CN102924501B - A kind of preparation method of methyl alkoxy acetoxysilane and the de-acetic acid type room temperature sealing silicone sulfide glue of application thereof - Google Patents
A kind of preparation method of methyl alkoxy acetoxysilane and the de-acetic acid type room temperature sealing silicone sulfide glue of application thereof Download PDFInfo
- Publication number
- CN102924501B CN102924501B CN201210431735.0A CN201210431735A CN102924501B CN 102924501 B CN102924501 B CN 102924501B CN 201210431735 A CN201210431735 A CN 201210431735A CN 102924501 B CN102924501 B CN 102924501B
- Authority
- CN
- China
- Prior art keywords
- acetoxysilane
- methyl
- acetic acid
- alkoxy
- preparation
- 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
Abstract
The invention discloses a kind of preparation method of methyl alkoxy acetoxysilane and the de-acetic acid type room temperature sealing silicone sulfide glue of application thereof, relate to the preparation field of alkoxy acyloxy.The step of preparation method is: be that methyl triacetoxysilane and the alcohols of 1:1 puts into reactor by mol ratio, stirring reaction 2 hours at the temperature of 50 DEG C, form methyl alkoxy acetoxysilane crude product, deviate from the acetic acid in described crude product under negative pressure, form methyl alkoxy acetoxysilane finished product.The Tc of the de-acetic acid type room temperature sealing silicone sulfide glue prepared by the present invention is less than-10 DEG C, and not only Tc is lower, be convenient to the use of people, and adhesive property is better.
Description
Technical field
The present invention relates to the preparation field of alkoxy acyloxy, be specifically related to a kind of preparation method of methyl alkoxy acetoxysilane and the de-acetic acid type room temperature sealing silicone sulfide glue of application thereof.
Background technology
De-acetic acid type room temperature sealing silicone sulfide glue (hereinafter referred to as RTV-1 glue) is one of main products in condensed type liquid silastic, is mainly used in encapsulating various electronic devices and components and electric installation.
The linking agent preparing RTV-1 glue used is made primarily of methyl triacetoxysilane, but, ctystallizing point due to methyl triacetoxysilane is about 40 DEG C, and the RTV-1 glue therefore prepared with methyl triacetoxysilane will occur solid particulate in colloid and cannot normally use when temperature is lower in the winter time.
In order to solve the problem, people add tetramethoxy-silicane in methyl triacetoxysilane, and the ctystallizing point of tetramethoxy-silicane self is lower, and then reduce the ctystallizing point of methyl triacetoxysilane prepared therefrom.But introduce four sense links in tetramethoxy-silicane, add the cross-linking density of methyl triacetoxysilane, therefore, the adhesive property of the RTV-1 glue that the methyl triacetoxysilane adding tetramethoxy-silicane is prepared is poor.
Application number is that the patent of invention of CN200910061452.X discloses a kind of alkyl acyloxy silane mixture and preparation method thereof, and alkyl acyloxy silane mixture comprises methyl triacetoxysilane and alkyl triacetoxysilane.Although the alkyl acyloxy silane mixture prepared by the preparation method described in this patent of invention can reduce certain ctystallizing point, when temperature is less than-10 DEG C, alkyl acyloxy silane mixture still can crystallization.
Summary of the invention
For the defect existed in prior art, the object of the present invention is to provide the de-acetic acid type room temperature sealing silicone sulfide glue of a kind of preparation method of methyl alkoxy acetoxysilane and application thereof, not only Tc is lower for the de-acetic acid type room temperature sealing silicone sulfide glue (RTV-1 glue) prepared by the present invention, be convenient to the use of people, and adhesive property is better.
The preparation method of methyl alkoxy acetoxysilane provided by the invention, comprise the following steps: be that methyl triacetoxysilane and the alcohols of 1:1 puts into reactor by mol ratio, stirring reaction 2 hours at the temperature of 50 DEG C, form methyl alkoxy acetoxysilane crude product, deviate from the acetic acid in described crude product under negative pressure, form methyl alkoxy acetoxysilane finished product.
