulating barrier, stop heat transmission and fire-retardant, but platinum price is high; 3) such as aluminium hydroxide, hydroxideMagnesium, basic zinc carbonate etc. can pyrolytic produce the material of water, inert gas, can absorb heat reduce material surface temperature,Form barrier layer and stop heat transmission, but adopt inorganic filler to realize the fire-retardant high filler loading capacity that needs of V0, cause density and viscosity highAnd inorganic filler meeting is separated with base glue.
Therefore, up to now, how to realize Halogen, low-density, UL94-V0 fire-retardant and not containing the stable storing of organotinTitanate esters system silicon rubber is a problem in the urgent need to address.
It is little, corrosion-free and not stanniferous to contact material that titanate esters dealcoholized type flame-proof silicon rubber has smell, at electronic apparatusIndustry is widely applied. But need the fire-retardant filler of high filler loading capacity to realize halogen-free flameproof, this can cause occurring viscosity high,The adverse effect such as processing characteristics is bad, filler and base glue are separated.
Summary of the invention
The object of this invention is to provide a kind of low-density, halogen-free, titanate esters catalysis and there is high efficiency flame retardanceThe preparation method of organic silicon rubber and this organic silicon rubber; Provide a kind of solution inorganic filler compatible with organosilicon system simultaneouslyThe method of property.
In order to realize object of the present invention, a kind of low-density halogen-free flameproof one pack system titanate esters catalyst chamber temperature vulcanizable silicone is proposedRubber, described silicon rubber is made up of the component of following mass fraction:
The α of modification, 100 parts of alpha, omega-dihydroxy polydimethyl siloxanes;
10 ~ 40 parts of Alpha-hydroxy-ω-methyl dimethyl silicone polymers of modification;
10 ~ 20 parts of inorganic functional fillers;
3 ~ 10 parts of fume colloidal silicas;
0.5 ~ 2 part of carbon black;
1 ~ 5 part of fumed titanium dioxide;
1 ~ 15 part of crosslinking agent;
1 ~ 10 part of titanate catalyst;
0 ~ 5 part of silane coupler;
The α of described modification, alpha, omega-dihydroxy polydimethyl siloxane is the material with following structure:
Structural formula I
Wherein n=200 ~ 1000, viscosity 0.5Pas ~ 20Pas 25 DEG C time;
Described modification Alpha-hydroxy-ω-methyl dimethyl silicone polymer is to have following structural material:
Structural formula II
Wherein n=5 ~ 100, viscosity 2mPas ~ 100mPas 25 DEG C time;
Described inorganic functional filler comprises aluminium hydroxide, aluminium oxide, magnesium hydroxide, magnesium carbonate, zinc carbonate, hydroxideZinc, basic zinc carbonate, Firebrake ZB, calcium carbonate, red phosphorus, APP one or more mixtures wherein;
Described fume colloidal silica is the vapor phase method hard charcoal through HMDS or dimethyldichlorosilane processingBlack, specific area is 100 ~ 300 ㎡/g;
Described carbon black is contact method or furnace black;
Described fumed titanium dioxide is untreated, and specific area is 100 ~ 300 ㎡/g;
Described crosslinking agent is tetramethoxy-silicane, vinyltrimethoxy silane, MTMS, propyl group front threeOne or more in TMOS, anilinomethyl trimethoxy silane;
Described silane coupler is amino silane coupler, 3-glycidyl ether oxygen propyl trimethoxy silicane, sulfydrylThe reactant of one or more coupling agents in one type of silane coupling agent, isocyanates silane coupler;
Described inorganic functional filler is preferably untreated aluminium hydroxide, and particle diameter is 4000 ~ 7000 orders.
Described carbon black is preferably the acetylene method carbon black in furnace black, and specific area is 50 ~ 100 ㎡/g.
Described catalyst is preferably the ethyl acetoacetate chelate of isopropyl titanate.
Described crosslinking agent is preferably methyl trimethoxy oxosilane.
