CN114369184A - Modified rubber and high-performance foam and adhesive tape prepared from same - Google Patents
Modified rubber and high-performance foam and adhesive tape prepared from same Download PDFInfo
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- CN114369184A CN114369184A CN202111644259.6A CN202111644259A CN114369184A CN 114369184 A CN114369184 A CN 114369184A CN 202111644259 A CN202111644259 A CN 202111644259A CN 114369184 A CN114369184 A CN 114369184A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/42—Introducing metal atoms or metal-containing groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/32—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof from compositions containing microballoons, e.g. syntactic foams
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- 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
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/26—Porous or cellular plastics
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/22—Expandable microspheres, e.g. Expancel®
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2353/00—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers
- C08J2353/02—Characterised by the use of block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Derivatives of such polymers of vinyl aromatic monomers and conjugated dienes
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- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/124—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present on both sides of the carrier, e.g. double-sided adhesive tape
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- 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
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
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- 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
- C09J2400/00—Presence of inorganic and organic materials
- C09J2400/20—Presence of organic materials
- C09J2400/24—Presence of a foam
- C09J2400/243—Presence of a foam in the substrate
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- 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
- C09J2433/00—Presence of (meth)acrylic polymer
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- 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
- C09J2453/00—Presence of block copolymer
- C09J2453/006—Presence of block copolymer in the substrate
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- Adhesive Tapes (AREA)
Abstract
The invention discloses a modified rubber and high-performance foam and adhesive tape prepared from the same, wherein SBS or SIS rubber is modified, small molecules containing C (N) O are bonded to a rubber molecular chain to obtain the modified rubber with high adhesive force, so that the high-performance foam is prepared, and C (N) O can be crosslinked with acrylic adhesives on two sides, so that a firm bridge is erected between a rubber foam base material and the acrylic adhesive to solve the problem of adhesive force between the rubber foam base material and the acrylic adhesive, the defect that the conventional rubber foam base material and the pressure-sensitive adhesive have insufficient adhesive force and cannot meet the high-performance requirement is overcome, the adhesive force between the rubber foam base material and the pressure-sensitive adhesive is enhanced, the excellent impact resistance of the rubber foam base material is retained, and the application space in the field of the impact-resistant pressure-sensitive adhesive in China is wide.
Description
Technical Field
The invention relates to the technical field of pressure-sensitive adhesives, in particular to a modified rubber and high-performance foam and adhesive tape prepared from the modified rubber.
Background
In the development of adhesive tapes for 3C products, a substrate such as PET, foam, rubber, etc. is generally required to provide a supporting, cushioning or strength-increasing effect according to its application environment. Once the base material is introduced, the problem of base material adhesion is necessarily involved, wherein rubber is more difficult to adhere to the pressure-sensitive adhesive, and compared with the conventional method of applying corona to the surface of the rubber base material, the method can increase the surface energy of the base material to a certain extent so as to increase the adhesion, but when higher requirements are made on the performance of products such as buffer resistance, shear resistance and the like, the base material and the surface adhesive are generally cracked due to insufficient adhesion; the other method is to perform priming on the surface of a rubber substrate to increase the surface energy, and the method has the disadvantages that on one hand, some chemical components in part of the priming agent can damage the substrate to different degrees to cause the substrate to lose the original strength or elasticity, and on the other hand, the priming agent and corona striking are similar to each other and belong to physical methods to increase the adhesive force, and the priming agent cannot meet the requirements when the product has higher requirements.
Disclosure of Invention
The invention aims to provide a modified rubber and high-performance foam and adhesive tape prepared from the modified rubber, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme: the modified rubber comprises the following components in parts by weight: 80-120 parts of rubber, 15-55 parts of bifunctional micromolecules, 0.0001-0.1 part of platinum catalyst, 300-450 parts of toluene and 1-3 parts of antioxidant;
the structural formula of the bifunctional small molecule is as follows:
further, the rubber is any one of SBS rubber or SIS rubber; the antioxidant is antioxidant 1010.
