CN104371107A - Hydrogen-containing MQ silicon resin and preparation method thereof - Google Patents
Hydrogen-containing MQ silicon resin and preparation method thereof Download PDFInfo
- Publication number
- CN104371107A CN104371107A CN201410588673.3A CN201410588673A CN104371107A CN 104371107 A CN104371107 A CN 104371107A CN 201410588673 A CN201410588673 A CN 201410588673A CN 104371107 A CN104371107 A CN 104371107A
- Authority
- CN
- China
- Prior art keywords
- parts
- preparation
- hydrogeneous
- hexamethyldisiloxane
- silicone resin
- 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.)
- Pending
Links
Landscapes
- Silicon Polymers (AREA)
Abstract
The invention provides a hydrogen-containing MQ silicon resin with a general formula of [(CH3)2HSiO1/2]a[(CH3)3SiO1/2]b[SiO2]c, wherein M/Q is 0.6-0.9. The invention also provides a preparation method of the hydrogen-containing MQ silicon resin, comprising the following steps: uniformly mixing and stirring a monofunctional monomer, a catalyst, water and a cosolvent, wherein the monofunctional monomer comprises tetramethyldisiloxane and hexamethyldisiloxane, and the catalyst is acid; adding tetraethoxysilane at room temperature in five minutes with vigorous stirring, and reacting for 1-3 hours; and then neutralizing with an alkali, extracting with an extracting agent for layering, and performing reduced pressure dehydration on an extract to obtain the hydrogen-containing MQ silicon resin. By adopting the preparation method disclosed by the invention, the hydrogen-containing MQ resin is prepared by using a tetraethoxysilane method, various powdery and fluidic MQ resins and an MQ resin with different H contents can be prepared by adjusting M/Q, and the hydrogen-containing MQ silicon resin is mainly used for crosslinking agents and reinforcing agents containing molding rubber, can achieve a satisfactory effect, and has the advantages of convenience in operation, readily available raw materials, easy control, short time and the like.
Description
Technical field
The invention belongs to polymeric material field, be specifically related to a kind of hydrogeneous MQ silicone resin and preparation method thereof.
Background technology
Silicone resin is the thermoset organopolysiloxane system (performed polymer) with highly cross-linked structure.Its preparation method is raw material usually with organosilicon, and by hydrolysis, condensation, reset, can make and there is directly link active gene on the silicon atoms, as the resin of hydroxyl, hydrogen atom, alkoxyl group, vinyl, phenyl etc., in order to shelf-stable and application convenience, most of product is all dissolved in the inert organic solvents such as toluene or dimethylbenzene and is sold with varnish.
Silicone resin possesses splendid various character, as thermotolerance, weathering resistance, electrical insulating property, chemical resistant properties, hydrophobicity, cementability and flame retardant resistance etc.In addition, other resins can also be obtained by modification, as modifications such as vinylformic acid, phenolic aldehyde, epoxies.Therefore, they can be widely used in insulation protection material material alive, resistance to combustion, weather-proof, corrosion resistant material (coating), metal protective coating; waterproof construction, moisture-proof coating, optical coating; releasing agent, tackiness agent, the fields such as semiconductor package coatings and packaging electronic components.
Hydrogeneous MQ is the one in MQ, and it has on the SI-H key of hyperergy and chain and has (SIO
2) key band, so can by with CH
2=CH-double bond ,-OH etc. carry out the crosslinking reaction such as addition and condensation, also can make the chemical meending material of silicon rubber, can be obtained the silicone resin of various functional activity in the scope of broadness by silicon oxidation, silanization, SI-H key wherein can also and C
6h
10o
2cH in (allyl glyceroether)
2=CH-reaction generates the tackifier with epoxy group(ing), and it can store at ambient temperature.
At present, for the preparation method of hydrogeneous MQ silicone resin usually based on the cohydrolysis of silane, condensation.
The US20060081864A1 of Waoker Chemie GmbH discloses hydrogeneous MQ silicone resin by will containing the chlorosilane of Si-OH, alkyl oxosilane, H at low temperatures
2o and sulfuric acid reaction, to equilibrium state, then add toluene/water to mixture and neutralize by being separated, and decompression is except low molecule.