Described silane coupler is preferably the reactant of amino silane coupler and epoxies silane coupler.
The present invention also proposes the preparation of described low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubberMethod, comprises step:
(1) modified alpha, the preparation of alpha, omega-dihydroxy polydimethyl siloxane:
Appropriate viscosity α, alpha, omega-dihydroxy polydimethyl siloxane, end capping reaction catalyst, tetramethoxy-silicane are by certain matterAmount is than adding reaction attached middle school, at N2In atmosphere, 120-150 DEG C of stirring reaction 4 ~ 8h, then at 100 DEG C, be greater than-0.09MPa is trueUnder empty condition, heat 1 ~ 2h and remove excessive tetramethoxy-silicane and other low-boiling-point substances, remove by filter catalysis after being then down to room temperatureAgent;
(2) preparation of the Alpha-hydroxy-ω of modification-methyl dimethyl silicone polymer:
Appropriate viscosity Alpha-hydroxy-ω-methyl dimethyl silicone polymer, end capping reaction catalyst, tetramethoxy-silicane are by oneDetermine mass ratio and add reaction attached middle school, at N2In atmosphere, 120-150 DEG C of stirring reaction 4 ~ 8h,, then at 100 DEG C, be greater than-Under 0.09MPa vacuum condition, heat 1 ~ 2h and remove excessive tetramethoxy-silicane and other low-boiling-point substances, be then down to mistake after room temperatureFilter catalyst;
(3) surface modification treatment of filler:
10 ~ 40 parts of Alpha-hydroxy-ω-methyl dimethyl silicone polymers of the modification of above-mentioned preparation, inorganic functional filler 10 ~ 201 ~ 5 part of part, 0.5 ~ 2 part of carbon black, fumed titanium dioxide add in high speed dispersion mixer, in be greater than-0.09MPa of vacuum barUnder part, mix, then, after nitrogen vacuum breaker, under nitrogen protection, stirring reaction 1 ~ 2h under 100 ~ 130 DEG C of conditions, then in thisUnder be greater than-0.09MPa of temperature and vacuum condition, remove low-boiling-point substance and realize the surface modification to filler;
(4) by 110 DEG C ~ 130 DEG C drying and dewaterings of fume colloidal silica 3 ~ 5 hours;
(5), under room temperature, in the filler systems of modification, add the α of above-mentioned modification, alpha, omega-dihydroxy polydimethyl siloxane 100Part, in vacuum > stir 10 ~ 15min under-0.09MPa condition; Add 3 ~ 10 parts of fume colloidal silicas, in vacuum >-Stirring reaction 15 ~ 20min under 0.09MPa condition; Add 1 ~ 15 part of crosslinking agent, 1 ~ 10 part of catalyst, 0 ~ 5 part of silane coupler,In vacuum > stirring reaction 30min ~ 60min obtains the catalysis of low-density halogen-free flameproof one pack system titanate esters under-0.09MPa conditionRoom temperature vulcanized silicone rubber.
The present invention be mainly realize preparation not halogen-containing, low-density, low viscosity, processing characteristics is good, storge quality is goodWithout being separated and meeting the dealcoholized type room temperature vulcanized silicone rubber of the indices of RoHS and REACH.
Main feature is the α that adopts modification, and alpha, omega-dihydroxy polydimethyl siloxane is the α-hydroxyl of base polymer, modificationBase-ω-methyl dimethyl silicone polymer, inorganic functional filler, crosslinking agent, fume colloidal silica, carbon black, vapor phase method titanium dioxideTitanium, coupling agent, catalyst etc. carry out chemical reaction in high speed dispersion stirred tank under vacuum condition, preparation anti-flammability alcohol typeSilicon rubber. It has excellent flame retardancy energy, electric property, storage stability, has especially realized low-density fire-retardant and improved and fill outThe compatibility of material and base glue.