A preparation method of modified rubber comprises the following steps:
s1, preparing bifunctional small molecules
a. To a reaction charged with tolueneAdding siloxane with hydroxyl end-capped side chain containing vinyl and siloxane with hydrogen end-capped into a container, magnetically stirring, and introducing N2Protecting, namely adding an alkynol inhibitor, heating to 70 ℃ in an oil bath, adding a platinum catalyst, and reacting for 3-4 hours to obtain siloxane with a side chain containing a silicon-hydrogen active group, wherein the siloxane is a first intermediate;
b. adding isophorone diisocyanate and dibutyltin dilaurate catalyst into a reaction vessel filled with toluene, magnetically stirring, and introducing N2Protecting, heating the oil bath to 70 ℃, slowly dropwise adding the first intermediate into the container, continuously detecting the content of O-C-N groups during the reaction, and cooling and discharging when the content is less than one third of the added amount to obtain the bifunctional micromolecules;
s2, adding rubber and toluene into the reaction vessel, and introducing N2Protecting, heating the oil bath to 35-45 ℃, stirring for 1-2h until the rubber is dissolved, heating the oil bath to 75 ℃, adding the bifunctional micromolecules into the reaction vessel, stirring for 0.3-0.5h, adding the platinum catalyst, continuously stirring for reaction for 4-5h, adding the antioxidant, uniformly mixing, stopping heating, cooling the rubber in the reaction vessel to 20-40 ℃, and discharging to obtain the modified rubber.
Further, in step S1, the molar ratio of the hydroxyl-terminated side chain vinyl-containing siloxane to the hydrogen-terminated siloxane to the alkynol inhibitor to the platinum catalyst to the isophorone diisocyanate to the dibutyltin dilaurate catalyst is 1: 1.1: (0.0001-0.001): (0.0001-0.001): 2: (0.00001-0.001).
When the base material of the conventional impact-resistant adhesive tape is selected, the requirement on the base material is not high, the conventional rubber base material can be used for meeting the supporting, buffering or strength increasing effects of the adhesive tape, but when the working environment has higher requirements on the performance of a product, the adhesive tape is cracked and the product is damaged frequently due to insufficient adhesive force between the base material and the pressure-sensitive adhesive, so that the problem of the adhesive force between the rubber base material and the pressure-sensitive adhesive is improved, and the high-performance foam adhesive tape is prepared on the basis.
The structure of the rubber base material is adjusted, and when the modified rubber is synthesized, the self-prepared bifunctional micromolecules are added to modify SIS or SBS rubber, the main chain of the bifunctional micromolecules is a silicon chain, the side chain contains Si-H, and the bifunctional micromolecules can perform addition reaction with C-C double bonds of the SIS or SBS rubber, so that the SIS or SBS rubber contains O-C-N.
When the acrylic pressure-sensitive adhesive is attached to the acrylic pressure-sensitive adhesive, OH or COOH contained in the acrylic pressure-sensitive adhesive is combined with O-C-N to perform a crosslinking reaction, so that the adhesive force of the acrylic pressure-sensitive adhesive to a rubber substrate is remarkably increased.
Further, the high-performance foam prepared from the modified rubber comprises the following components in parts by weight: 10-50 parts of ethyl ester, 0.15-3 parts of foaming agent, 95-175 parts of modified rubber, 0.5-3 parts of black color paste and 0.5-3 parts of curing agent.
A preparation method of high-performance foam prepared from modified rubber comprises the following steps: adding ethyl ester and a foaming agent into a reaction container, adding modified rubber after uniform dispersion, stirring for 10-15min, adding black color paste, continuing to stir for 15-25min, adding a curing agent, continuing to stir for 10-15min to obtain mixed glue, coating the mixed glue on a release film by using a scraper type coating machine, heating and drying the mixed glue, and drying and peeling to obtain the high-performance foam.
Furthermore, the foaming agent is an expandable microspheric foaming agent, and the curing agent is an isocyanate curing agent in parts by weight.
Further, the heating and drying apparatus is an oven, the temperature gradient of the oven is set to 50 ℃, 60 ℃, 85 ℃, 110 ℃, 155 ℃ and 110 ℃, and the time of each temperature gradient is 3 min.
Further, the thickness of the high-performance foam is 60-100 μm, and the release film is a 50 μm transparent PET release film.
A modified rubber high-performance foam adhesive tape comprises high-performance foam and acrylic pressure-sensitive adhesive coated on two sides of the high-performance foam.
Compared with the prior art, the invention has the following beneficial effects: according to the invention, SBS or SIS rubber is modified, small molecules containing C-N-O are bonded to a rubber molecular chain, and C-N-O can be crosslinked with acrylic adhesive on two sides, so that a firm bridge is erected between a rubber base material and the acrylic adhesive to solve the problem of adhesive force between the rubber base material and the acrylic adhesive, the defects that the conventional rubber base material and the pressure-sensitive adhesive are insufficient in adhesive force and cannot meet high-performance requirements are overcome, the excellent impact resistance of the rubber base material is maintained while the problem of adhesive force between the rubber base material and the pressure-sensitive adhesive is enhanced, and the application space in the field of impact-resistant pressure-sensitive adhesives in China is wide.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a structural formula of a bifunctional small molecule prepared by the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments 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 of the 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
S1, placing 1mol of siloxane with hydroxyl-terminated side chain containing vinyl and 1.1mol of siloxane with hydrogen-terminated end into a container containing a magnetic stirring bar and a toluene solvent, and introducing N2And (3) protecting, adding 0.01mmol of alkynol inhibitor, heating to 70 ℃, adding 0.1mmol of platinum catalyst, and reacting in a silicon oil bath for 3-4 hours to obtain siloxane with a side chain containing a silicon-hydrogen active group, wherein the siloxane is a first intermediate.
S2, placing 2mol of isophorone diisocyanate and 0.01mmol of dibutyltin dilaurate catalyst into a container containing a magnetic stirrer and toluene, and introducing N2Protection, 1mol of the first intermediate is slowly added dropwise into a container at 70 ℃, and the reaction period is determined by detecting the content of O ═ C ═ N groupsAnd (3) in the reaction process, when the content of the bifunctional micromolecules is less than one third of the addition amount, cooling and discharging, and storing in a dark place to obtain the bifunctional micromolecules.
S3, adding 100g of SIS and 400g of toluene into a container with a mechanical stirring device, and introducing N2Protecting, heating to 40 ℃ inside the solution, and stirring for 1-2h until the rubber is dissolved; and heating to 75 ℃, adding 20g of bifunctional micromolecules into the container, stirring for 0.3h, adding 0.7mg of platinum catalyst, continuing to react for 4-5h, adding 10101.5 g of antioxidant, cooling and discharging to obtain the modified rubber.
S4, adding 0.2g of expandable microsphere foaming agent into 12g of ethyl ester, uniformly dispersing, adding into 100g of modified rubber solution, stirring for 10min, adding 1g of black color paste into the mixture, stirring for 20min, finally adding 1g of isocyanate curing agent into the mixture, stirring for 10min, coating 80um dry glue on a 50um transparent PET release film through a scraper type coating machine, setting the temperature gradient of an oven to be 50 ℃, 60 ℃, 85 ℃, 110 ℃, 155 ℃ and 110 ℃, and setting the time of each temperature gradient to be 3min to obtain high-performance foam; and (3) coating acrylic pressure-sensitive adhesive with the thickness of 50 mu m on two sides to obtain the impact-resistant adhesive tape.
Example 2
This example increased the amount of difunctional small molecule added in step S3 compared to example 1.
1.1mol of siloxane with hydroxyl end-capped side chain containing vinyl and 1.1mol of siloxane with hydrogen end-capped side chain are placed in a container with a magnetic stirring bar and a toluene solvent, and N is introduced2And (3) protecting, adding 0.01mmol of alkynol inhibitor, heating to 70 ℃, adding 0.1mmol of platinum catalyst, and reacting in a silicon oil bath for 3-4 hours to obtain siloxane with a side chain containing a silicon-hydrogen active group, wherein the siloxane is a first intermediate.
2. 2mol of isophorone diisocyanate and 0.01mmol of dibutyltin dilaurate catalyst are placed in a container containing a magnetic stirrer and toluene, and then N is introduced2Protection, slowly dripping 1mol of the first intermediate into a container at 70 ℃, determining the reaction process by detecting the content of O ═ C ═ N groups during the reaction, cooling and discharging when the content is less than one third of the addition amount, and keeping the temperature away from lightAnd storing to obtain the bifunctional group micromolecule.
3. 100g of SIS and 400g of toluene are introduced into a vessel equipped with a mechanical stirring device and then N is introduced2Protecting, heating to 40 ℃ inside the solution, and stirring for 1-2h until the rubber is dissolved; and heating to 75 ℃, adding 30g of bifunctional micromolecules into the container, stirring for 0.3h, adding 0.7mg of platinum catalyst, continuing to react for 4-5h, adding 10101.5 g of antioxidant, cooling and discharging to obtain the modified rubber.
4. Adding 0.2g of expandable microsphere foaming agent into 12g of ethyl ester, uniformly dispersing, adding into 100g of modified rubber solution, stirring for 10min, adding 1g of black color paste into the mixture, stirring for 20min, finally adding 1g of isocyanate curing agent into the mixture, stirring for 10min, coating 80um dry glue on a 50um transparent PET release film by a scraper type coating machine, setting the temperature gradient of an oven to be 50 ℃, 60 ℃, 85 ℃, 110 ℃, 155 ℃ and 110 ℃, and setting the time of each temperature gradient to be 3min to obtain high-performance foam; and (3) coating acrylic pressure-sensitive adhesive with the thickness of 50 mu m on two sides to obtain the impact-resistant adhesive tape.
Example 3
This example increased the amount of difunctional small molecule added in step S3 compared to example 1.
1.1mol of siloxane with hydroxyl end-capped side chain containing vinyl and 1.1mol of siloxane with hydrogen end-capped side chain are placed in a container with a magnetic stirring bar and a toluene solvent, and N is introduced2And (3) protecting, adding 0.01mmol of alkynol inhibitor, heating to 70 ℃, adding 0.1mmol of platinum catalyst, and reacting in a silicon oil bath for 3-4 hours to obtain siloxane with a side chain containing a silicon-hydrogen active group, wherein the siloxane is a first intermediate.
2. 2mol of isophorone diisocyanate and 0.01mmol of dibutyltin dilaurate catalyst are placed in a container containing a magnetic stirrer and toluene, and then N is introduced2And (3) protection, slowly dropwise adding 1mol of the first intermediate into a container at 70 ℃, determining the reaction process by detecting the content of O ═ C ═ N groups during the reaction, and when the content is less than one third of the addition amount, cooling and discharging, and storing in a dark place to obtain the bifunctional micromolecules.
3. 100g of the powderSIS and 400g toluene were charged into a vessel equipped with a mechanical stirring device, and N was introduced2Protecting, heating to 40 ℃ inside the solution, and stirring for 1-2h until the rubber is dissolved; and heating to 75 ℃, adding 45g of bifunctional micromolecules into the container, stirring for 0.3h, adding 0.7mg of platinum catalyst, continuing to react for 4-5h, adding 10101.5 g of antioxidant, cooling and discharging to obtain the modified rubber.
4. Adding 0.2g of expandable microsphere foaming agent into 12g of ethyl ester, uniformly dispersing, adding into 100g of modified rubber solution, stirring for 10min, adding 1g of black color paste into the mixture, stirring for 20min, finally adding 1g of isocyanate curing agent into the mixture, stirring for 10min, coating 80um dry glue on a 50um transparent PET release film by a scraper type coating machine, setting the temperature gradient of an oven to be 50 ℃, 60 ℃, 85 ℃, 110 ℃, 155 ℃ and 110 ℃, and setting the time of each temperature gradient to be 3min to obtain high-performance foam; and (3) coating acrylic pressure-sensitive adhesive with the thickness of 50 mu m on two sides to obtain the impact-resistant adhesive tape.
Comparative example 1
Compared with example 1, this comparative example adds the use of pentenediol instead of the hydroxy-terminated side chain vinyl-containing siloxane in the preparation of difunctional small molecules.
1. Placing 1mol of amylene diol and 1.1mol of hydrogen terminated siloxane in a container containing a magnetic stirrer and toluene solvent, and then introducing N2And (3) protecting, adding 0.01mmol of alkynol inhibitor, heating to 70 ℃, adding 0.1mmol of platinum catalyst, and reacting in a silicon oil bath for 3-4 hours to obtain alkane with a side chain containing a silicon-hydrogen active group, wherein the alkane is used as a first intermediate.
2. 2mol of isophorone diisocyanate and 0.01mmol of dibutyltin dilaurate catalyst are placed in a container containing a magnetic stirrer and toluene, and then N is introduced2And (3) protection, slowly dropwise adding 1mol of the first intermediate into a container at 70 ℃, determining the reaction process by detecting the content of O ═ C ═ N groups during the reaction, and when the content is less than one third of the addition amount, cooling and discharging, and storing in a dark place to obtain the bifunctional micromolecules.
3. 100g of SIS and 400g of toluene are introduced into a vessel equipped with a mechanical stirring deviceThen is turned on N2Protecting, heating to 40 ℃ inside the solution, and stirring for 1-2h until the rubber is dissolved; and heating to 75 ℃, adding 20g of bifunctional micromolecules into the container, stirring for 0.3h, adding 0.7mg of platinum catalyst, continuing to react for 4-5h, adding 10101.5 g of antioxidant, cooling and discharging to obtain the modified rubber.
4. Adding 0.2g of expandable microsphere foaming agent into 12g of ethyl ester, uniformly dispersing, adding into 100g of modified rubber solution, stirring for 10min, adding 1g of black color paste into the mixture, stirring for 20min, finally adding 1g of isocyanate curing agent into the mixture, stirring for 10min, coating 80um dry glue on a 50um transparent PET release film by a scraper type coating machine, setting the temperature gradient of an oven to be 50 ℃, 60 ℃, 85 ℃, 110 ℃, 155 ℃ and 110 ℃, and setting the time of each temperature gradient to be 3min to obtain high-performance foam; and (3) coating acrylic pressure-sensitive adhesive with the thickness of 50 mu m on two sides to obtain the impact-resistant adhesive tape.
Comparative example 2
In comparison with example 1, this comparative example did not prepare a modified rubber, and an impact-resistant adhesive tape was produced using SIS rubber as it is.
Adding 0.2g of expandable microsphere foaming agent into 12g of ethyl ester, uniformly dispersing, adding into 100g of SIS rubber solution, stirring for 10min, adding 1g of black color paste into the mixture, stirring for 20min, finally adding 1g of isocyanate curing agent into the mixture, stirring for 10min, coating 80um dry glue on a 50um transparent PET release film by a scraper type coating machine, setting the temperature gradient of an oven to be 50 ℃, 60 ℃, 85 ℃, 110 ℃, 155 ℃ and 110 ℃, and setting the time of each temperature gradient to be 3min to obtain high-performance foam; and (3) coating acrylic pressure-sensitive adhesive with the thickness of 50 mu m on two sides to obtain the impact-resistant adhesive tape.
The products prepared in examples 1-3 and comparative examples 1-2 were characterized:
testing the peeling force of the rubber: tested according to ASTM D3330 standard;
and (3) dynamic shear testing: attaching a double-sided adhesive tape between two SUSs, wherein the attaching area is 25mm multiplied by 25mm, a pulling machine selects a 'constant pressure 215N' mode to press in 215N, after the pressed sample is stood for 2 days in the environment of 23 +/-1 ℃ and 50 +/-5% RH, the pulling machine selects a 'shear strength' mode to test, and the maximum force value is recorded;
the DuPont impact test method comprises the following steps: die-cutting the double-sided adhesive into a 2mm wide square sample, respectively attaching a square SUS plate with the side length of 24.5mm and a square SUS frame with the side length of 20.5mm to two sides, pressing the two sides by a tensile machine in a mode of 'constant pressure 215N', standing the sample for 2 days at 23 +/-1 ℃ and 50 +/-5% RH after pressing, vertically impacting the sample at the height of 1m by adopting stainless steel balls with different weights, and recording the damaged ball number of the sample.
Pendulum bob impact test: attaching a double-sided adhesive tape between two SUS blocks with the side length of 24.5mm and 1mm, placing the SUS block with the side length of 1mm in the middle, attaching the SUS blocks with the area of 1mm multiplied by 1mm, pressing the SUS blocks with the side length of 1mm in a mode of 'constant pressure 215N' by a tensile machine in 35N, standing the pressed samples for 2 days in an environment with the temperature of 23 +/-1 ℃ and the RH of 50 +/-5%, testing by using a pendulum impact testing machine, and recording a test result;
tensile breaking test: cutting 3 sample strips of 15mm by 80mm in the transverse direction and the longitudinal direction, reserving 30mm at two ends of each sample strip for fixing the sample strips, wherein the length of each sample strip is 20mm, clamping the sample strips on a clamp, keeping the direction vertical, inputting the length, the width and the thickness of each sample strip in software, stretching at the speed of 200mm/min, and after the sample strips are broken, automatically stopping an instrument and outputting data of tensile strength and breaking elongation.
The test data are shown in the following table:
it can be seen from the comparison of examples 1-3 that with the increase of the addition amount of the bifunctional small molecule, the performance characteristics of the high-performance foam adhesive tape increase, which indicates that the bifunctional small molecule is indeed modified with rubber and crosslinked with the acrylic pressure-sensitive adhesive, thereby enhancing the performance of the adhesive tape.
By comparing example 1 with comparative example 1, it can be seen that the substitution of the hydroxyl-terminated side chain vinyl-containing siloxane with the pentenediol in comparative example 1 results in the reduction of the generated functional group with O ═ C ═ N, and the poor crosslinking degree with the acrylic pressure-sensitive adhesive, thus resulting in the reduction of the performance.
By comparing the example 1 with the comparative example 2, it can be seen that the foam adhesive tape prepared in the comparative example 2 does not use the modified rubber, the acrylic pressure sensitive adhesive has no chemical crosslinking with the rubber substrate, and the performance is poor.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A modified rubber characterized by: the modified rubber comprises the following components in parts by weight: 80-120 parts of rubber, 15-55 parts of bifunctional micromolecules, 0.0001-0.1 part of platinum catalyst, 300-450 parts of toluene and 1-3 parts of antioxidant;
the structural formula of the bifunctional small molecule is as follows:
2. the modified rubber according to claim 1, wherein: the rubber is any one of SBS rubber or SIS rubber; the antioxidant is antioxidant 1010.
3. A preparation method of modified rubber is characterized by comprising the following steps:
s1, preparing bifunctional small molecules
a. Adding hydroxyl-terminated siloxane with vinyl-containing side chain and hydrogen-terminated siloxane into a reaction vessel filled with toluene, magnetically stirring, and introducing N2Protecting, namely adding an alkynol inhibitor, heating to 70 ℃ in an oil bath, adding a platinum catalyst, and reacting for 3-4 hours to obtain siloxane with a side chain containing a silicon-hydrogen active group, wherein the siloxane is a first intermediate;
b. adding isophorone diisocyanate and dibutyltin dilaurate catalyst into a reaction vessel filled with toluene, magnetically stirring, and introducing N2Protecting, heating the oil bath to 70 ℃, slowly dropwise adding the first intermediate into the container, continuously detecting the content of O-C-N groups during the reaction, and cooling and discharging when the content is less than one third of the added amount to obtain the bifunctional micromolecules;
s2, adding rubber and toluene into the reaction vessel, and introducing N2Protecting, heating the oil bath to 35-45 ℃, stirring for 1-2h until the rubber is dissolved, heating the oil bath to 75 ℃, adding the bifunctional micromolecules into the reaction vessel, stirring for 0.3-0.5h, adding the platinum catalyst, continuously stirring for reaction for 4-5h, adding the antioxidant, uniformly mixing, stopping heating, cooling the rubber in the reaction vessel to 20-40 ℃, and discharging to obtain the modified rubber.