The CN101295032A of Shix.Etsu Chemical Co.Ltd discloses hydrogeneous MQ silicone resin and passes through phenyl chlorosilane, dissolve in toluene by the linear silicone oils of Si-Cl gene end-blocking with containing silicon hydride chlorid, gained solution is dripped in water again and is hydrolyzed, condensation, wash with water, alkali cleaning neutralise mixt, decompression is de-low obtained.
The CN98806411.1 of Allied Signal lnc discloses and promotes that the cohydrolysis-condensation reaction of hydrogenation three halosilanes monomer and organic three halosilanes obtains Organhydridosiloxaneresins resins by two phase solvent system (i.e. the mixture of nonpolar, polar solvent and water) and solid catalyst, more after filtration and de-low and obtained.
But above-mentioned method for making runs into numerous technical problems, as reaction conditions is difficult to control controls of being also careful such as () temperature of reaction, time, stirring, speed; Method is complicated, and have a large amount of product purification steps complicated, difficulty gives preparation, and difficulty gives preparation high molecular, the hydrogeneous MQ silicone resin of high transmission rate.Due to side reaction particularly gel reaction, will transmittance be caused to decline in hydrogeneous MQ silicone resin preparation process, thus limit its range of application; Circulation ratio is not good, and the product property difficulty of different batches gives prediction etc.
The people such as Li Zhiming use hydroxyl silicone resin, various containing hydrogen silicone oil (high hydrogeneous and higher containing hydrogen silicone oil), containing linear and ring-type containing hydrogen silicone oil, at weakly alkaline ammonia salt, (produce liquid hydrogeneous MQ silicone resin under the catalysis of triethylamine Dian volatile salt, products obtained therefrom limits its purposes because hydrogen content is too high.
In P727 in " organosilicon synthesis technique and product application " book of the work such as pungent Song Shi, (five) also describe the method for making of methyl hydrogen MQ silicone resin, namely by from (Me
3si)
2o, hydrochloric acid, raw spirit, water set out, at a certain temperature with 1h in by Si (OEt)
4add in system and react, by the neutralization of the oil phase that separates, dry, filter, decompression desolventizes SiOEt content is the product of 1.9%, then by itself and a certain amount of (HMe
2si)
2o adds in system, nitrogen filled protection, heats up; and under agitation add three fluosulfonic acid and water again, keep 6h at 80 DEG C, add dimethyl formamide after being chilled to 62 DEG C again and catalyzer is precipitated; be chilled to room temperature after preserving 1h add in NaHCO3 and filter, decompression is de-low must containing the MQ resin of SiH6.2%.
" silane coupling agent and the silicone resin " one of Huang Wenrun work is in book P214, also proposition tetraethyl silicate system is containing HMQ resin. he be by water, hydrochloric acid, methyl alcohol, hydrogeneous double-seal head in flask, first be cooled to 0 DEG C, through 4h instill tetraethyl silicate and react again at 0 DEG C 1h then 20 DEG C of decompressions, distillation, washing, drying and obtain.Again by water, hydrochloric acid, methyl alcohol, MMH and MM in flask.Instill tetraethyl silicate through 4h under stirring, keep material temperature lower than 30 DEG C, then react 1h, decompression be washed to neutrality again drying obtain hydrogeneous MQ, molecular formula is [(CH
3)
2hSiO
1/2]
16[CH
3siO
1/2]
4[SiO
2]
22.
Obviously, above method is complicated, and loaded down with trivial details, the time is long, and temperature is low, and even will operate at 0-20 DEG C, this brings difficulty to suitability for industrialized production.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of hydrogeneous MQ silicone resin is provided, be mainly used in linking agent and the strengthening agent of add-on type glue, gratifying effect can be reached, a kind of preparation method of hydrogeneous MQ silicone resin is also provided, adopt tetraethoxy legal system for hydrogeneous MQ silicone resin, and can various powder, fluid be made by regulating M/Q and measure different MQ resins containing H, it is easy to operate, and starting material are easy to get, easy to control, the time is short.