In the present invention, adopt the compositional flame-retardant system of inorganic functional filler, titanium-containing compound, carbon black composition, in combustion processIn, low-temperature region is divided heat of desorption and produced inert gas blocking oxygen by inorganic functional filler to be realized fire-retardant; Middle high-temperature area titaniumElement can be induced into carbon, carbon black increase becomes carbon efficiencies and realizes fire-retardant; The crystal transfer heat absorption of high-temperature area titanium dioxide, simultaneouslyOrganosilicon self can produce that fine and close silica stops the degraded of thermal oxide and fire-retardant.
Beneficial effect of the present invention:
(1) use the α of modification, alpha, omega-dihydroxy polydimethyl siloxane, has improved the processability of titanate esters catalyst system and catalyzingEnergy, storge quality, can prepare low viscous silicon rubber;
(2) use Alpha-hydroxy-ω-methyl dimethyl silicone polymer of modification to inorganic functional filler, carbon black, vapor phase methodTitanium dioxide carries out surface treatment, has improved the flame retarding efficiency of filler, has improved filler and silicon rubber Miscibility, color is equalEven property and storage stability and electrical property;
(3) the present invention hinders by the composite UL94-V0 rank that realizes of inorganic functional filler, titanium-containing compound and carbon blackCombustion, simultaneously filling adding amount few, there is no halogen, high, the fire-retardant good stability of flame retarding efficiency, and do not discharge any poison gas that has when burningBody;
(4) compared with prior art, the silicon rubber density of preparation is lower, viscosity adjustable extent is wider, cost is lower, andFor Wuxi separating methanol curing system, corrosion-free to contact material, can to meet RoHS and REACH indices, meets European UnionEtc. standard, meet the requirement of electronic enterprises.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, to thisBright further description.
Embodiment 1
The α of modification, the preparation of alpha, omega-dihydroxy polydimethyl siloxane
At N2Under protection, by the α of 1000 parts of 1500mPas, alpha, omega-dihydroxy polydimethyl siloxane, 100 parts of tetramethyl oxygen5 parts of base silanes, end-blocking catalyst carbonic acid calcium (or zinc carbonate, zinc oxide) add in reaction vessel, stirring reaction 6h at 130 DEG C(according to the different of end capping reaction catalyst and add the difference of tetramethoxy-silicane amount, those skilled in the art can be to reactionTemperature, time are carried out suitable adjustment), then at 100 DEG C, vacuum > under-0.09MPa condition, extract low-boiling-point substance and excessiveTetramethoxy-silicane, obtain the α that structural formula is the modification of I, alpha, omega-dihydroxy polydimethyl siloxane.
Embodiment 2
The preparation of Alpha-hydroxy-ω-methyl dimethyl silicone polymer of modification
At N2Under protection, by Alpha-hydroxy-ω of 500 parts of 50mPas-methyl dimethyl silicone polymer, 100 parts of tetramethyl oxygen5 parts of base silanes, end-blocking catalyst carbonic acid calcium (or zinc carbonate, zinc oxide) add in reaction vessel, stirring reaction 6h at 130 DEG C(according to the different of end capping reaction catalyst and add the difference of tetramethoxy-silicane amount, those skilled in the art can be to reactionTemperature, time are carried out suitable adjustment), then at 100 DEG C, vacuum > under-0.09MPa condition, extract low-boiling-point substance and excessiveTetramethoxy-silicane, obtain Alpha-hydroxy-ω that structural formula is the modification of II-methyl dimethyl silicone polymer.
