CN113999645A - Soft mica plate adhesive and preparation method thereof - Google Patents
Soft mica plate adhesive and preparation method thereof Download PDFInfo
- Publication number
- CN113999645A CN113999645A CN202111159423.4A CN202111159423A CN113999645A CN 113999645 A CN113999645 A CN 113999645A CN 202111159423 A CN202111159423 A CN 202111159423A CN 113999645 A CN113999645 A CN 113999645A
- Authority
- CN
- China
- Prior art keywords
- parts
- mica plate
- temperature
- dimethylbenzene
- adhesive
- 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
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- 239000010445 mica Substances 0.000 title claims abstract description 31
- 229910052618 mica group Inorganic materials 0.000 title claims abstract description 31
- 239000000853 adhesive Substances 0.000 title claims abstract description 24
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims abstract description 36
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000005054 phenyltrichlorosilane Substances 0.000 claims abstract description 10
- ORVMIVQULIKXCP-UHFFFAOYSA-N trichloro(phenyl)silane Chemical compound Cl[Si](Cl)(Cl)C1=CC=CC=C1 ORVMIVQULIKXCP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- 238000006116 polymerization reaction Methods 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000008096 xylene Substances 0.000 description 6
- 239000008399 tap water Substances 0.000 description 4
- 235000020679 tap water Nutrition 0.000 description 4
- 238000000034 method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000010835 comparative analysis Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Silicon Polymers (AREA)
Abstract
The invention belongs to the field of preparation of mica plate adhesives, and provides a soft mica plate adhesive and a preparation method thereof. The adhesive comprises the following raw material components in parts by mass: 20-25 parts of dimethyldichlorosilane, 45-60 parts of dimethylbenzene and 30-35 parts of phenyltrichlorosilane. The adhesive is applied to the mica plate, so that the mica plate can be ensured to have certain softness, certain strength and toughness, and the performance of the mica plate is improved.
Description
Technical Field
The invention belongs to the field of preparation of mica plate adhesives, and particularly relates to a soft mica plate adhesive and a preparation method thereof.
Background
The soft mica plate is made by taking mica paper as a base material and adding an adhesive through processes of sizing, pressing and the like, and is generally used in various motors and household appliances because of excellent performances of high temperature resistance, fire resistance, heat insulation and the like. However, the prior soft mica plate adopts MQ resin and silicon rubber reinforced materials as adhesives, and the processed mica plate is too soft, and the strength and toughness of the mica plate do not meet the application requirements of the soft mica plate.
Disclosure of Invention
The invention aims to provide a soft mica plate adhesive and a preparation method thereof aiming at the defects in the prior art, and the adhesive is applied to a mica plate, so that the mica plate can be ensured to have certain softness and certain strength and toughness.
The object of the invention is achieved by the following technical measures.
The invention provides a soft mica plate adhesive which comprises the following raw material components in parts by mass: 20-25 parts of dimethyldichlorosilane, 45-60 parts of dimethylbenzene and 30-35 parts of phenyltrichlorosilane.
The invention also provides a preparation method of the mica softening plate adhesive, which comprises the following steps:
(1) adding 250 parts of deionized water 200 and 22-28 parts of dimethylbenzene into a three-neck flask with a stirrer, a thermometer and a dropping pipe, and fully stirring;
(2) keeping the temperature in the three-neck flask below 30 ℃, mixing 20-25 parts of dimethyldichlorosilane, 30-35 parts of phenyltrichlorosilane and 80-100 parts of dimethylbenzene, then dropwise adding the mixture into the three-neck flask at a constant speed through a dropwise adding pipe, and continuously stirring for half an hour after dropwise adding;
(3) transferring the materials in the three-mouth flask to a separating funnel, removing the aqueous solution at the lower end, adding water, washing to be neutral, putting the materials into the three-mouth flask with a stirrer, a thermometer and a condenser, adding 0.02-0.05 part of zinc octoate, arranging a conical flask at the tail end of the condenser, heating, stirring, carrying out concentration polymerization, keeping the temperature for half an hour after the temperature is raised to 150-160 ℃, and adding 30-35 parts of dimethylbenzene to prepare the adhesive with 50% solid content after the temperature is lowered to the normal temperature.