First aspect of the present invention is to provide a kind of hydrogeneous MQ silicone resin, and the general formula of described hydrogeneous MQ silicone resin is: [(CH
3)
2hSiO
1/2]
a[(CH
3)
3siO
1/2]
b[SiO
2]
c, its M/Q is 0.6-0.9.
Preferably, its M/Q value is 0.7-0.8.
Preferably, the hexamethyldisiloxane in the monofunctional monomer of described hydrogeneous MQ silicone resin and the mass ratio of tetramethyl disiloxane (hydrogeneous double-seal head) are (7 ~ 18): (8 ~ 10).
More preferably, the hexamethyldisiloxane in the monofunctional monomer of described hydrogeneous MQ silicone resin and the mass ratio of tetramethyl disiloxane are (9 ~ 15): (8 ~ 10).
More preferably, the hexamethyldisiloxane in the monofunctional monomer of described hydrogeneous MQ silicone resin and the mass ratio of tetramethyl disiloxane are (11 ~ 13): (8 ~ 10).
Second aspect of the present invention is to provide the preparation method of the hydrogeneous MQ silicone resin described in the present invention first aspect, comprises the following steps:
Step 1, by monofunctional monomer, catalyzer, water and solubility promoter mixing and stirring, described monofunctional monomer comprises tetramethyl disiloxane and hexamethyldisiloxane, and described catalyzer is acid;
Step 2, in five minutes under strong stirring and room temperature, adds tetraethoxy, reaction 1-3h;
Step 3, then with alkali neutralization, extraction agent extracting and demixing, gets extraction liquid decompression and takes off low, both.
Preferably, according to mass fraction meter, in whole preparation method, the consumption of each raw material is: monofunctional monomer 100-300 part, catalyzer 35-70 part, water 80-125 part, solubility promoter 30-50 part, tetraethoxy 400-600 part, extraction agent 500-600 part.
Preferably, the hexamethyldisiloxane in described monofunctional monomer and the mass ratio of tetramethyl disiloxane are (7 ~ 18): (8 ~ 10).
More preferably, the hexamethyldisiloxane in described monofunctional monomer and the mass ratio of tetramethyl disiloxane are (9 ~ 15): (8 ~ 10).
More preferably, the hexamethyldisiloxane in described monofunctional monomer and the mass ratio of tetramethyl disiloxane are (11 ~ 13): (8 ~ 10).
Wherein, again in tetraethoxy method, described catalyzer is used for catalysis teos hydrolysis and obtains silicic acid to carry out next step condensation reaction, described catalyzer adopts acid, can be acid conventional in tetraethoxy method, such as, can be one or more in hydrochloric acid, fluosulfonic acid, sulfuric acid, Hydrogen bromide, hydrofluoric acid and hydroiodic acid HI etc.
Described alkali, for neutralizing described catalyzer, is preferably mineral alkali, such as, can be one or more in sodium bicarbonate, sodium carbonate, saleratus, salt of wormwood, potassium hydroxide, sodium hydroxide, ammoniacal liquor and cesium carbonate etc.
Preferably, described solubility promoter is water-soluble alcoholic solvent, is preferably C
1~ C
3alcoholic solvent, such as, in methyl alcohol, ethanol, n-propyl alcohol and Virahol one or more.
Described extraction agent can be one or more in esters solvent, ketones solvent, aliphatic hydrocarbon solvents, cycloaliphatic hydrocarbon kind solvent, aromatic hydrocarbons solvent and ether solvent.Can be such as one or more in ethyl acetate, methyl acetate, propyl acetate, acetone, butanone, mibk, pimelinketone, toluene, dimethylbenzene, ether, tetrachloromethane, sherwood oil and tetrahydrofuran (THF) etc.
Preferably, according to mass fraction meter, the consumption of whole preparation method's Raw is: hexamethyldisiloxane 110 parts, tetramethyl disiloxane 100 parts, tetraethoxy 500 parts, hydrochloric acid 70 parts, 110 parts, water, methyl alcohol 50 parts, toluene 520 parts.It is 0.19% that this programme can obtain hydrogen content, and entirely can be dissolved in the aqueous hydrogeneous MQ silicone resin of toluene in the ratio of 1:1.