Embodiment 3
200 parts of Alpha-hydroxy-ω-methyl dimethyl silicone polymers of modification, 150 parts, aluminium hydroxide, 10 parts of acetylene carbon blacks, gas20 parts of phase method titanium dioxide add in high speed dispersion mixer, in vacuum > mix under-0.09MPa condition, then nitrogen is broken trueAfter sky, under nitrogen protection, stirring reaction 2h under 120 DEG C of conditions, then in this temperature and vacuum > under-0.09MPa conditionAfter removing low-boiling-point substance, be cooled to room temperature, nitrogen vacuum breaker, adds the α of above-mentioned modification, alpha, omega-dihydroxy polydimethyl siloxane 1000Part, in vacuum > stir 10min under-0.09MPa condition; Add again 40 parts of fume colloidal silicas, in vacuum >-0.09MPaUnder condition, stir 15min; Finally add the ethyl acetoacetate chelate 20 of 30 parts of MTMSs, isopropyl titanate(aminopropyl triethoxysilane and glycidoxy-propyltrimethoxy silane are anti-according to 1:2.5 mol ratio for part, silane couplerAnswer thing) 10 parts, in vacuum > stirring reaction 40min under-0.09MPa condition, obtain low-density halogen-free flameproof one pack system titanate estersCatalysis room temperature vulcanized silicone rubber, this product performance index is described in detail as table one.
Embodiment 4
Except adding 180 parts, acetylene carbon black, aluminium hydroxide add 15 parts, fumed titanium dioxide to add 10 especially, other worksSkill and composition addition, with embodiment 3, obtain low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber, this productProduct performance indications are described in detail as table one
Embodiment 5
Except adding 120 parts, acetylene carbon black, aluminium hydroxide add 10 parts, fumed titanium dioxide to add 40 especially, other worksSkill and composition addition, with embodiment 3, obtain low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber, this productProduct performance indications are described in detail as table one
Embodiment 6
Except Alpha-hydroxy-ω-methyl dimethyl silicone polymer addition of modification is 350 parts, other techniques and composition addAmount, with embodiment 3, obtains low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber, and this product performance index is detailedCarefully describe as table one.
Comparative example 1
Except not adding acetylene carbon black, other techniques and composition addition, with embodiment 3, obtain the properties of product of silicon rubberIndex is described in detail as table one.
Comparative example 2
Except not adding fumed titanium dioxide, other techniques and composition addition, with embodiment 3, obtain the product of silicon rubberProduct performance indications are described in detail as table one.
Comparative example 3
Except not adding aluminium hydroxide, other techniques and composition addition, with embodiment 3, obtain the properties of product of silicon rubberIndex is described in detail as table one.
Comparative example 4
Identical with composition and the addition of embodiment 3, prepare according to following process: the Alpha-hydroxy-ω-methyl of modification20 parts of 200 parts of dimethyl silicone polymers, 150 parts, aluminium hydroxide, 10 parts of acetylene carbon blacks, fumed titanium dioxide add high speed dispersionIn mixer, in vacuum > mix under-0.09MPa condition, then after nitrogen vacuum breaker, under nitrogen protection, add modificationα, 1000 parts of alpha, omega-dihydroxy polydimethyl siloxanes, in vacuum > stir 10min under-0.09MPa condition; Add again vapor phase method40 parts of white carbons, in vacuum > stir 15min under-0.09MPa condition; Finally add 30 parts of MTMSs, metatitanic acid20 parts of the ethyl acetoacetate chelates of isopropyl ester, silane coupler (aminopropyl triethoxysilane and epoxypropoxy threeMethoxy silane is according to the reactant of 1:2.5 mol ratio) 10 parts, in vacuum > stirring reaction 40min under-0.09MPa condition,The product performance index that obtains silicon rubber is described in detail as table one
Low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber prepared by said method, by GB/T-13477 its surface drying times of test, GBT1410-2006 test volume resistivity, UL-94 standard testing flame retardant rating, density agar diffusion methodViscosity when density, plate viscometer method are tested 25 DEG C while testing 25 DEG C. Storage stability method of testing: by airtight good uncuredSilicon rubber is put into 70 DEG C of baking oven 168h, takes out to be cooledly to room temperature, tests respectively surface drying time, viscosity, resistance by above-mentioned standardCombustion grade, specific insulation. After putting into two 85 (85% humidity/85 DEG C) baking oven 1000h, gets by film after investigation is simultaneously solidifiedGo out, be placed to after room temperature by above-mentioned standard testing flame retardant rating, specific insulation, characterize weather resistance.