Compared with the prior art, the soft mica plate adhesive and the preparation method thereof are applied to the mica plate, can ensure that the mica plate has certain softness, can also ensure that the mica plate has certain strength and toughness, and can also realize different softness requirements by changing the proportion of the dimethyldichlorosilane and the phenyltrichlorosilane.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the implementation methods of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
2200g of deionized water and 220g of dimethylbenzene are added into a three-neck flask provided with a stirrer, a thermometer and a dropping pipe, and the stirrer is opened to fully stir; adding 200g of mixed dimethyldichlorosilane, 300g of phenyltrichlorosilane and 900g of xylene into a dropping pipe, carrying out uniform dropping operation at 30 ℃, and stirring for half an hour after the dropping is finished; transferring the materials in the three-mouth flask to a separating funnel, removing the aqueous solution at the lower end, adding tap water for washing until the materials are neutral, putting the materials into the three-mouth flask with a stirrer, a thermometer and a condenser, adding 0.3g of zinc octoate, arranging a conical flask at the tail end of the condenser, heating and stirring, carrying out concentration polymerization, keeping the temperature for half an hour after the temperature is raised to 155 ℃, adding 310g of dimethylbenzene to prepare the soft mica plate adhesive with the solid content of about 50 percent after the temperature is lowered to the normal temperature.
Example 2
2400g of deionized water and 230g of xylene are added into a three-neck flask provided with a stirrer, a thermometer and a dropping pipe, and the stirrer is opened to fully stir; adding 200g of mixed dimethyldichlorosilane, 350g of phenyltrichlorosilane and 950g of xylene into a dropping pipe, performing uniform dropping operation at 30 ℃, and stirring for half an hour after the dropping operation is finished; transferring the materials in the three-mouth flask to a separating funnel, removing the aqueous solution at the lower end, adding tap water for washing until the materials are neutral, putting the materials into the three-mouth flask with a stirrer, a thermometer and a condenser, adding 0.4g of zinc octoate, arranging a conical flask at the tail end of the condenser, heating and stirring, carrying out concentration polymerization, keeping the temperature for half an hour after the temperature is increased to 160 ℃, adding 320g of dimethylbenzene to prepare the soft mica plate adhesive with the solid content of about 50 percent after the temperature is reduced to the normal temperature.
Example 3
Adding 2500g of deionized water and 260g of dimethylbenzene into a three-neck flask provided with a stirrer, a thermometer and a dropping pipe, and opening the stirrer to fully stir; adding 250g of mixed dimethyldichlorosilane, 300g of phenyltrichlorosilane and 850g of xylene into a dropping pipe, performing uniform dropping operation at 30 ℃, and stirring for half an hour after the dropping operation is finished; transferring the materials in the three-mouth flask to a separating funnel, removing the aqueous solution at the lower end, adding tap water for washing until the materials are neutral, putting the materials into the three-mouth flask with a stirrer, a thermometer and a condenser, adding 0.2g of zinc octoate, arranging a conical flask at the tail end of the condenser, heating and stirring, carrying out concentration polymerization, keeping the temperature for half an hour after the temperature is raised to 150 ℃, adding 300g of dimethylbenzene to prepare the soft mica plate adhesive with the solid content of about 50 percent after the temperature is lowered to the normal temperature.
Example 4
2100g of deionized water and 250g of xylene are added into a three-neck flask provided with a stirrer, a thermometer and a dropping pipe, and the stirrer is opened to fully stir; adding 220g of mixed dimethyldichlorosilane, 350g of phenyltrichlorosilane and 1000g of xylene into a dropping pipe, performing uniform dropping operation at 30 ℃, and stirring for half an hour after the dropping operation is finished; transferring the materials in the three-mouth flask to a separating funnel, removing the aqueous solution at the lower end, adding tap water for washing until the materials are neutral, putting the materials into the three-mouth flask with a stirrer, a thermometer and a condenser, adding 0.4g of zinc octoate, arranging a conical flask at the tail end of the condenser, heating and stirring, carrying out concentration polymerization, keeping the temperature for half an hour after the temperature is increased to 160 ℃, adding 350g of dimethylbenzene to prepare the soft mica plate adhesive with the solid content of about 50 percent after the temperature is reduced to the normal temperature.
Examples 1-4 comparative analysis applied to Soft mica plates
Details not described in this specification are within the skill of the art that are well known to those skilled in the art.
The scope of the invention is not limited to the above-described embodiments, and it is apparent that various modifications and variations can be made to the present invention by those skilled in the art without departing from the scope and spirit of the invention. It is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.
Claims (2)
1. The soft mica plate adhesive is characterized in that: the adhesive comprises the following raw material components in parts by mass: 20-25 parts of dimethyldichlorosilane, 45-60 parts of dimethylbenzene and 30-35 parts of phenyltrichlorosilane.