Preferably, according to mass fraction meter, the consumption of whole preparation method's Raw is: hexamethyldisiloxane 70 parts, tetramethyl disiloxane 100 parts, tetraethoxy 540 parts, hydrochloric acid 70 parts, 120 parts, water, methyl alcohol 50 parts, toluene 520 parts.It is 0.18% that this programme can obtain hydrogen content, and entirely can be dissolved in the hydrogeneous MQ silicone resin of toluene in the ratio of 1:1.
Preferably, according to mass fraction meter, the consumption of whole preparation method's Raw is: hexamethyldisiloxane 180 parts, tetramethyl disiloxane 80 parts, tetraethoxy 500 parts, hydrochloric acid 70 parts, 110 parts, water, methyl alcohol 50 parts, toluene 520 parts.It is 0.16% that this programme can obtain hydrogen content, and entirely can be dissolved in the hydrogeneous MQ silicone resin of toluene in the ratio of 1:1.
The present invention adopts tetraethoxy legal system for hydrogeneous MQ resin, and can various powder, fluid be made by regulating M/Q and measure different MQ resins containing H, be mainly used in linking agent and the strengthening agent of add-on type glue, gratifying effect can be reached, it has easy to operate, the advantages such as starting material are easy to get, easy to control, and the time is short.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further, to understand the present invention better.
Embodiment 1
MMH (hydrogeneous double-seal head) 100g, MM (hexamethyldisiloxane) 180g, water 110g, methyl alcohol 50g, hydrochloric acid 70g are joined in the flask of 3000mL, stir, under room temperature (water-bath 15 ~ 35 DEG C) violent stirring, by constant pressure funnel, tetraethoxy 500g is instilled in flask in 5min, reaction (hydrolysis, condensation) 2.5h, then adds AR level NaHCO
3being neutralized to pH is 7 ~ 8, add toluene 500ml and extract 0.5h, again solution is moved into layering in separating funnel, water layer is abandoned it, toluene layer (oil reservoir) adds in flask, subtract de-low in constant temperature shell type well heater intensification pressure, obtaining hydrogen content is 0.19%, and entirely can be dissolved in the aqueous hydrogeneous MQ silicone resin of toluene in the ratio of 1:1 (mass ratio).
Embodiment 2
MMH (hydrogeneous double-seal head) 80g, MM (hexamethyldisiloxane) 180g, water 110g, methyl alcohol 50g, hydrochloric acid 70g are joined in the flask of 3000mL, stir, under room temperature (water-bath 15 ~ 35 DEG C) violent stirring, by constant pressure funnel, tetraethoxy 500g is instilled in flask in 3min, reaction (hydrolysis, condensation) 2 ~ 3h, then adds AR level NaHCO
3being neutralized to pH is 7 ~ 8, add toluene 500ml and extract 0.5h, again solution is moved into layering in separating funnel, water layer is abandoned it, toluene layer (oil reservoir) adds in flask, subtract de-low in constant temperature shell type well heater intensification pressure, obtaining hydrogen content is 0.16%, and entirely can be dissolved in the hydrogeneous MQ silicone resin of white powder of toluene in the ratio of 1:1 (mass ratio).
Embodiment 3
MMH (hydrogeneous double-seal head) 100g, MM (hexamethyldisiloxane) 70g, water 120g, methyl alcohol 50g, hydrochloric acid 70g are joined in the flask of 3000mL, stir, under room temperature (water-bath 15 ~ 35 DEG C) violent stirring, by constant pressure funnel, tetraethoxy 500g is instilled in flask in 3min, reaction (hydrolysis, condensation) 2 ~ 3h, then adds AR level NaHCO
3being neutralized to pH is 7 ~ 8, add toluene 500ml and extract 0.5h, again solution is moved into layering in separating funnel, water layer is abandoned it, toluene layer (oil reservoir) adds in flask, subtract de-low in constant temperature shell type well heater intensification pressure, obtaining hydrogen content is 0.18%, and entirely can be dissolved in the hydrogeneous MQ silicone resin of toluene in the ratio of 1:1 (mass ratio).