Claims (7)
1. a low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber, is characterized in that described silicon rubberComponent by following mass fraction forms:
The α of modification, 100 parts of alpha, omega-dihydroxy polydimethyl siloxanes;
10 ~ 40 parts of Alpha-hydroxy-ω-methyl dimethyl silicone polymers of modification;
10 ~ 20 parts of inorganic functional fillers;
3 ~ 10 parts of fume colloidal silicas;
0.5 ~ 2 part of carbon black;
1 ~ 5 part of fumed titanium dioxide;
1 ~ 15 part of crosslinking agent;
1 ~ 10 part of titanate catalyst;
0 ~ 5 part of silane coupler;
The α of described modification, alpha, omega-dihydroxy polydimethyl siloxane is the material with following structure:
Structural formula I
Wherein n=200 ~ 1000, viscosity 0.5Pas ~ 20Pas 25 DEG C time;
Alpha-hydroxy-ω-methyl dimethyl silicone polymer of described modification is the material with following structure:
Structural formula II
Wherein n=5 ~ 100, viscosity 2mPas ~ 100mPas 25 DEG C time;
Described inorganic functional filler is selected from aluminium hydroxide, aluminium oxide, magnesium hydroxide, magnesium carbonate, zinc carbonate, zinc hydroxide, alkaliThe mixture of one or more in formula zinc carbonate, Firebrake ZB, calcium carbonate, red phosphorus, APP;
Described fume colloidal silica is the fume colloidal silica through HMDS or dimethyldichlorosilane processing, thanSurface area is 100 ~ 300 ㎡/g;
Described carbon black is contact method or furnace black;
Described fumed titanium dioxide is untreated, and specific area is 100 ~ 300 ㎡/g;
Described crosslinking agent is tetramethoxy-silicane, vinyltrimethoxy silane, MTMS, propyl trimethoxyOne or more in silane, anilinomethyl trimethoxy silane;
Described silane coupler is amino silane coupler, 3-glycidyl ether oxygen propyl trimethoxy silicane, sulfydryl eka-siliconThe reactant of one or more coupling agents in alkane coupling agent, isocyanates silane coupler.
2. low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber according to claim 1, its featureBe, described inorganic functional filler is untreated aluminium hydroxide, and particle diameter is 4000 ~ 7000 orders.
3. low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber according to claim 2, its featureBe, described carbon black is the acetylene method carbon black in furnace black, and specific area is 50 ~ 100 ㎡/g.
4. low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber according to claim 1, its featureBe the ethyl acetoacetate chelate that described titanate catalyst is isopropyl titanate.
5. low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber according to claim 4, its featureBe, described crosslinking agent is methyl trimethoxy oxosilane.
6. low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber according to claim 5, its featureBe, described silane coupler is the reactant of amino silane coupler and epoxies silane coupler.