2. A preparation method of a soft mica plate adhesive is characterized by comprising the following steps:
(1) adding 250 parts of deionized water 200 and 22-28 parts of dimethylbenzene into a three-neck flask with a stirrer, a thermometer and a dropping pipe, and fully stirring;
(2) keeping the temperature in the three-neck flask below 30 ℃, mixing 20-25 parts of dimethyldichlorosilane, 30-35 parts of phenyltrichlorosilane and 80-100 parts of dimethylbenzene, then dropwise adding the mixture into the three-neck flask at a constant speed through a dropwise adding pipe, and continuously stirring for half an hour after dropwise adding;
(3) transferring the materials in the three-mouth flask to a separating funnel, removing the aqueous solution at the lower end, adding water, washing to be neutral, putting the materials into the three-mouth flask with a stirrer, a thermometer and a condenser, adding 0.02-0.05 part of zinc octoate, arranging a conical flask at the tail end of the condenser, heating, stirring, carrying out concentration polymerization, keeping the temperature for half an hour after the temperature is raised to 150-160 ℃, and adding 30-35 parts of dimethylbenzene to prepare the adhesive with the solid content of 50 percent after the temperature is reduced to the normal temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111159423.4A CN113999645A (en) | 2021-09-30 | 2021-09-30 | Soft mica plate adhesive and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111159423.4A CN113999645A (en) | 2021-09-30 | 2021-09-30 | Soft mica plate adhesive and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113999645A true CN113999645A (en) | 2022-02-01 |
Family
ID=79922118
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111159423.4A Pending CN113999645A (en) | 2021-09-30 | 2021-09-30 | Soft mica plate adhesive and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113999645A (en) |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1180848A (en) * | 1956-08-09 | 1959-06-09 | Thomson Houston Comp Francaise | Water resistant mica paper |
| FR1198853A (en) * | 1957-02-13 | 1959-12-10 | Thomson Houston Comp Francaise | Organopolysiloxane-based compositions |
| GB832966A (en) * | 1955-06-13 | 1960-04-21 | Westinghouse Electric Corp | Improvements in or relating to liquid polysiloxanes |
| US4029635A (en) * | 1975-01-15 | 1977-06-14 | General Electric Company | Silicone resins useful for forming mica laminate |
| DE102005030580B3 (en) * | 2005-06-30 | 2006-12-07 | Wacker Chemie Ag | Producing glass-mica tape useful for insulation comprises impregnating mica paper and/or glass cloth with a silicone composition and laminating with mica paper and/or glass cloth and curing |
| CN101343365A (en) * | 2008-08-28 | 2009-01-14 | 杭州师范大学 | Preparation method for methyl phenyl vinyl polysiloxane for packaging LED |
| CN103540289A (en) * | 2013-05-23 | 2014-01-29 | 杭州师范大学 | Preparation method and application of organic silicon resin adhesive |
| CN103881100A (en) * | 2014-02-20 | 2014-06-25 | 常州市嘉诺有机硅有限公司 | Toughened organic silicone high-temperature adhesive resin and preparation process thereof |
| CN108384479A (en) * | 2018-02-01 | 2018-08-10 | 苏州太湖电工新材料股份有限公司 | Adhesive of high heat conduction low resin mica tape and preparation method thereof and low resin mica tape |
-
2021
- 2021-09-30 CN CN202111159423.4A patent/CN113999645A/en active Pending
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB832966A (en) * | 1955-06-13 | 1960-04-21 | Westinghouse Electric Corp | Improvements in or relating to liquid polysiloxanes |
| FR1180848A (en) * | 1956-08-09 | 1959-06-09 | Thomson Houston Comp Francaise | Water resistant mica paper |
| FR1198853A (en) * | 1957-02-13 | 1959-12-10 | Thomson Houston Comp Francaise | Organopolysiloxane-based compositions |
| US4029635A (en) * | 1975-01-15 | 1977-06-14 | General Electric Company | Silicone resins useful for forming mica laminate |
| DE102005030580B3 (en) * | 2005-06-30 | 2006-12-07 | Wacker Chemie Ag | Producing glass-mica tape useful for insulation comprises impregnating mica paper and/or glass cloth with a silicone composition and laminating with mica paper and/or glass cloth and curing |
| CN101343365A (en) * | 2008-08-28 | 2009-01-14 | 杭州师范大学 | Preparation method for methyl phenyl vinyl polysiloxane for packaging LED |
| CN103540289A (en) * | 2013-05-23 | 2014-01-29 | 杭州师范大学 | Preparation method and application of organic silicon resin adhesive |
| CN103881100A (en) * | 2014-02-20 | 2014-06-25 | 常州市嘉诺有机硅有限公司 | Toughened organic silicone high-temperature adhesive resin and preparation process thereof |
| CN108384479A (en) * | 2018-02-01 | 2018-08-10 | 苏州太湖电工新材料股份有限公司 | Adhesive of high heat conduction low resin mica tape and preparation method thereof and low resin mica tape |
Non-Patent Citations (3)
| Title |
|---|
| 《云母综合利用》编写组: "《云母综合利用》", 29 February 1984, 中国建筑工业出版社 * |
| 李步春: "甲基硅树脂合成新工艺", 《有机硅材料》 * |
| 陆宪良等: "有机硅胶粘剂在耐火云母带中的应用", 《华东理工大学学报》 * |
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| PB01 | Publication | ||
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20220201 |
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| RJ01 | Rejection of invention patent application after publication |