Mix with in the silicon rubber of 0.13% silicon oil of low hydrogen content of 0.5g, the hydrogeneous MQ silicone resin of 0.5g and 25g, making sheet under platinum catalyst catalysis, record sheets thus obtained tensile strength and reach 8.7MPa, elongation at break reaches 520%, and tear strength reaches 15kN/m.
Be described in detail specific embodiments of the invention above, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, equalization conversion done without departing from the spirit and scope of the invention and amendment, all should contain within the scope of the invention.
Claims (10)
1. a hydrogeneous MQ silicone resin, is characterized in that, the general formula of described hydrogeneous MQ silicone resin is: [(CH
3)
2hSiO
1/2]
a[(CH
3)
3siO
1/2]
b[SiO
2]
c, its M/Q is 0.6-0.9.
2. hydrogeneous MQ silicone resin according to claim 1, is characterized in that, the hexamethyldisiloxane in the monofunctional monomer of described hydrogeneous MQ silicone resin and the mass ratio of tetramethyl disiloxane are (7 ~ 18): (8 ~ 10).
3. a preparation method for the hydrogeneous MQ silicone resin described in claim 1 or 2, is characterized in that, comprise the following steps:
Step 1, by monofunctional monomer, catalyzer, water and solubility promoter mixing and stirring, described monofunctional monomer comprises tetramethyl disiloxane and hexamethyldisiloxane, and described catalyzer is acid;
Step 2, in five minutes under strong stirring and room temperature, adds tetraethoxy, reaction 1-3h;
Step 3, then with alkali neutralization, extraction agent extracting and demixing, gets extraction liquid decompression and takes off low, both.
4. preparation method according to claim 3, is characterized in that, according to mass fraction meter, in whole preparation method, the consumption of each raw material is:
Monofunctional monomer 100-300 part, catalyzer 35-70 part, water 80-125 part, solubility promoter 30-50 part, tetraethoxy 400-600 part, extraction agent 500-600 part.
5. preparation method according to claim 4, is characterized in that, the hexamethyldisiloxane in described monofunctional monomer and the mass ratio of tetramethyl disiloxane are (7 ~ 18): (8 ~ 10).
6. preparation method according to claim 3, is characterized in that, described catalyzer is one or more in hydrochloric acid, fluosulfonic acid, sulfuric acid, Hydrogen bromide, hydrofluoric acid and hydroiodic acid HI; Described alkali is mineral alkali, comprises one or more in sodium bicarbonate, sodium carbonate, saleratus, salt of wormwood, potassium hydroxide, sodium hydroxide, ammoniacal liquor and cesium carbonate.
7. preparation method according to claim 3, is characterized in that, described solubility promoter is C
1~ C
3alcoholic solvent, described extraction agent is one or more in esters solvent, ketones solvent, aliphatic hydrocarbon solvents, cycloaliphatic hydrocarbon kind solvent, aromatic hydrocarbons solvent and ether solvent.
8. according to the preparation method in claim 4-7 described in any one, it is characterized in that, according to mass fraction meter, the consumption of whole preparation method's Raw is: hexamethyldisiloxane 110 parts, tetramethyl disiloxane 100 parts, tetraethoxy 500 parts, hydrochloric acid 70 parts, 110 parts, water, methyl alcohol 50 parts, toluene 520 parts.
9. according to the preparation method in claim 4-7 described in any one, it is characterized in that, according to mass fraction meter, the consumption of whole preparation method's Raw is: hexamethyldisiloxane 70 parts, tetramethyl disiloxane 100 parts, tetraethoxy 540 parts, hydrochloric acid 70 parts, 120 parts, water, methyl alcohol 50 parts, toluene 520 parts.
10. according to the preparation method in claim 4-7 described in any one, it is characterized in that, according to mass fraction meter, the consumption of whole preparation method's Raw is: hexamethyldisiloxane 180 parts, tetramethyl disiloxane 80 parts, tetraethoxy 500 parts, hydrochloric acid 70 parts, 110 parts, water, methyl alcohol 50 parts, toluene 520 parts.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410588673.3A CN104371107A (en) | 2014-10-28 | 2014-10-28 | Hydrogen-containing MQ silicon resin and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410588673.3A CN104371107A (en) | 2014-10-28 | 2014-10-28 | Hydrogen-containing MQ silicon resin and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104371107A true CN104371107A (en) | 2015-02-25 |
Family
ID=52550318
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410588673.3A Pending CN104371107A (en) | 2014-10-28 | 2014-10-28 | Hydrogen-containing MQ silicon resin and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104371107A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104804191A (en) * | 2015-04-01 | 2015-07-29 | 江苏三木化工股份有限公司 | MQ silicon resin for packaging large-scale integrated circuit and preparation method |
| CN105461929A (en) * | 2015-12-23 | 2016-04-06 | 山东东岳有机硅材料有限公司 | Synthetic method of high-quality phenyl hydrogen-containing silicone oil applied to LED (Light Emitting Diode) packaging |
| CN105694046A (en) * | 2016-02-06 | 2016-06-22 | 浙江汉邦化工有限公司 | Preparation method of highly-branched block polyether-aminosiloxane finishing agent |
| CN108441165A (en) * | 2017-12-30 | 2018-08-24 | 深圳市安品有机硅材料有限公司 | Low-gravity organic silicon potting adhesive and preparation method thereof |
| CN110092913A (en) * | 2019-02-01 | 2019-08-06 | 莱芜市雅达电子材料有限公司 | A kind of MQ resin of the base containing Si-H and preparation method thereof |
| WO2020134004A1 (en) * | 2018-12-28 | 2020-07-02 | 湖州五爻硅基材料研究院有限公司 | Polysiloxane powder having no irritant odor during heating and preparation method therefor |
| CN114292588A (en) * | 2021-12-28 | 2022-04-08 | 东莞市贝特利新材料有限公司 | High-abrasion organic silicon coating and preparation method and application thereof |
| CN114574099A (en) * | 2021-12-28 | 2022-06-03 | 杭州圭臬新材料科技有限公司 | Addition type liquid silicon rubber composite film using octadiene modified MQ resin as reinforcing material and manufacturing method thereof |
| CN114835951A (en) * | 2022-05-24 | 2022-08-02 | 佛山金戈新材料股份有限公司 | MQ surface modified heat-conducting powder and preparation method and application thereof |
-
2014
- 2014-10-28 CN CN201410588673.3A patent/CN104371107A/en active Pending
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104804191A (en) * | 2015-04-01 | 2015-07-29 | 江苏三木化工股份有限公司 | MQ silicon resin for packaging large-scale integrated circuit and preparation method |
| CN105461929A (en) * | 2015-12-23 | 2016-04-06 | 山东东岳有机硅材料有限公司 | Synthetic method of high-quality phenyl hydrogen-containing silicone oil applied to LED (Light Emitting Diode) packaging |
| CN105461929B (en) * | 2015-12-23 | 2018-03-27 | 山东东岳有机硅材料有限公司 | A kind of synthetic method of high-quality phenyl hydrogen-containing silicon oil for LED encapsulation |
| CN105694046A (en) * | 2016-02-06 | 2016-06-22 | 浙江汉邦化工有限公司 | Preparation method of highly-branched block polyether-aminosiloxane finishing agent |
| CN108441165A (en) * | 2017-12-30 | 2018-08-24 | 深圳市安品有机硅材料有限公司 | Low-gravity organic silicon potting adhesive and preparation method thereof |
| WO2020134004A1 (en) * | 2018-12-28 | 2020-07-02 | 湖州五爻硅基材料研究院有限公司 | Polysiloxane powder having no irritant odor during heating and preparation method therefor |
| CN111801369A (en) * | 2018-12-28 | 2020-10-20 | 浙江三时纪新材科技有限公司 | Polysiloxane powder without pungent smell during heating and preparation method thereof |