7. the low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber as described in any one in claim 1-6Preparation method, comprise step:
(1) modified alpha, the preparation of alpha, omega-dihydroxy polydimethyl siloxane:
Appropriate viscosity α, alpha, omega-dihydroxy polydimethyl siloxane, end capping reaction catalyst, tetramethoxy-silicane are pressed certain mass ratioAdd in reactor, at N2In atmosphere, 120-150 DEG C of stirring reaction 4 ~ 8h, then at 100 DEG C, be greater than-0.09MPa vacuum barUnder part, heat 1 ~ 2h and remove excessive tetramethoxy-silicane and other low-boiling-point substances, remove by filter catalyst after being then down to room temperature;
(2) preparation of the Alpha-hydroxy-ω of modification-methyl dimethyl silicone polymer:
Appropriate viscosity Alpha-hydroxy-ω-methyl dimethyl silicone polymer, end capping reaction catalyst, tetramethoxy-silicane are by certain matterAmount is than adding in reactor, at N2In atmosphere, 120-150 DEG C of stirring reaction 4 ~ 8h, then at 100 DEG C, be greater than-0.09MPa is trueUnder empty condition, heat 1 ~ 2h and remove excessive tetramethoxy-silicane and other low-boiling-point substances, remove by filter catalysis after being then down to room temperatureAgent;
(3) surface modification treatment of filler:
10 ~ 40 parts of Alpha-hydroxy-ω-methyl dimethyl silicone polymers of the modification of above-mentioned preparation, 10 ~ 20 parts of inorganic functional fillers,1 ~ 5 part of 0.5 ~ 2 part of carbon black, fumed titanium dioxide add in high speed dispersion mixer, in vacuum > mixed under-0.09MPa conditionEven, then after nitrogen vacuum breaker, under nitrogen protection, stirring reaction 1 ~ 2h under 100 ~ 130 DEG C of conditions, then in this temperature andVacuum > remove low-boiling-point substance and realize the surface modification to filler under-0.09MPa condition;
(4) by 110 DEG C ~ 130 DEG C drying and dewaterings of fume colloidal silica 3 ~ 5 hours;
(5), under room temperature, in the filler systems of modification, add the α of above-mentioned modification, 100 parts of alpha, omega-dihydroxy polydimethyl siloxanes, inVacuum > stir 10 ~ 15min under-0.09MPa condition; Add 3 ~ 10 parts of fume colloidal silicas, in vacuum >-0.09MPa barStirring reaction 15 ~ 20min under part; Add 1 ~ 15 part of crosslinking agent, 1 ~ 10 part of titanate catalyst, 0 ~ 5 part of silane coupler, Yu ZhenReciprocal of duty cycle > stirring reaction 30min ~ 60min obtains low-density halogen-free flameproof one pack system titanate esters catalysis room temperature under-0.09MPa conditionSulphurated siliastic.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410066445.XA CN103834172B (en) | 2014-02-26 | 2014-02-26 | Low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410066445.XA CN103834172B (en) | 2014-02-26 | 2014-02-26 | Low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103834172A CN103834172A (en) | 2014-06-04 |
| CN103834172B true CN103834172B (en) | 2016-05-18 |
Family
ID=50798084
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410066445.XA Active CN103834172B (en) | 2014-02-26 | 2014-02-26 | Low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103834172B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BR112017015276B1 (en) * | 2015-01-28 | 2022-09-06 | Dow Corning Corporation | GEL, CONDENSATION-CURABLE GEL COMPOSITION, METHOD OF MANUFACTURING A GEL, AND, USE OF A GEL |
| CN106084236B (en) * | 2016-06-06 | 2018-12-11 | 武汉大学 | A kind of room temperature vulcanized sili cone rubber and its crosslinking agent |
| CN109749453B (en) * | 2018-12-28 | 2021-06-22 | 广州市白云化工实业有限公司 | Titanate catalytic composition, preparation method and application thereof |
| CN114716968A (en) * | 2022-03-28 | 2022-07-08 | 老树根实业有限公司 | Organic silicon adhesive and production process thereof |
| CN115991875B (en) * | 2023-02-15 | 2023-12-15 | 杭州之江有机硅化工有限公司 | Titanate catalyst for dealcoholized room temperature vulcanized silicone rubber and preparation method thereof |
| CN116376028A (en) * | 2023-05-22 | 2023-07-04 | 江苏至昕新材料有限公司 | Powder surface treating agent and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002240A (en) * | 2010-11-22 | 2011-04-06 | 绵阳惠利电子材料有限公司 | Flame-retardant dealcoholization type room-temperature curing silicon rubber |
| CN102757647A (en) * | 2012-07-11 | 2012-10-31 | 东莞兆舜有机硅新材料科技有限公司 | Single-component catalytic dealcoholized room temperature vulcanized (RTV) silicone rubber and preparation method thereof |
-
2014
- 2014-02-26 CN CN201410066445.XA patent/CN103834172B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002240A (en) * | 2010-11-22 | 2011-04-06 | 绵阳惠利电子材料有限公司 | Flame-retardant dealcoholization type room-temperature curing silicon rubber |
| CN102757647A (en) * | 2012-07-11 | 2012-10-31 | 东莞兆舜有机硅新材料科技有限公司 | Single-component catalytic dealcoholized room temperature vulcanized (RTV) silicone rubber and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103834172A (en) | 2014-06-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103834172B (en) | Low-density halogen-free flameproof one pack system titanate esters catalysis room temperature vulcanized silicone rubber and preparation method thereof | |
| CN101735619B (en) | Halogen-free flame-retarded heat-conducting organic silicon electronic potting adhesive and preparation method thereof | |
| CN103265813B (en) | Foaming type encapsulating silica gel composition | |
| CN102002240B (en) | Flame-retardant dealcoholization type room-temperature curing silicon rubber | |
| CN103131381B (en) | High-performance environmentally-friendly flame retardant type organic electron pouring sealant and preparation method thereof | |
| CN103146340B (en) | Low-viscosity high-heat-conductivity organic silicon electronic pouring sealant and preparation method thereof | |
| CN104031389B (en) | Moisture-proof heat type room temperature silicon sulfide rubber composition | |
| CN103044922A (en) | Halogen-free flame retardant, high-temperature resisting and rapidly solidified deacetone silicon rubber and preparation method thereof | |
| CN101985550A (en) | One-component room temperature vulcanizing silicone fireproof sealant and preparation method thereof | |
| CN102977613B (en) | Method for preparing halogen-free and flame-retardant silicon rubber | |
| CN103865271A (en) | Nano hybrid material modified organosilicone heat-conductive electronic pouring sealant and preparation method of sealant | |
| WO2013017090A1 (en) | Halogen-free flame-retardant addition type organosilicon encapsulant for electronic appliances | |
| CN104804705A (en) | Low release quantity additive halogen-free flame-retardant heat-conduction organic silicon pouring sealant and preparation method thereof | |
| CN103351627A (en) | Addition type heat-conducting silicon rubber and preparation method thereof | |
| CN102675882A (en) | Addition type heat-conducting anti-settling silicon rubber and preparation method thereof | |
| CN103694949A (en) | Halogen-free flame retardant heat-conducting organic silicon sealing material for solar photovoltaic module and preparation of material | |
| CN110591382A (en) | Low-density halogen-free flame-retardant graphene heat-conducting silica gel and preparation method thereof | |
| CN106147698A (en) | Photovoltaic component terminal box heat conductive flame-retarding organic silicon potting adhesive and preparation method | |
| CN108912688A (en) | A kind of new energy car battery Embedding Material and preparation method thereof | |
| CN110591378A (en) | Closed-cell organic silicon foaming adhesive and preparation method thereof | |
| CN109096471A (en) | A kind of novel P-N-Si cooperative resistance combustion epoxy curing agent and preparation method thereof | |
| CN111876129A (en) | Low-density high-heat-conductivity pouring sealant | |
| JP4255088B1 (en) | Hybrid composition | |
| CN113462165A (en) | Heat-conducting organic silicon pouring sealant for inverter inductor and preparation method thereof | |
| CN110204900B (en) | Flame-retardant organopolysiloxane composition and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C53 | Correction of patent for invention or patent application | ||
| CB02 | Change of applicant information |
Address after: 100041 Beijing City, Shijingshan District Badachu high tech Park Park Road No. 5 Applicant after: BEIJING TIANSHAN NEW MATERIAL TECHNOLOGY CO., LTD. Address before: 100041, No. 7 middle Garden Road, Badachu hi tech park, Beijing, Shijingshan District Applicant before: Beijing TONSAN Adhesive Co., Ltd. |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: APPLICANT; FROM: BEIJING TONSAN ADHESIVE CO., LTD. TO: BEIJING TIANSHAN NEW MATERIAL TECHNOLOGY CO., LTD. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |