CN115926712A - Bi-component silane modified polyether conductive sealant and preparation method thereof - Google Patents

Bi-component silane modified polyether conductive sealant and preparation method thereof Download PDF

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CN115926712A
CN115926712A CN202211743029.XA CN202211743029A CN115926712A CN 115926712 A CN115926712 A CN 115926712A CN 202211743029 A CN202211743029 A CN 202211743029A CN 115926712 A CN115926712 A CN 115926712A
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component
parts
polyether
modified polyether
silane
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袁胤纶
杨传伟
薛有泉
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Guangzhou Baiyun Chemical Industry Co Ltd
Guangdong Baiyun Technology Co Ltd
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Guangzhou Baiyun Chemical Industry Co Ltd
Guangdong Baiyun Technology Co Ltd
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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Abstract

The invention relates to a two-component silane modified polyether conductive sealant and a preparation method thereof, wherein silane modified polyether is used as a basic prepolymer, a two-component conductive silane modified polyether adhesive is developed, after A and B components are mixed, the inner layer and the outer layer of the adhesive are cured simultaneously, the adhesive can be completely cured basically for about 2d, the deep layer curing speed is high, the adhesive has excellent advantages in the application of repairing and filling joints of some deep conductive modules and the like, and the storage period and the working life of the adhesive are prolonged relative to a single-component formula; meanwhile, the modified carbon nano tube is added, so that the silane modified polyether adhesive has good conductivity.

Description

Bi-component silane modified polyether conductive sealant and preparation method thereof
Technical Field
The invention belongs to the technical field of sealants, and particularly relates to a bi-component silane modified polyether conductive sealant and a preparation method thereof.
Background
The conductive adhesive is an adhesive with certain conductive performance after being cured or dried, and generally takes matrix resin and conductive filler, namely conductive particles as main components, and the conductive particles are combined together through the bonding action of the matrix resin to form a conductive path so as to realize the conductive connection of bonded materials. Most of the conductive adhesives used in the current market are filler type, and are mainly epoxy, polyurethane and acrylic resin. The epoxy adhesive has high bonding strength, wide bonding range and high hardness, but the epoxy adhesive has relatively poor elasticity due to high crosslinking density of the polymer, is brittle after curing, and is limited to be used in places with certain displacement capacity; polyurethanes also have relatively high bond strengths, and suffer from the disadvantages of being environmentally unfriendly, relatively poor alkali resistance when prepared, and releasing CO during crosslinking 2 Certain corrosion may be caused during application; acrylic resins have good optical properties, are resistant to water, oil and alkali, and have the defects of poor heat resistance and easy cracking when the environmental temperature changes rapidly.
The silane modified polyether has the characteristics that the main chain is polyether and the end group is blocked by silane, so the silane modified polyether has the advantages of silicone adhesive and polyurethane adhesive, has wide adhesive range, high adhesive strength, good elasticity and impact resistance, releases few small molecules during curing, and hardly causes corrosion to a substrate and the environment during application. At present, researches on conductive polyether adhesives are relatively few, and Chinese patent CN110527474A invents a single-component conductive silane modified polyether adhesive, but because the curing speed of the single component is basically 3-6mm/24h, deep curing cannot be rapidly realized in an application scene needing deep rapid curing, and the failure is caused. Therefore, it is necessary to provide a silane modified polyether conductive sealant which can rapidly realize deep curing.
Disclosure of Invention
The invention aims to develop a bi-component silane modified polyether conductive sealant, which is cured from inside to outside simultaneously after two components are mixed, so as to achieve the purpose of quick curing.
The invention also aims to provide a preparation method of the two-component silane modified polyether conductive sealant.
The technical scheme adopted for realizing the aim of the invention is as follows:
the bi-component silane modified polyether conductive sealant is characterized by comprising a component A and a component B, wherein the component A comprises the following raw materials in parts by weight:
Figure BDA0004030778370000021
the component B comprises the following raw materials in parts by weight:
Figure BDA0004030778370000022
wherein the modified carbon nano tube is obtained by the following method: 1) Heating chemical vapor deposition equipment to 700-900 ℃, firstly introducing a hydrogen and nitrogen mixed gas on a gold-plated silicon wafer substrate, then introducing ethylene gas, and obtaining a carbon nano tube after 5-10 min; 2) Adding the carbon nano tube and the coupling agent into 10 parts of toluene solvent according to the mass ratio of 1.1: 1, fully mixing and reacting for 10-15 min, and performing suction filtration to obtain the modified carbon nano tube.
The silane modified polyether is one or more of dimethoxy silyl terminated polyether, diethoxy silyl terminated polyether, trimethoxy silyl terminated polyether and triethoxy silyl terminated polyether.
The coupling agent is one or more than one of gamma-aminopropyltriethoxysilane, N-aminoethyl-gamma-aminopropyltrimethoxysilane, N-aminoethyl-gamma-aminopropyltriethoxysilane and gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane.
The reinforcing filler is one or a mixture of more than one of nano calcium carbonate, heavy calcium carbonate, silica micropowder, talcum powder and kaolin.
The thixotropic agent is one or a mixture of more than one of polyamide wax, fumed silica, nanoscale diatomite and hydrogenated castor oil; the light stabilizer is one or more of a mixture of a Pasteur ultraviolet absorbent Tinuvin UV-P, tinuvin UV-9, tinuvin 326, tinuvin 540 and Tinuvin 770; the heat stabilizer is one or a mixture of more than one of Pasteur antioxidants Irganox 245, irganox 1010 and Irganox 1035.
The plasticizer is one or a mixture of more than one of polyether polyol plasticizer and phthalate plasticizer; the catalyst is one or more of dibutyltin dilaurate (DBTDL), dioctyltin diacetate, chelated tin, stannous octoate or diorganotin bis (beta-diketone ester).
The preparation method of the bi-component silane modified polyether conductive sealant is characterized by comprising the following steps:
1) Adding silane modified polyether, modified carbon nano tubes, reinforcing filler, thixotropic agent, light stabilizer, heat stabilizer and plasticizer into a kneading machine for vacuum high-speed kneading, wherein the material temperature is 60-120 ℃, the vacuum degree is-0.06-0.099 MPa, the mixing time is 60-180min, and the component A is obtained after cooling to the normal temperature;
2) Adding the reinforcing filler, the plasticizer, the coupling agent and the catalyst into a high-speed dispersion machine according to the formula ratio, stirring for 30-60 min at a high speed in vacuum, wherein the vacuum degree is-0.06-0.099 MPa, and cooling to normal temperature to obtain the component B.
According to the invention, silane modified polyether is used as a basic prepolymer, a two-component conductive silane modified polyether adhesive is developed, after the A component and the B component are mixed, the adhesive is cured from inside to outside at the same time, the adhesive can be completely cured within about 2d basically, the deep curing speed is high, the adhesive has excellent advantages in the application of repairing and filling joints of some deep conductive modules and the like, and the storage period and the application life of the adhesive are prolonged relative to a single-component formula; meanwhile, the silane modified polyether adhesive is endowed with good conductivity by adding the modified carbon nano tube.
Detailed Description
The following detailed description of the embodiments of the present invention is provided by way of specific examples, which are provided to facilitate understanding and application of the present invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles defined herein may be applied to other embodiments without the use of inventive faculty. Therefore, the present application is not limited to the embodiments herein, and those skilled in the art, in light of the present disclosure, will recognize that changes may be made in the form and detail of the embodiments without departing from the scope or spirit of the application.
The modified carbon nanotubes were obtained in the following examples:
1) Heating chemical vapor deposition equipment to 800 ℃, firstly introducing a mixed gas of hydrogen and nitrogen on a gold-plated silicon wafer substrate, then introducing ethylene gas, and obtaining a carbon nano tube after 10 min; 2) Adding the carbon nano tube and the coupling agent into 10 parts of toluene solvent according to the mass ratio of 1.1: 1, fully mixing and reacting for 12min, and performing suction filtration to obtain the modified carbon nano tube.
Example 1
The bi-component silane modified polyether conductive sealant is prepared by the following steps of:
1) Preparation of a component A:
100 parts of trimethoxysilyl-terminated polyether, 40 parts of modified carbon nanotube, 70 parts of nano calcium carbonate, 5 parts of polyamide wax, 6 parts of Tinuvin 326,6 parts of Irganox 1010 and 10 parts of polyoxypropylene triol PPG3000 are added into a kneader, mixed at a high speed for 120min at a temperature of 90 ℃ and a vacuum degree of-0.09 MPa, and cooled to normal temperature to prepare the component A.
2) B, preparation of a component:
adding 50 parts of heavy calcium carbonate, 40 parts of DIDP (diisodecyl phthalate), 8 parts of N-aminoethyl-gamma-aminopropyltrimethoxysilane and 0.5 part of DBTDL into a reaction kettle, stirring at high speed in vacuum with the vacuum degree of-0.09 MPa, blending for 40min, and cooling to normal temperature to obtain the component B.
When in use, the component A and the component B are uniformly mixed according to the volume ratio of 1: 1 to prepare the bi-component silane modified polyether conductive sealant, and the performance indexes are shown in table 1.
Example 2
The bi-component silane modified polyether conductive sealant is prepared by the following steps of:
1) Preparation of a component A:
100 parts of trimethoxysilyl-terminated polyether, 70 parts of modified carbon nano tube, 70 parts of nano calcium carbonate, 3 parts of polyamide wax, 6 parts of Tinuvin 326,6 parts of Irganox 1010 and 30 parts of polyoxypropylene triol PPG3000 are added into a kneader, and the mixture is mixed at a high speed for 150min at a temperature of 90 ℃ and a vacuum degree of-0.09 MPa, and cooled to normal temperature to prepare the component A.
2) B, preparation of a component:
60 parts of heavy calcium carbonate, 50 parts of DIDP,10 parts of gamma-aminopropyltriethoxysilane and 0.8 part of DBTDL are added into a reaction kettle, stirred at high speed in vacuum with the vacuum degree of-0.09 MPa, blended for 40min and cooled to normal temperature to prepare the component B.
When in use, the component A and the component B are uniformly mixed according to the volume ratio of 1: 1 to prepare the bi-component silane modified polyether conductive sealant, and the performance indexes are shown in table 1.
Example 3
The bi-component silane modified polyether conductive sealant is prepared by the following steps of:
1) Preparing a component A:
100 parts of trimethoxysilyl-terminated polyether, 100 parts of modified carbon nano tube, 70 parts of heavy calcium carbonate, 6 parts of hydrogenated castor oil, 6 parts of Tinuvin 326,6 parts of Irganox 1010 and 20 parts of polyoxypropylene triol PPG3000 are added into a kneader, mixed at a high speed for 150min at a temperature of 90 ℃ and a vacuum degree of-0.09 MPa, and cooled to normal temperature to prepare the component A.
2) B, preparation of a component:
adding 50 parts of kaolin, 50 parts of DIDP,5 parts of N-aminoethyl-gamma-aminopropyltrimethoxysilane and 0.8 part of DBTDL into a reaction kettle, stirring at high speed in vacuum with the vacuum degree of-0.09 MPa, blending for 40min, and cooling to normal temperature to obtain the component B.
When in use, the component A and the component B are uniformly mixed according to the volume ratio of 1: 1 to prepare the bi-component silane modified polyether conductive sealant, and the performance indexes are shown in table 1.
Example 4
The bi-component silane modified polyether conductive sealant is prepared by the following steps of:
1) Preparing a component A:
100 parts of dimethoxy silyl terminated polyether, 40 parts of modified carbon nanotube, 70 parts of nano calcium carbonate, 5 parts of fumed silica, 6 parts of Tinuvin 326,6 parts of Irganox 1010 and 10 parts of polyoxypropylene glycol PPG2000 are added into a kneader, and the components are mixed at a high speed for 120min at a temperature of 90 ℃ and a vacuum degree of-0.09 MPa, and cooled to normal temperature to prepare the component A.
2) B, preparation of a component:
taking 50 parts of kaolin, 40 parts of DIDP,8 parts of N-aminoethyl-gamma-aminopropyltrimethoxysilane and 1.2 parts of chelated tin, adding into a reaction kettle, stirring at high speed in vacuum with the vacuum degree of-0.09 MPa, blending for 40min, and cooling to normal temperature to obtain the component B.
When in use, the component A and the component B are uniformly mixed according to the volume ratio of 1: 1 to prepare the bi-component silane modified polyether conductive sealant, and the performance indexes are shown in table 1.
Example 5
The bi-component silane modified polyether conductive sealant is prepared by the following steps of:
1) Preparation of a component A:
100 parts of dimethoxy silyl terminated polyether, 70 parts of modified carbon nano tube, 70 parts of nano calcium carbonate, 4 parts of polyamide wax, 6 parts of Tinuvin 326,6 parts of Irganox 1010 and 10 parts of polyoxypropylene glycol PPG2000 are added into a kneader, mixed at a high speed for 120min at a temperature of 90 ℃ and a vacuum degree of-0.09 MPa, and cooled to normal temperature to prepare the component A.
2) B, preparation of a component:
adding 60 parts of heavy calcium carbonate, 50 parts of DIDP,5 parts of N-aminoethyl-gamma-aminopropyltrimethoxysilane and 1.8 parts of chelated tin into a reaction kettle, stirring at high speed in vacuum with the vacuum degree of-0.09 MPa, blending for 40min, and cooling to normal temperature to obtain the component B.
When in use, the component A and the component B are uniformly mixed according to the volume ratio of 1: 1 to prepare the bi-component silane modified polyether conductive sealant, and the performance indexes are shown in table 1.
Comparative example 1
The silane modified polyether adhesive of the comparative example is prepared by the following method in parts by weight:
1) Preparation of a component A:
100 parts of trimethoxysilyl terminated polyether, 110 parts of nano calcium carbonate, 5 parts of polyamide wax, 6 parts of Tinuvin 326,6 parts of Irganox 1010 and 10 parts of polyoxypropylene triol PPG3000 are added into a kneader, and the mixture is mixed at a high speed for 120min at the temperature of 90 ℃ and the vacuum degree of-0.09 MPa, and is cooled to normal temperature to prepare the component A.
3) B, preparation of a component:
adding 50 parts of heavy calcium carbonate, 40 parts of DIDP,8 parts of N-aminoethyl-gamma-aminopropyltrimethoxysilane and 0.5 part of DBTDL into a reaction kettle, stirring at high speed in vacuum with the vacuum degree of-0.09 MPa, blending for 40min, and cooling to normal temperature to obtain the component B.
When the adhesive is used, the component A and the component B are uniformly mixed according to the volume ratio of 1: 1 to prepare the double-component silane modified polyether adhesive, and the performance indexes are shown in table 1.
Comparative example 2
The silane modified polyether gum of the embodiment is prepared by the following method in parts by weight:
1) Preparation of a component A:
100 parts of trimethoxysilyl-terminated polyether, 40 parts of silver powder, 70 parts of nano calcium carbonate, 5 parts of polyamide wax, 6 parts of Tinuvin 326,6 parts of Irganox 1010 and 10 parts of PPG3000 are added into a kneader, and are mixed at a high speed for 120min at a temperature of 90 ℃ and a vacuum degree of-0.09 MPa, and the mixture is cooled to normal temperature to obtain the component A.
3) B, preparation of a component:
adding 50 parts of heavy calcium carbonate, 40 parts of DIDP,8 parts of N-aminoethyl-gamma-aminopropyltrimethoxysilane and 0.5 part of DBTDL into a reaction kettle, stirring at high speed in vacuum with the vacuum degree of-0.09 MPa, blending for 40min, and cooling to normal temperature to obtain the component B.
When the conductive polyether adhesive is used, the component A and the component B are uniformly mixed according to the volume ratio of 1: 1 to prepare the double-component silane modified conductive polyether adhesive, and the performance indexes are shown in table 1.
TABLE 1 product Performance index
Figure BDA0004030778370000061
As can be seen from Table 1, the conductive effect of the two-component silane modified polyether conductive sealant prepared by adding the modified carbon nanotubes is more excellent than that of the two-component silane modified conductive polyether sealant prepared by adopting the traditional conductive material.

Claims (7)

1. The bi-component silane modified polyether conductive sealant is characterized by comprising a component A and a component B, wherein the component A comprises the following raw materials in parts by weight:
Figure QLYQS_1
the component B comprises the following raw materials in parts by weight:
Figure QLYQS_2
wherein the modified carbon nano tube is obtained by the following method: 1) Heating chemical vapor deposition equipment to 700-900 ℃, firstly introducing a hydrogen and nitrogen mixed gas on a gold-plated silicon wafer substrate, then introducing ethylene gas, and obtaining a carbon nano tube after 5-10 min; 2) Adding the carbon nano tube and the coupling agent into 10 parts of toluene solvent according to the mass ratio of 1.1: 1, fully mixing and reacting for 10-15 min, and performing suction filtration to obtain the modified carbon nano tube.
2. The two-component silane-modified polyether conductive sealant according to claim 1, wherein the silane-modified polyether is one or more of dimethoxysilyl terminated polyether, diethoxysilyl terminated polyether, trimethoxysilyl terminated polyether and triethoxysilyl terminated polyether.
3. The two-part silane-modified polyether conductive sealant according to claim 1, wherein the coupling agent is one or more selected from the group consisting of γ -aminopropyltriethoxysilane, N-aminoethyl- γ -aminopropyltrimethoxysilane, N-aminoethyl- γ -aminopropyltriethoxysilane, and γ - (2, 3-epoxypropoxy) propyltrimethoxysilane.
4. The two-component silane-modified polyether conductive sealant as claimed in claim 1, wherein the reinforcing filler is one or more of nano calcium carbonate, ground calcium carbonate, silica micropowder, talc powder and kaolin.
5. The two-component silane-modified polyether conductive sealant according to claim 1, wherein the thixotropic agent is one or more of polyamide wax, fumed silica, nano-scale diatomite and hydrogenated castor oil; the light stabilizer is one or more of a mixture of a Pasteur ultraviolet absorbent Tinuvin UV-P, tinuvin UV-9, tinuvin 326, tinuvin 540 and Tinuvin 770; the heat stabilizer is one or a mixture of more than one of Pasteur antioxidants Irganox 245, irganox 1010 and Irganox 1035.
6. The two-component silane modified polyether conductive sealant as claimed in claim 1, wherein the plasticizer is one or a mixture of more than one of polyether polyol plasticizer and phthalate plasticizer; the catalyst is one or more of dibutyltin dilaurate, dioctyltin diacetate, chelated tin, stannous octoate or diorganotin bis (beta-diketone ester).
7. The preparation method of the two-component silane modified polyether conductive sealant as claimed in claims 1 to 6, which is characterized by comprising the following steps:
1) Adding silane modified polyether, modified carbon nano tubes, reinforcing filler, thixotropic agent, light stabilizer, heat stabilizer and plasticizer into a kneading machine for vacuum high-speed kneading, wherein the material temperature is 60-120 ℃, the vacuum degree is-0.06-0.099 MPa, the mixing time is 60-180min, and the component A is obtained after cooling to normal temperature;
2) Adding the reinforcing filler, the plasticizer, the coupling agent and the catalyst into a high-speed dispersion machine according to the formula ratio, stirring for 30-60 min at a high speed in vacuum, wherein the vacuum degree is-0.06-0.099 MPa, and cooling to normal temperature to obtain the component B.
CN202211743029.XA 2022-12-30 2022-12-30 Bi-component silane modified polyether conductive sealant and preparation method thereof Pending CN115926712A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030202930A1 (en) * 2002-04-30 2003-10-30 Dodelet Jean Pol Process for preparing carbon nanotubes
US20110064645A1 (en) * 2009-09-14 2011-03-17 National Cheng Kung University Carbon nanotube and method for producing the same
CN103937258A (en) * 2014-04-02 2014-07-23 山东大学 Conductive silicone rubber with high elastic resilience and preparation method thereof
CN110527474A (en) * 2019-09-06 2019-12-03 武汉奥克特种化学有限公司 A kind of silane modified polyether Conductive sealant and preparation method thereof
CN111171757A (en) * 2020-02-26 2020-05-19 广州市白云化工实业有限公司 Modified carbon nanotube, epoxy conductive adhesive and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030202930A1 (en) * 2002-04-30 2003-10-30 Dodelet Jean Pol Process for preparing carbon nanotubes
US20110064645A1 (en) * 2009-09-14 2011-03-17 National Cheng Kung University Carbon nanotube and method for producing the same
CN103937258A (en) * 2014-04-02 2014-07-23 山东大学 Conductive silicone rubber with high elastic resilience and preparation method thereof
CN110527474A (en) * 2019-09-06 2019-12-03 武汉奥克特种化学有限公司 A kind of silane modified polyether Conductive sealant and preparation method thereof
CN111171757A (en) * 2020-02-26 2020-05-19 广州市白云化工实业有限公司 Modified carbon nanotube, epoxy conductive adhesive and preparation method thereof

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