| CN111868142A (en) * | 2018-12-28 | 2020-10-30 | 浙江三时纪新材科技有限公司 | Preparation method of spherical silicon resin powder or connected body thereof and spherical silicon resin powder or connected body thereof obtained by preparation method |
| CN111801369B (en) * | 2018-12-28 | 2021-05-18 | 浙江三时纪新材科技有限公司 | Polysiloxane powder without pungent smell during heating and preparation method thereof |
| CN110092913A (en) * | 2019-02-01 | 2019-08-06 | 莱芜市雅达电子材料有限公司 | A kind of MQ resin of the base containing Si-H and preparation method thereof |
| CN114292588A (en) * | 2021-12-28 | 2022-04-08 | 东莞市贝特利新材料有限公司 | High-abrasion organic silicon coating and preparation method and application thereof |
| CN114574099A (en) * | 2021-12-28 | 2022-06-03 | 杭州圭臬新材料科技有限公司 | Addition type liquid silicon rubber composite film using octadiene modified MQ resin as reinforcing material and manufacturing method thereof |
| CN114835951A (en) * | 2022-05-24 | 2022-08-02 | 佛山金戈新材料股份有限公司 | MQ surface modified heat-conducting powder and preparation method and application thereof |
| CN114835951B (en) * | 2022-05-24 | 2024-06-04 | 广东金戈新材料股份有限公司 | MQ surface modified heat conducting powder and preparation method and application thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104371107A (en) | Hydrogen-containing MQ silicon resin and preparation method thereof | |
| CN104152104B (en) | A kind of autohension organic silicon pressure-sensitive adhesive and preparation method thereof | |
| CN103756627B (en) | The fast cured silicone seal gum of the weather-proof dealcoholizing-type of shelf-stable | |
| CN103242532B (en) | Preparation method of environment-friendly solventless liquid silicone resin | |
| CN102181055B (en) | Preparation method of reactive MQ silicon resin | |
| CN101747632A (en) | Organic silicon rubber encapsulating material for high-power LED | |
| CN104892942A (en) | Tackifier for addition-type organic silicon rubber and preparation method thereof | |
| CN103044683A (en) | Modified MQ silicone resin and preparation method thereof | |
| CN104086772A (en) | Uramido modified MQ silicon resin, and preparation method and application thereof | |
| CN103819679B (en) | A kind of preparation method of one pack system POSS/ add-on type silicones nano composite material | |
| CN107880773B (en) | Water-based epoxy modified silicone resin coating and preparation method thereof | |
| CN101781328B (en) | Preparation method of cyclosiloxane | |
| KR20140024244A (en) | Hydrosilicone resin and preparation process thereof | |
| CN104610549A (en) | Modified fluorine-containing silicone oil and preparation method thereof | |
| CN104098916A (en) | Addition type ultra-soft silicone rubber, as well as preparation method and application thereof | |
| CN102897765A (en) | Method for preparing 3-aminopropyl triethoxy silane hydrolysate | |
| CN103087320A (en) | Preparation method of hydroxyl-terminated polymethylphenyl silicone oil | |
| CN103540289A (en) | Preparation method and application of organic silicon resin adhesive | |
| CN103450481A (en) | Preparation method of methyl phenyl vinyl silicone | |
| CN105273682B (en) | LED glass ball bulb lamps are explosion-proof to use add-on type silica-gel composition | |
| CN106380858A (en) | Low-hardness high-percentage elongation two-component addition-type rubber and production method thereof | |
| CN103484057B (en) | Preparation method of silicone resin for adhesion of solvent-free environment-friendly glass fiber | |
| CN107641466A (en) | A kind of organosilicon solvent-free dip varnish and preparation method thereof | |
| CN105461929A (en) | Synthetic method of high-quality phenyl hydrogen-containing silicone oil applied to LED (Light Emitting Diode) packaging | |
| CN105440694B (en) | Organopolysiloxane composition and preparation method thereof and semiconductor devices |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20150225 |
|
| RJ01 | Rejection of invention patent application after publication |