4. The modified rubber according to claim 3, wherein: in step S1, the molar ratio of the hydroxyl-terminated siloxane having a vinyl-containing side chain, the hydrogen-terminated siloxane, the alkynol inhibitor, the platinum catalyst, the isophorone diisocyanate, and the dibutyltin dilaurate catalyst is 1: 1.1: (0.00001-0.001): (0.00001-0.001): 2: (0.00001-0.001).
5. The high-performance foam prepared from the modified rubber according to any one of claims 1 to 4, wherein: the high-performance foam comprises the following components in parts by weight: 10-50 parts of ethyl ester, 0.15-3 parts of foaming agent, 95-175 parts of modified rubber, 0.5-3 parts of black color paste and 0.5-3 parts of curing agent.
6. A preparation method of high-performance foam prepared from modified rubber is characterized by comprising the following steps: adding ethyl ester and a foaming agent into a reaction kettle container, adding modified rubber after uniform dispersion, stirring for 10-15min, adding black color paste, continuing to stir for 15-25min, adding a curing agent, continuing to stir for 10-15min to obtain mixed glue, coating the mixed glue on a release film by using a scraper type coating machine, heating and drying the release film, and drying and peeling to obtain the high-performance foam.
7. The method for preparing the high-performance foam prepared from the modified rubber as claimed in claim 6, wherein the method comprises the following steps: wherein the foaming agent is an expandable microspheric foaming agent, and the curing agent is an isocyanate curing agent.
8. The method for preparing the high-performance foam prepared from the modified rubber as claimed in claim 6, wherein the method comprises the following steps: the heating and drying apparatus is an oven, the temperature gradient of the oven is set to 50 ℃, 60 ℃, 85 ℃, 110 ℃, 155 ℃ and 110 ℃, and the time of each temperature gradient is 3 min.
9. The method for preparing the high-performance foam prepared from the modified rubber as claimed in claim 6, wherein the method comprises the following steps: the thickness of the high-performance foam is 60-100 mu m, and the release film is a transparent PET release film with the thickness of 50 mu m.
10. A modified rubber high-performance foam adhesive tape is characterized in that: the modified rubber high-performance foam adhesive tape is composed of high-performance foam and acrylic pressure-sensitive adhesive coated on two sides of the high-performance foam.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111644259.6A CN114369184A (en) | 2021-12-30 | 2021-12-30 | Modified rubber and high-performance foam and adhesive tape prepared from same |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111644259.6A CN114369184A (en) | 2021-12-30 | 2021-12-30 | Modified rubber and high-performance foam and adhesive tape prepared from same |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115785452A (en) * | 2022-11-10 | 2023-03-14 | 杭州崇耀科技发展有限公司 | Anti-fog additive for coating release agent and preparation method thereof |
-
2021
- 2021-12-30 CN CN202111644259.6A patent/CN114369184A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 郭扬等: "《药用有机化学》", 中国医药科技出版社, pages: 351 - 352 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115785452A (en) * | 2022-11-10 | 2023-03-14 | 杭州崇耀科技发展有限公司 | Anti-fog additive for coating release agent and preparation method thereof |
| CN115785452B (en) * | 2022-11-10 | 2023-09-12 | 杭州崇耀科技发展有限公司 | Anti-fog additive for coating release agent and preparation method thereof |
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