On the basis of technique scheme, described alcohols is methyl alcohol, ethanol, Virahol, the trimethyl carbinol or ethylene glycol monomethyl ether.
On the basis of technique scheme, described negative pressure is-0.098Mpa.
De-acetic acid type room temperature sealing silicone sulfide glue provided by the invention, comprise hydroxy-end capped polydimethyl sily oxide, alkyl-blocked polydimethylsiloxane, linking agent, silicon-dioxide and catalyzer, it is characterized in that: described linking agent is the arbitrary described methyl alkoxy acetoxysilane finished product of claim 1 to 5.
On the basis of technique scheme, described de-acetic acid type room temperature sealing silicone sulfide glue comprises 100 parts of hydroxy-end capped polydimethyl sily oxide, 10 parts of alkyl-blocked polydimethylsiloxanes, 8 parts of methyl alkoxy acetoxysilane finished products, 8 parts of silicon-dioxide and 0.03 part of catalyzer by mass parts.
On the basis of technique scheme, the Tc of described de-acetic acid type room temperature sealing silicone sulfide glue is less than-10 DEG C.
On the basis of technique scheme, the tensile strength of described de-acetic acid type room temperature sealing silicone sulfide glue is 0.96Mpa ~ 1.18Mpa.
On the basis of technique scheme, the elongation of described de-acetic acid type room temperature sealing silicone sulfide glue is 385% ~ 455%.
Beneficial effect of the present invention is:
(1) when the present invention prepares RTV-1 glue, adopt methyl alkoxy acetoxysilane as linking agent, because methyl alkoxy acetoxysilane ctystallizing point is lower, the Tc of the RTV-1 glue therefore prepared by methyl alkoxy acetoxysilane is low; Due in methyl alkoxy acetoxysilane containing alkoxyl group and acetoxyl group two kinds of active groups, the adhesive property of the RTV-1 glue therefore prepared by methyl alkoxy acetoxysilane is better.
(2), when the present invention prepares methyl alkoxy acetoxysilane, be difficult to produce harmful composition (as Acetyl Chloride 98Min., hydrochloric acid etc.), safer.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.
The preparation method of the methyl alkoxy acetoxysilane that the embodiment of the present invention provides, comprise the following steps: be that methyl triacetoxysilane and the alcohols of 1:1 puts into reactor by mol ratio, stirring reaction 2 hours at the temperature of 50 DEG C, form methyl alkoxy acetoxysilane crude product, deviate from the acetic acid in crude product under negative pressure, form methyl alkoxy acetoxysilane finished product.
Negative pressure in above-mentioned preparation method is-0.098Mpa; Alcohols can select methyl alcohol, ethanol, Virahol, the trimethyl carbinol or ethylene glycol monomethyl ether.
The de-acetic acid type room temperature sealing silicone sulfide glue (RTV-1 glue) that the embodiment of the present invention provides, comprise 100 parts of hydroxy-end capped polydimethyl sily oxide, 10 parts of alkyl-blocked polydimethylsiloxanes, 8 parts of linking agents, 8 parts of silicon-dioxide and 0.03 part of catalyzer by mass parts, wherein linking agent is the methyl alkoxy acetoxysilane finished product prepared by above-mentioned preparation method
Be specifically described below by six embodiments.
Embodiment 1
440g(2mol is added in the there-necked flask of 1L) methyl triacetoxysilane and 64g(2mol) methyl alcohol, stirring reaction 2 hours at the temperature of 50 DEG C, form the methyl alkoxy acetoxysilane crude product containing methyl methoxy base diacetoxy silane, under the pressure of-0.098Mpa, deviate from the acetic acid in crude product, form the methyl alkoxy acetoxysilane finished product (hereinafter referred to as finished product 1) that 382g contains methyl methoxy base acetoxysilane.
