CN113004525A - Low-viscosity methyl modified polysiloxane and preparation method thereof - Google Patents
Low-viscosity methyl modified polysiloxane and preparation method thereof Download PDFInfo
- Publication number
- CN113004525A CN113004525A CN202110243682.9A CN202110243682A CN113004525A CN 113004525 A CN113004525 A CN 113004525A CN 202110243682 A CN202110243682 A CN 202110243682A CN 113004525 A CN113004525 A CN 113004525A
- Authority
- CN
- China
- Prior art keywords
- modified polysiloxane
- hydrogen
- methyl
- low
- parts
- 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
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
-
- 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
-
- 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
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
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)
- Silicon Polymers (AREA)
Abstract
The invention discloses a low-viscosity methyl modified polysiloxane and a preparation method thereof, wherein the low-viscosity methyl modified polysiloxane comprises the following raw materials in parts by weight: 100 parts of hydrogen-containing silicone oil and 50-180 parts of olefin. The low-viscosity methyl modified polysiloxane is prepared by using methylhydrogen dichlorosilane as a raw material and sequentially performing hydrolysis, neutralization, telomerization, adsorption decoloration, filtration, hydrosilylation, depreciation and filtration, can be used for a silicone sealant plasticizer, a powder surface treatment agent and a silicone adhesive color paste pigment, has a wide application field, improves the added value of the methylhydrogen dichlorosilane, is simple and convenient to operate, has the yield of more than 90 percent, does not generate harmful substances, and is environment-friendly.
Description
Technical Field
The invention relates to the technical field of polysiloxane, in particular to low-viscosity methyl modified polysiloxane and a preparation method thereof.
Background
Organosilicon is a novel high molecular material, has excellent temperature resistance, weather resistance, ultraviolet resistance and stable electrical insulating property, can be used as a special material for aviation and military use, can also be used in the civil field, and has expanded application range: building, electronic and electric, textile, automobile, machinery, leather and paper making, chemical light industry, metal and paint, medical treatment and the like. A large amount of byproduct methyl hydrogen dichlorosilane can be formed in the production process of the organosilicon monomer methyl chlorosilane, and serious safety and environmental protection problems are easily caused due to low added value and complex treatment process. At present, methyl hydrogen dichlorosilane is mainly used for preparing hydrogen-containing silicone oil, and has the problems of complex process flow, strict operation requirements, generation of three wastes and the like.
Disclosure of Invention
The invention aims to provide low-viscosity methyl modified polysiloxane which comprises the following raw materials in parts by weight: 100 parts of hydrogen-containing silicone oil and 50-180 parts of olefin.
Preferably, the hydrogen content of the hydrogen-containing silicone oil is 0.5-1.6% by mass.
Preferably, the hydrogen-containing silicone oil comprises the following raw materials in parts by weight: 30-80 parts of methyl hydrogen dichlorosilane, 5-50 parts of octamethylcyclotetrasiloxane, 10-30 parts of hydrogen-containing end-capping reagent and 15-30 parts of water.
Preferably, the hydrogen-containing end-capping agent is methyldisiloxane.
The invention also provides a preparation method of the low-viscosity methyl modified polysiloxane, which comprises the following specific steps:
s1: injecting metered methyl hydrogen dichlorosilane, octamethylcyclotetrasiloxane, hydrogen-containing end-capping reagent and water into a hydrolysis kettle, and hydrolyzing, acid-separating neutralizing, telomerizing, adsorbing and decolorizing and filtering at 0-15 ℃ to obtain the finished product of hydrogen-containing silicone oil;
s2: firstly, carrying out addition reaction on the hydrogen-containing silicone oil prepared in the last step and olefin under the condition of a catalyst to obtain methyl modified polysiloxane;
s3: and (3) removing low viscosity, decoloring and filtering the methyl modified polysiloxane to obtain the finished product of the low viscosity methyl modified polysiloxane.
Preferably, the viscosity of the finished low-viscosity methyl modified polysiloxane is 500-20000 mm2/s, the molecular weight is 5000-80000, the pH value is 6.0-8.0, and the specific gravity is 0.93-0.96.
Preferably, the addition reaction is carried out in a Venturi mixer, the reaction temperature is 25-55 ℃, and the reaction time is 2-12 hours.
Preferably, the olefin is any one of ethylene, propylene, butene, pentene, hexene, octene, decene, dodecene, tetradecene, styrene, isobornene, acrylate, methacrylate, and vinyl acetate.
Preferably, the temperature for removing the low-boiling-point substances is 160-210 ℃, the vacuum condition is-0.08-0.10 MPa, and the removal time is 1-3 h.
Preferably, the catalyst used in the addition reaction is a platinum complex catalyst, and the addition amount of the platinum complex catalyst is 50-200 PPm.
Compared with the prior art, the invention has the beneficial effects that: the low-viscosity methyl modified polysiloxane is prepared by using methylhydrogen dichlorosilane as a raw material and sequentially performing hydrolysis, neutralization, telomerization, adsorption decoloration, filtration, hydrosilylation, depreciation and filtration, can be used for a silicone sealant plasticizer, a powder surface treatment agent and a silicone adhesive color paste pigment, has a wide application field, improves the added value of the methylhydrogen dichlorosilane, is simple and convenient to operate, has the yield of more than 90 percent, does not generate harmful substances, and is environment-friendly.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1:
the low-viscosity methyl modified polysiloxane is characterized by having a molecular weight of 5000-80000 and being prepared by sequentially adopting the following steps:
step one, injecting metered methyl hydrogen dichlorosilane, octamethylcyclotetrasiloxane (D4), hydrogen-containing end-capping reagent (methyl disiloxane) and water into a hydrolysis kettle (0-15 ℃), and hydrolyzing, acid-separating neutralizing, telomerizing, adsorbing and decolorizing and filtering under normal pressure to obtain the finished product hydrogen-containing silicone oil with the hydrogen content of 0.5 percent by mass. Wherein the weight ratio of the methylhydrodichlorosilane to the cyclotetrasiloxane (D4) to the hydrogen-containing end-capping reagent to the water is 30:45:5: 20;
and step two, pumping the hydrogen-containing silicone oil prepared in the step one into a Venturi mixer in a vertical reaction kettle through a centrifugal pump, then adding a platinum complex catalyst of 50PPm, dropwise adding octene, stirring, mixing and circulating, circularly reacting for 6 hours under the conditions of normal pressure, temperature of 45 ℃ and rotating speed of 60r/min to obtain methyl modified polysiloxane, finally keeping for 1.5 hours under the conditions of 180 ℃ and vacuum degree of-0.090 MPa to remove low-boiling-point substances, and finally adsorbing, decoloring and filtering through activated carbon to obtain the low-viscosity methyl modified polysiloxane, wherein the weight ratio of the hydrogen-containing silicone oil to the octene is 100:50, and the gas adopted for bubbling during the removal of the low-boiling-point substances is nitrogen.
The polysiloxane prepared had a viscosity (25 ℃ mm2/s) of 1000, a pH of 7, a specific gravity of 0.96, a purity of 90% and a yield of 80%.
Example 2:
the procedure is as in example 1, except that:
in the first step, the weight ratio of the methylhydrogen dichlorosilane to the cyclotetrasiloxane (D4) to the hydrogen-containing end-capping reagent to the water is 40:25:10: 25; the mass percentage of hydrogen in the hydrogen-containing silicone oil is 0.8%;
in the second step, the weight ratio of the hydrogen-containing silicone oil to the octene is 100:80, the addition amount of the platinum complex catalyst is 70PPm, the rotation speed is 100r/min, the reaction time is 8h, the temperature for removing low-boiling-point substances is 190 ℃, and the vacuum degree is-0.090 MPa.
The polysiloxane prepared had a viscosity (25 ℃ mm2/s) of 5000, a specific gravity of 0.95, a purity of 92% and a yield of 82%.
Example 3:
the procedure is as in example 1, except that:
in the first step, the weight ratio of the methylhydrogen dichlorosilane to the cyclotetrasiloxane (D4) to the hydrogen-containing end-capping reagent to the water is 50:10:15: 25; the mass percentage of hydrogen in the hydrogen-containing silicone oil is 1.2%;
in the second step, the weight ratio of the hydrogen-containing silicone oil to the octene is 100:130, the addition amount of the platinum complex catalyst is 100PPm, the rotation speed is 100r/min, the reaction time is 10h, the temperature for removing low-boiling-point substances is 200 ℃, and the vacuum degree is-0.095 MPa.
The polysiloxane thus prepared had a viscosity (25 ℃ mm2/s) of 10000, a specific gravity of 0.94, a purity of 93% and a yield of 83%.
Example 4:
the procedure is as in example 1, except that:
in the first step, the weight ratio of the methylhydrogen dichlorosilane to the cyclotetrasiloxane (D4) to the hydrogen-containing end-capping reagent to the water is 60:0:15: 25; the mass percentage of hydrogen in the hydrogen-containing silicone oil is 1.5%;
in the second step, the weight ratio of the hydrogen-containing silicone oil to the octene is 100:170, the addition amount of the platinum complex catalyst is 100PPm, the rotation speed is 100r/min, the reaction time is 12h, the temperature for removing low-boiling-point substances is 210 ℃, and the vacuum degree is-0.095 MPa.
The polysiloxane thus obtained had a viscosity (25 ℃ mm2/s) of 20000, a specific gravity of 0.93, a purity of 95% and a yield of 85%.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A low viscosity methyl-modified polysiloxane characterized by: the raw materials are as follows by weight: 100 parts of hydrogen-containing silicone oil and 50-180 parts of olefin.
2. A low viscosity methyl-modified polysiloxane according to claim 1, which is characterized in that: the hydrogen content of the hydrogen-containing silicone oil is 0.5-1.6% by mass.
3. A low viscosity methyl-modified polysiloxane according to claim 2, which is characterized in that: the hydrogen-containing silicone oil comprises the following raw materials in parts by weight: 30-80 parts of methyl hydrogen dichlorosilane, 5-50 parts of octamethylcyclotetrasiloxane, 10-30 parts of hydrogen-containing end-capping reagent and 15-30 parts of water.
4. A low viscosity methyl-modified polysiloxane according to claim 3, which is characterized in that: the hydrogen-containing end-capping agent is methyl disiloxane.
5. A method for producing the low-viscosity methyl-modified polysiloxane of claim 4, which comprises: the method comprises the following specific steps:
s1: injecting metered methyl hydrogen dichlorosilane, octamethylcyclotetrasiloxane, hydrogen-containing end-capping reagent and water into a hydrolysis kettle, and hydrolyzing, acid-separating neutralizing, telomerizing, adsorbing and decolorizing and filtering at 0-15 ℃ to obtain the finished product of hydrogen-containing silicone oil;
s2: firstly, carrying out addition reaction on the hydrogen-containing silicone oil prepared in the last step and olefin under the condition of a catalyst to obtain methyl modified polysiloxane;
s3: and (3) removing low viscosity, decoloring and filtering the methyl modified polysiloxane to obtain the finished product of the low viscosity methyl modified polysiloxane.
6. The method for preparing a low viscosity methyl-modified polysiloxane according to claim 5, wherein: the viscosity of the finished low-viscosity methyl modified polysiloxane is 500-20000 mm2The molecular weight is 5000-80000, the pH value is 6.0-8.0, and the specific gravity is 0.93-0.96.
7. The method for preparing a low viscosity methyl-modified polysiloxane according to claim 5, wherein: the addition reaction is carried out in a Venturi mixer, the reaction temperature is 25-55 ℃, and the reaction time is 2-12 hours.
8. The method for preparing a low viscosity methyl-modified polysiloxane according to claim 5, wherein: the olefin is any one of ethylene, propylene, butene, pentene, hexene, octene, decene, dodecene, tetradecene, styrene, isobornene, acrylate, methacrylate and vinyl acetate.
9. The method for preparing a low viscosity methyl-modified polysiloxane according to claim 5, wherein: the temperature for removing the low-boiling-point substances is 160-210 ℃, the vacuum condition is-0.08-0.10 MPa, and the removal time is 1-3 h.
10. The method for preparing a low viscosity methyl-modified polysiloxane according to claim 5, wherein: the catalyst used in the addition reaction is a platinum complex catalyst, and the addition amount of the platinum complex catalyst is 50-200 PPm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110243682.9A CN113004525A (en) | 2021-03-05 | 2021-03-05 | Low-viscosity methyl modified polysiloxane and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110243682.9A CN113004525A (en) | 2021-03-05 | 2021-03-05 | Low-viscosity methyl modified polysiloxane and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113004525A true CN113004525A (en) | 2021-06-22 |
Family
ID=76406311
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110243682.9A Pending CN113004525A (en) | 2021-03-05 | 2021-03-05 | Low-viscosity methyl modified polysiloxane and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113004525A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974157A (en) * | 2010-11-02 | 2011-02-16 | 中昊晨光化工研究院 | Synthesis method of phenyl hydrogen-containing silicone oil |
| CN104710618A (en) * | 2015-03-16 | 2015-06-17 | 南京博明科技有限责任公司 | Production technology for continuously producing high-hydrogen silicone oil |
| CN112358619A (en) * | 2020-10-15 | 2021-02-12 | 佛山市顺德区天采有机硅有限公司 | Preparation method of methyl modified polysiloxane with adjustable viscosity |
-
2021
- 2021-03-05 CN CN202110243682.9A patent/CN113004525A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101974157A (en) * | 2010-11-02 | 2011-02-16 | 中昊晨光化工研究院 | Synthesis method of phenyl hydrogen-containing silicone oil |
| CN104710618A (en) * | 2015-03-16 | 2015-06-17 | 南京博明科技有限责任公司 | Production technology for continuously producing high-hydrogen silicone oil |
| CN112358619A (en) * | 2020-10-15 | 2021-02-12 | 佛山市顺德区天采有机硅有限公司 | Preparation method of methyl modified polysiloxane with adjustable viscosity |
Non-Patent Citations (1)
| Title |
|---|
| 马凤国等: "高含氢硅油调聚法制备低含氢硅油的研究", 《有机硅材料》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102643549B (en) | Dealcoholized flame-retardant silicone sealant and preparation method thereof | |
| CN102942896B (en) | Single-component addition type high adhesion organic silicon rubber | |
| CN103865389A (en) | Preparation method of novel addition-type solvent-free organosilicone isolation agent | |
| CN104387546A (en) | Phenyl organic silicon modified polyurethane resin, preparation method and application thereof | |
| CN101121861B (en) | Low-viscosity solvent-free organic silicon insulation impregnating varnish and preparation method thereof | |
| CN104513644B (en) | Transparent pouring sealant and use thereof | |
| CN104530967A (en) | Reactive organosilicon waterproofing agent as well as preparation method and application thereof | |
| DE102011086862A1 (en) | Composition of olefinically functionalized siloxane oligomers based on alkoxysilanes | |
| CN103044683A (en) | Modified MQ silicone resin and preparation method thereof | |
| CN111793210B (en) | Preparation method of RTV (room temperature vulcanized) silicone rubber tackifier | |
| CN106146850A (en) | A kind of additional organosilicon impregnating resin viscosifier and preparation method thereof | |
| CN103288865A (en) | Method for producing tetraethyl orthosilicate by use of organic silicon azeotrope | |
| CN107417920B (en) | System and method for producing high-hydrogen-content silicone oil | |
| CN107189071B (en) | Preparation method of platinum catalyst for liquid silicone rubber | |
| CN107459651A (en) | Organopolysiloxane resins and preparation method thereof | |
| CN100471898C (en) | Method of preparing star-type multi-arm silicon oil | |
| CN102757458B (en) | Method and device for preparing tetramethyldihydrodisiloxane | |
| CN113004525A (en) | Low-viscosity methyl modified polysiloxane and preparation method thereof | |
| CN105461929A (en) | Synthetic method of high-quality phenyl hydrogen-containing silicone oil applied to LED (Light Emitting Diode) packaging | |
| CN106010423B (en) | A kind of preparation method of addition-type silicon rubber adhesion promoters | |
| CN107641466A (en) | A kind of organosilicon solvent-free dip varnish and preparation method thereof | |
| CN106479394A (en) | A kind of preparation method for organic silica gel system viscosifier | |
| CN116284798A (en) | Preparation method of polyurethane modified organosilicon tackifier and application of polyurethane modified organosilicon tackifier in silicone rubber | |
| JPH0616812A (en) | Trifunctional hydrogenated siloxane fluid | |
| CN109337074A (en) | A kind of synthetic method of LED packaging plastic bonding agent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210622 |