The RTV-1 glue prepared by finished product 1, comprises polydimethylsiloxane, 80g finished product 1(linking agent that the hydroxy-end capped polydimethyl sily oxide of 1000g, 100g are alkyl-blocked), 80g silicon-dioxide and 0.3g dibutyltin diacetate (catalyzer).
Embodiment 2
440g(2mol is added in the there-necked flask of 1L) methyl triacetoxysilane and 92g(2mol) ethanol, stirring reaction 2 hours at the temperature of 50 DEG C, form the methyl alkoxy acetoxysilane crude product containing methyl ethoxy diacetoxy silane, under the pressure of-0.098Mpa, deviate from the acetic acid in crude product, form the methyl alkoxy acetoxysilane finished product (hereinafter referred to as finished product 2) that 415g contains methyl ethoxy diacetoxy silane.
The RTV-1 glue prepared by finished product 2, comprises polydimethylsiloxane, 80g finished product 2(linking agent that the hydroxy-end capped polydimethyl sily oxide of 1000g, 100g are alkyl-blocked), 80g silicon-dioxide and 0.3g dibutyltin diacetate (catalyzer).
Embodiment 3
440g(2mol is added in the there-necked flask of 1L) methyl triacetoxysilane and 120g(2mol) Virahol, stirring reaction 2 hours at the temperature of 50 DEG C, form the methyl alkoxy acetoxysilane crude product containing methyl isopropyl oxygen base diacetoxy silane, under the pressure of-0.450Mpa, deviate from the acetic acid in crude product, form the methyl alkoxy acetoxysilane finished product (hereinafter referred to as finished product 3) that 442g contains methyl isopropyl oxygen base diacetoxy silane.
The RTV-1 glue prepared by finished product 3, comprises polydimethylsiloxane, 80g finished product 3(linking agent that the hydroxy-end capped polydimethyl sily oxide of 1000g, 100g are alkyl-blocked), 80g silicon-dioxide and 0.3g dibutyltin diacetate (catalyzer).
Embodiment 4
440g(2mol is added in the there-necked flask of 1L) methyl triacetoxysilane and 148g(2mol) trimethyl carbinol, stirring reaction 2 hours at the temperature of 50 DEG C, form the methyl alkoxy acetoxysilane crude product containing methyl-tert butoxy diacetoxy silane, under the pressure of-0.098Mpa, deviate from the acetic acid in crude product, form the methyl alkoxy acetoxysilane finished product (hereinafter referred to as finished product 4) that 470g contains methyl-tert butoxy diacetoxy silane.
The RTV-1 glue prepared by finished product 4, comprises polydimethylsiloxane, 80g finished product 4(linking agent that the hydroxy-end capped polydimethyl sily oxide of 1000g, 100g are alkyl-blocked), 80g silicon-dioxide and 0.3g dibutyltin diacetate (catalyzer).
Embodiment 5
440g(2mol is added in the there-necked flask of 1L) methyl triacetoxysilane and 152g(2mol) ethylene glycol monomethyl ether, stirring reaction 2 hours at the temperature of 50 DEG C, form the methyl alkoxy acetoxysilane crude product containing methyl (2-methoxy ethoxy) diacetoxy silane, under the pressure of-0.098Mpa, deviate from the acetic acid in crude product, form the methyl alkoxy acetoxysilane finished product (hereinafter referred to as finished product 5) that 475g contains methyl (2-methoxy ethoxy) diacetoxy silane.
The RTV-1 glue prepared by finished product 5, comprises polydimethylsiloxane, 80g finished product 5(linking agent that the hydroxy-end capped polydimethyl sily oxide of 1000g, 100g are alkyl-blocked), 80g silicon-dioxide and 0.3g dibutyltin diacetate (catalyzer).
Embodiment 6
The RTV-1 glue prepared by methyl triacetoxysilane, comprises polydimethylsiloxane, 80g methyl triacetoxysilane (linking agent), 80g silicon-dioxide and 0.3g dibutyltin diacetate (catalyzer) that the hydroxy-end capped polydimethyl sily oxide of 1000g, 100g are alkyl-blocked.
Verify the RTV-1 glue in embodiment 1 to embodiment 6 respectively, the performance perameter before RTV-1 adhesive curing and after solidification is see table 1.Known, there is crystalline particle after the RTV-1 glue in embodiment 6 deposits 24 hours at the temperature of-10 DEG C; Nodeless mesh particle (namely Tc is less than-10 DEG C) after 24 hours not only deposited by RTV-1 glue in embodiment 1 to embodiment 5 at the temperature of-10 DEG C, and growth rate is better, meets the index of GB/T14683-2003 " silicone construction sealant ".
Performance perameter in table 1, embodiment 1 to embodiment 6 before RTV-1 adhesive curing and after solidification
The present invention is not limited to above-mentioned embodiment, and for those skilled in the art, under the premise without departing from the principles of the invention, can also make some improvements and modifications, these improvements and modifications are also considered as within protection scope of the present invention.The content be not described in detail in this specification sheets belongs to the known prior art of professional and technical personnel in the field.
Claims (2)
1. the preparation method of a methyl alkoxy acetoxysilane, it is characterized in that, comprise the following steps: be that methyl triacetoxysilane and the alcohols of 1:1 puts into reactor by mol ratio, stirring reaction 2 hours at the temperature of 50 DEG C, form methyl alkoxy acetoxysilane crude product, deviate from the acetic acid in described crude product under negative pressure, form methyl alkoxy acetoxysilane finished product, described alcohols is methyl alcohol, ethanol, Virahol or ethylene glycol monomethyl ether.
2. the preparation method of methyl alkoxy acetoxysilane as claimed in claim 1, is characterized in that: described negative pressure is-0.098Mpa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210431735.0A CN102924501B (en) | 2012-10-31 | 2012-10-31 | A kind of preparation method of methyl alkoxy acetoxysilane and the de-acetic acid type room temperature sealing silicone sulfide glue of application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210431735.0A CN102924501B (en) | 2012-10-31 | 2012-10-31 | A kind of preparation method of methyl alkoxy acetoxysilane and the de-acetic acid type room temperature sealing silicone sulfide glue of application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102924501A CN102924501A (en) | 2013-02-13 |
| CN102924501B true CN102924501B (en) | 2015-08-19 |
Family
ID=47639454
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210431735.0A Active CN102924501B (en) | 2012-10-31 | 2012-10-31 | A kind of preparation method of methyl alkoxy acetoxysilane and the de-acetic acid type room temperature sealing silicone sulfide glue of application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102924501B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103450246B (en) * | 2013-08-22 | 2016-05-25 | 浙江衢州硅宝化工有限公司 | The preparation method of methyl acetoxyl group methoxy silane |
| CN115322438B (en) * | 2022-07-12 | 2023-06-06 | 湖北新蓝天新材料股份有限公司 | Methyl alkoxy acetoxy silane mixture with low crystallization temperature and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3296195A (en) * | 1963-12-20 | 1967-01-03 | Gen Electric | Curable composition |
| WO2001079212A1 (en) * | 2000-04-17 | 2001-10-25 | Vyacheslav Vasilievich Kireev | Silicon derivatives of fragrant, flavouring and medicinal substances |
| CN1608111A (en) * | 2001-11-09 | 2005-04-20 | 通用电气公司 | Synthesis and use of alkylalkoxy acyloxysilanes and blends thereof for use as a crosslinking agent in moisture curing rtv's |
| US20120196225A1 (en) * | 2011-01-27 | 2012-08-02 | Namitek Specialty Materials Corp. | Photo Patternable Coating Compositions of Silicones and Organic-Inorganic Hybrids |
-
2012
- 2012-10-31 CN CN201210431735.0A patent/CN102924501B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3296195A (en) * | 1963-12-20 | 1967-01-03 | Gen Electric | Curable composition |
| WO2001079212A1 (en) * | 2000-04-17 | 2001-10-25 | Vyacheslav Vasilievich Kireev | Silicon derivatives of fragrant, flavouring and medicinal substances |
| CN1608111A (en) * | 2001-11-09 | 2005-04-20 | 通用电气公司 | Synthesis and use of alkylalkoxy acyloxysilanes and blends thereof for use as a crosslinking agent in moisture curing rtv's |
| US20120196225A1 (en) * | 2011-01-27 | 2012-08-02 | Namitek Specialty Materials Corp. | Photo Patternable Coating Compositions of Silicones and Organic-Inorganic Hybrids |
Non-Patent Citations (2)
| Title |
|---|
| 《RTV防污闪涂料的研究》;秦瑞等;《现代涂料与涂装》;CNKI;20090920;第12卷(第9期);第4-10页 * |
| 《单组分室温硫化硅橡胶的配制(一)》;黄文润;《有机硅材料》;CNKI;20020722;第16卷(第4期);第32-40页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102924501A (en) | 2013-02-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103805128B (en) | A kind of synthetic method of high refractive index LED glue caking agent | |
| CN102146208B (en) | Method for preparing transparent dealcoholized single-component room temperature vulcanized silicone rubber | |
| CN105368063B (en) | It is a kind of to store stable single-component dealcoholization-type room temperature vulcanized silicone rubber | |
| CN104877138A (en) | Silicon resin with adhesive properties and preparation method of silicon resin | |
| CN102532434A (en) | UV (Ultraviolet)/moisture double cured silicon rubber and preparation method thereof | |
| CN105524282B (en) | Organic borosilicate adhesion promoters of high refractive index and its preparation method and application | |
| CN102924501B (en) | A kind of preparation method of methyl alkoxy acetoxysilane and the de-acetic acid type room temperature sealing silicone sulfide glue of application thereof | |
| CN109593510A (en) | Alkoxy end-capped organosilicon polymer, preparation method and single-component de-alcoholized organosilicon sealant | |
| CN102372733A (en) | Continuous preparation method for methyl trialkoxysilane | |
| CN101792653A (en) | Sealant for acrylic ester modified solar photovoltaic module and preparation method thereof | |
| CN104558612A (en) | Alkoxy-terminated polysiloxane polymer and preparation method thereof | |
| CN103896978A (en) | Preparation method for high-purity methylphenyl-dimethoxysilane | |
| CN105348536A (en) | Synthesis method of UV/moisture dual-curing polymer | |
| CN106590070B (en) | Obstruct infrared, heat-insulated transparent inorganic coating and its preparation method and application | |
| CN102775792B (en) | Modified hydrogen-containing silicone oil, preparation method and application thereof, and silicon rubber containing modified hydrogen-containing silicone oil | |
| CN104031392A (en) | Addition-type silica gel, and preparation method and application thereof | |
| CN102604579A (en) | Polyester glue specially used for compounding PET (polyethylene terephthalate) film and fluoride film of solar cell backboard and method for preparing same | |
| CN104927058B (en) | A kind of hydroxyl polysiloxane blocking modification method | |
| CN102604580A (en) | Polyester glue specially used for compounding PET (polyethylene terephthalate) film and PE (polyethylene) film of solar cell backboard and method for preparing same | |
| CN103897577B (en) | glass coating and preparation method thereof | |
| CN105925205A (en) | Production process for ultrahigh cut-off EVA (ethylene-vinyl acetate) packaging glue film | |
| CN103484057B (en) | Preparation method of silicone resin for adhesion of solvent-free environment-friendly glass fiber | |
| CN105255479A (en) | Preparation method of colloidal quantum dot fluorescent powder composite film | |
| CN106832958A (en) | Photocuring add-on type organopolysiloxane composition and its application in LED element encapsulation | |
| CN103756561B (en) | A kind of Novel automobile safety airbag coating silica gel material 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 | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |