CN116875267B - Flame-retardant rebound silicon rubber self-adhesive tape and preparation method thereof - Google Patents

Flame-retardant rebound silicon rubber self-adhesive tape and preparation method thereof Download PDF

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CN116875267B
CN116875267B CN202310972282.0A CN202310972282A CN116875267B CN 116875267 B CN116875267 B CN 116875267B CN 202310972282 A CN202310972282 A CN 202310972282A CN 116875267 B CN116875267 B CN 116875267B
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adhesive tape
silicone rubber
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neck flask
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CN116875267A (en
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芮章俊
李�荣
芮瑞
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Wuhu Hangfei Science and Technology Co Ltd
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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
    • 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
    • C08G77/22—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
    • C08G77/30—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen phosphorus-containing groups
    • 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
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic
    • 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
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • 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
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08—Macromolecular additives
    • 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
    • C09J7/10—Adhesives in the form of films or foils without carriers
    • 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
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C08K2003/2227—Oxides; Hydroxides of metals of aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/02—Flame or fire retardant/resistant
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00—Polymer mixtures characterised by other features
    • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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    • 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
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Abstract

The invention discloses a flame-retardant rebound silicon rubber self-adhesive tape and a preparation method thereof, and belongs to the technical field of self-adhesive tape processing. The invention is used for solving the technical problems that the self-adhesive property and rebound performance of the self-adhesive tape are reduced by adding the flame retardant into the silicone rubber in the prior art, and the preparation method of the silicone rubber self-adhesive tape needs further improvement, and the flame-retardant rebound silicone rubber self-adhesive tape comprises the following raw materials in parts by weight: 100-120 parts of methyl silicone rubber, 25-35 parts of modified silicone rubber, 13-17 parts of modified aluminum hydroxide, 12-14 parts of nano silicon oxide powder, 8-14 parts of hydroxyl silicone oil and 6-10 parts of cross-linking agent. The invention not only effectively improves the flame retardant property of the silicone rubber self-adhesive tape, but also optimizes the kneading process and improves the tensile property, rebound resilience and self-adhesive property of the self-adhesive tape.

Description

Flame-retardant rebound silicon rubber self-adhesive tape and preparation method thereof
Technical Field
The invention relates to the technical field of self-adhesive tape processing, in particular to a flame-retardant rebound silicon rubber self-adhesive tape and a preparation method thereof.
Background
Self-adhesive tape is a common adhesive product and is widely applied to the fields of industry, construction, electronics, medical treatment and the like. Conventional self-adhesive tapes typically use rubber or plastic as a substrate to which an adhesive is added to impart adhesion. However, some special application scenarios have higher performance requirements on self-adhesive tapes, such as fire disaster and other high temperature environments, and require flame retardant performance to prevent fire disaster from spreading; at the same time, for applications requiring frequent use, the rebound performance is also important to ensure stability and reliability for long-term use.
Silicone rubber is a special rubber material, also known as silicone rubber or silicone rubber material. The organic polymer is connected by a silicon-oxygen bond, and has excellent high temperature resistance, cold resistance, chemical corrosion resistance and electrical insulation property. Silicone rubber is widely used in many industrial fields due to its special chemical structure and properties.
The silicone rubber self-adhesive tapes in the prior art are non-flame-retardant, so that the application and popularization of the silicone rubber self-adhesive tapes in the electric power market are hindered. The main reason of slow research progress of flame-retardant silicone rubber self-adhesive tape is that the flame retardant has a great influence on tackifier, the self-adhesive tape is basically not sticky after the flame retardant is added into silicone rubber, and a certain contradiction often exists between the flame retardant property and the rebound resilience property of the silicone rubber, the rebound resilience property of the silicone rubber self-adhesive tape is reduced by the traditional flame retardant, the long-term use effect of the silicone rubber self-adhesive tape is influenced, and meanwhile, the preparation method of the silicone rubber self-adhesive tape also needs to be further improved so as to improve the quality of products.
In view of the technical drawbacks of this aspect, a solution is now proposed.
Disclosure of Invention
The invention aims to provide a flame-retardant rebound silicone rubber self-adhesive tape and a preparation method thereof, which are used for solving the technical problems that in the prior art, the silicone rubber self-adhesive tape is non-flame-retardant, the self-adhesive tape is basically not sticky after a flame retardant is added into the silicone rubber, the rebound resilience of the silicone rubber self-adhesive tape is reduced, the long-term use effect of the silicone rubber self-adhesive tape is affected, and the preparation method of the silicone rubber self-adhesive tape needs to be further improved.
The aim of the invention can be achieved by the following technical scheme:
the flame-retardant rebound silicone rubber self-adhesive tape comprises the following raw materials in parts by weight: 100-120 parts of methyl silicone rubber, 25-35 parts of modified silicone rubber, 13-17 parts of modified aluminum hydroxide, 12-14 parts of nano silicon oxide powder, 8-14 parts of hydroxyl silicone oil and 6-10 parts of cross-linking agent;
after 9, 10-dihydro-9-oxo-10-phenanthrene phosphate reacts with methyl vinyl diethoxy silane to generate an intermediate I, and the intermediate I, the methyl vinyl diethoxy silane and the triethoxy silane react in an acidic environment through polycondensation to generate the modified silicone rubber;
the modified aluminum hydroxide is prepared by carrying out surface modification on nano aluminum hydroxide by KH-570 and then carrying out surface modification on the nano aluminum hydroxide by KH-570.
Further, the cross-linking agent is one or more of diethyl sulfide and diisopropyl sulfide.
The preparation method of the flame-retardant rebound silicon rubber self-adhesive tape comprises the following steps:
s1, adding 9, 10-dihydro-9-oxo-10-phenanthrene phosphate, toluene and an initiator into a three-neck flask protected by nitrogen, stirring, raising the temperature of the three-neck flask to 80-90 ℃, dropwise adding 45wt% of methylvinyldiethoxysilane/toluene solution into the three-neck flask, and carrying out heat preservation reaction for 8-9h after the dropwise addition is completed, so as to obtain an intermediate I;
the synthesis reaction principle of the intermediate I is as follows:
s2, adding the intermediate I, methyl vinyl diethoxysilane, triethoxysilane and ethanol into a three-neck flask, uniformly mixing, adding hydrochloric acid into the three-neck flask, adjusting the pH value of the system to be 3-5, raising the temperature of the three-neck flask to 50-60 ℃, carrying out heat preservation reaction for 5-6 hours, and carrying out aftertreatment to obtain modified silicone rubber;
the synthetic reaction principle of the modified silicone rubber is as follows:
s3, adding the methyl silicone rubber, the nano silicon oxide powder and the hydroxyl silicone oil into a kneader, kneading for 20-30min, adding the modified silicone rubber and the modified aluminum hydroxide into the kneader, kneading for 10-15min, adding the cross-linking agent into the kneader, and kneading for 18-24min to obtain a kneaded material;
s4, transferring the kneaded material into an extruder while the kneaded material is hot, setting the temperature of the extruder to be 200-220 ℃, performing melt extrusion through the extruder, cooling and solidifying to form a strip-shaped extrusion adhesive tape, cutting the extrusion adhesive tape, and winding the cut extrusion adhesive tape onto a winding drum to obtain a self-adhesive tape finished product.
Further, in the step S1, the dosage ratio of the 9, 10-dihydro-9-oxo-10-phenanthrene phosphate, 45wt% of methyl vinyl diethoxysilane/toluene solution, toluene and an initiator is 7.2g to 11.8g to 25mL to 0.1g, wherein the initiator is azodiisobutyronitrile; the post-processing operation includes: after the reaction is completed, the temperature of the three-neck flask is kept at 80-90 ℃, toluene is distilled off under reduced pressure, and an intermediate I is obtained.
Further, in the step S2, the dosage ratio of the intermediate I, the methyl vinyl diethoxy silane, the triethoxy silane and the ethanol is 2.4g:4.2g:1g:42mL, the concentration of the hydrochloric acid is 1-2M, and the post-treatment operation comprises: after the reaction is completed, the temperature of the three-neck flask is increased to 65-75 ℃, the solvent is distilled off under reduced pressure, the solid is washed to be neutral by purified water, and then the solid is washed by absolute ethyl alcohol and is transferred to an oven with the temperature of 70-80 ℃ to be dried to constant weight, so that the modified silicon rubber is obtained.
Further, the preparation method of the modified aluminum hydroxide comprises the following steps: adding nano aluminum hydroxide, absolute ethyl alcohol and sodium hydroxide solution into a three-mouth flask, after ultrasonic dispersion for 30-50min, fixing the three-mouth flask on an iron stand with mechanical stirring, raising the temperature of the three-mouth flask to 55-65 ℃, dropwise adding a modified solution into the three-mouth flask, and after the dropwise addition, carrying out heat preservation reaction for 3-5h, and carrying out aftertreatment to obtain the modified aluminum hydroxide.
Further, the dosage ratio of the nano aluminum hydroxide to the absolute ethyl alcohol to the sodium hydroxide solution to the modified solution is 2g:7mL:1mL:3mL, the mass concentration of the sodium hydroxide solution is 10-16%, and the modified solution consists of KH-570 and the absolute ethyl alcohol according to the dosage ratio of 1g:2 mL; the post-processing operation includes: after the reaction is finished, suction filtration is carried out, filter cakes are dried after being washed to be neutral by purified water, the filter cakes are transferred into a drying oven with the temperature of 70-80 ℃ and dried to constant weight, and the modified aluminum hydroxide is obtained.
Further, in the step S4, the temperature of the kneader is 160-180 ℃, the rotating speed of the rollers is 30-40r/min, and the pressure between the rollers of the kneader is 40-50MPa.
The invention has the following beneficial effects:
1. in the preparation process, 9, 10-dihydro-9-oxo-10-phenanthrene phosphate and methyl vinyl diethoxy silane react in a toluene system through an initiator, 9, 10-dihydro-9-oxo-10-phenanthrene phosphate is grafted on the methyl vinyl diethoxy silane to obtain an intermediate I, and then the intermediate I, the methyl vinyl diethoxy silane and triethoxy silane undergo hydrolytic condensation reaction in an acidic ethanol water environment to prepare the modified silicone rubber with reticular crosslinking; the phosphorus-nitrogen structure of the 9, 10-dihydro-9-oxo-10-phenanthrene phosphate endows the surface with good affinity, and the crosslinking capability of the 9, 10-dihydro-9-oxo-10-phenanthrene phosphate improves the crosslinking degree of the modified silicone rubber and the methyl silicone rubber, so that the surface of the modified silicone rubber and the surface of other materials are more easily mutually adsorbed and the chemical bond forming capability is enhanced, and the adhesive property and the mechanical strength of the self-adhesive tape are improved; the 9, 10-dihydro-9-oxo-10-phenanthrene phosphate has good high temperature resistance, and the high temperature resistance of the self-adhesive tape is effectively improved due to the branch connection and the doping of the 9, 10-dihydro-9-oxo-10-phenanthrene phosphate, and the 9, 10-dihydro-9-oxo-10-phenanthrene phosphate can release gas with higher phosphorus content such as phosphoric acid oxide when being decomposed at high temperature, so that substances such as phosphoric acid and phosphate generated by decomposition can promote the carbonization reaction of silicon rubber, and a flame-retardant carbonization layer is formed. The charring layer can isolate oxygen and fuel and prevent further propagation of flame, thereby reducing heat energy transmission of flame and effectively inhibiting propagation of flame.
2. In the preparation process, methyl silicone rubber, nano silicon oxide powder and hydroxyl silicone oil are kneaded by a kneader, the hydroxyl silicone oil is taken as a dispersing agent, the nano silicon oxide powder and the methyl silicone rubber are fully and uniformly mixed and then are mixed with modified silicone rubber and modified aluminum hydroxide, and then a cross-linking agent is added for meshing, so that a uniformly mixed kneading material is prepared; the kneading time for fully and uniformly mixing the components is effectively shortened through the addition sequence of the components of the kneading materials and the kneading parameters of the kneader; the nano aluminum hydroxide surface is modified by KH-570, and the modified aluminum hydroxide surface is coated with KH-570, so that the dispersity of the modified aluminum hydroxide in a kneading material is effectively improved, the pores of the silicon rubber are filled by the addition of aluminum hydroxide and silicon oxide nano powder, the structure of the material is more compact, the mobility of polymer chains in the kneading material is reduced, the self-adhesive tape becomes more resistant to deformation, better mechanical strength and toughness are shown, the self-adhesive tape is promoted to have higher rebound resilience, and the heat resistance and mechanical property of the silicon rubber can be improved by the addition of 9, 10-dihydro-9-oxo-10-phenanthrene phosphate, so that the rebound resilience of the self-adhesive tape is further improved; the aluminum hydroxide can generate thermal decomposition reaction in a high-temperature environment, releases water vapor and absorbs heat, the temperature of the material is reduced, the silicon oxide nano powder can form a protective silicon oxide layer at high temperature and covers the surface of silicon rubber, and the nano aluminum hydroxide is matched with the nano silicon oxide and the 9, 10-dihydro-9-oxo-10-phenanthrene phosphate, so that a strong thermal barrier and a carbonization layer are formed on the self-adhesive tape during combustion, the propagation of flame is inhibited, the entry of oxygen is prevented, and the flame retardant property of the self-adhesive tape is improved.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in connection with the embodiments, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The preparation method of the flame-retardant rebound silicon rubber self-adhesive tape comprises the following steps:
s1, preparing modified silicon rubber
Weighing: adding 72g of 9, 10-dihydro-9-oxo-10-phenanthrene phosphate, 250mL of toluene and 1g of azodiisobutyronitrile into a three-neck flask protected by nitrogen, stirring, raising the temperature of the three-neck flask to 80 ℃, dropwise adding 118mL of 45wt% methyl vinyl diethoxysilane/toluene solution into the three-neck flask, carrying out heat preservation reaction for 8 hours after the dropwise addition is completed, keeping the temperature of the three-neck flask at 80 ℃, and carrying out reduced pressure distillation to remove toluene to obtain an intermediate I;
weighing: 48g of intermediate I, 84g of methyl vinyl diethoxysilane, 20g of triethoxysilane and 840mL of ethanol are added into a three-neck flask, 1M hydrochloric acid is added into the three-neck flask, the pH=3 of the system is regulated, the temperature of the three-neck flask is increased to 50 ℃, the temperature of the three-neck flask is kept for 5 hours, the temperature of the three-neck flask is increased to 65 ℃, the solvent is distilled off under reduced pressure, the solid is washed to be neutral by purified water, and then is washed by absolute ethyl alcohol, and is transferred into an oven with the temperature of 70 ℃ to be dried to constant weight, so that the modified silicon rubber is obtained.
S2, preparing modified aluminum hydroxide
Adding KH-570 and absolute ethyl alcohol into a beaker according to the dosage ratio of 1g to 2mL, and uniformly mixing to obtain a modified liquid;
weighing: adding 20g of nano aluminum hydroxide, 70mL of absolute ethyl alcohol and 10mL of 10-16wt% sodium hydroxide solution into a three-neck flask, after ultrasonic dispersion for 30min, fixing the three-neck flask on an iron stand with mechanical stirring, raising the temperature of the three-neck flask to 55 ℃, dropwise adding 30mL of modified solution into the three-neck flask, carrying out heat preservation reaction for 3h after dropwise adding, carrying out suction filtration, washing a filter cake with purified water to be neutral, then pumping, transferring the filter cake into a drying box with the temperature of 70 ℃, and drying to constant weight to obtain the modified aluminum hydroxide.
S3, preparing a kneading material
Setting the temperature of a kneader to 160 ℃, the rotating speed of the rollers to 30r/min, and the pressure between the rollers of the kneader to 40MPa;
weighing: 1000g of methyl silicone rubber, 120g of nano silicon oxide powder and 80g of hydroxyl silicone oil are added into a kneader, kneading is carried out for 20min, 250g of modified silicone rubber and 130g of modified aluminum hydroxide are added into the kneader, kneading is carried out for 10min, 60g of diethyl sulfide is added into the kneader, and kneading is carried out for 18min, thus obtaining the kneaded material.
S4, preparing self-adhesive tape
Transferring the kneaded material into an extruder while the kneaded material is hot, setting the temperature of the extruder to be 200 ℃, carrying out melt extrusion by the extruder, cooling and solidifying by cold air at 5 ℃ to form a strip-shaped extrusion adhesive tape, cutting the extrusion adhesive tape, and winding the cut extrusion adhesive tape onto a winding drum to obtain a self-adhesive tape finished product.
Example 2
The preparation method of the flame-retardant rebound silicon rubber self-adhesive tape comprises the following steps:
s1, preparing modified silicon rubber
Weighing: adding 72g of 9, 10-dihydro-9-oxo-10-phenanthrene phosphate, 250mL of toluene and 1g of azodiisobutyronitrile into a three-neck flask protected by nitrogen, stirring, raising the temperature of the three-neck flask to 85 ℃, dropwise adding 118mL of 45wt% methyl vinyl diethoxysilane/toluene solution into the three-neck flask, carrying out heat preservation reaction for 8.5h after the dropwise addition is finished, keeping the temperature of the three-neck flask at 85 ℃, and carrying out reduced pressure distillation to remove toluene to obtain an intermediate I;
weighing: 48g of intermediate I, 84g of methyl vinyl diethoxysilane, 20g of triethoxysilane and 840mL of ethanol are added into a three-neck flask, 1-2M hydrochloric acid is added into the three-neck flask, the pH=4 of the system is regulated, the temperature of the three-neck flask is increased to 55 ℃, the temperature of the three-neck flask is kept for 5.5 hours, the temperature of the three-neck flask is increased to 70 ℃, the solvent is distilled off under reduced pressure, the solid is washed to be neutral by purified water, and the solid is washed by absolute ethyl alcohol and then is transferred into an oven with the temperature of 75 ℃ to be dried to constant weight, so that the modified silicone rubber is obtained.
S2, preparing modified aluminum hydroxide
Adding KH-570 and absolute ethyl alcohol into a beaker according to the dosage ratio of 1g to 2mL, and uniformly mixing to obtain a modified liquid;
weighing: adding 20g of nano aluminum hydroxide, 70mL of absolute ethyl alcohol and 10mL of 10-16wt% sodium hydroxide solution into a three-neck flask, after ultrasonic dispersion for 40min, fixing the three-neck flask on an iron stand with mechanical stirring, raising the temperature of the three-neck flask to 60 ℃, dropwise adding 30mL of modified solution into the three-neck flask, carrying out heat preservation reaction for 4h after dropwise adding, carrying out suction filtration, washing a filter cake with purified water to be neutral, then pumping, transferring the filter cake into a drying box with the temperature of 75 ℃, and drying to constant weight, thus obtaining the modified aluminum hydroxide.
S3, preparing a kneading material
Setting the temperature of a kneader to 170 ℃, the rotating speed of the rollers to 35r/min, and the pressure between the rollers of the kneader to 45MPa;
weighing: 1100g of methyl silicone rubber, 130g of nano silicon oxide powder and 120g of hydroxyl silicone oil are added into a kneader, kneading is carried out for 25min, 300g of modified silicone rubber and 150g of modified aluminum hydroxide are added into the kneader, kneading is carried out for 13min, 80g of diisopropyl sulfide is added into the kneader, and kneading is carried out for 21min, thus obtaining the kneaded material.
S4, preparing self-adhesive tape
Transferring the kneaded material into an extruder while the kneaded material is hot, setting the temperature of the extruder to be 210 ℃, carrying out melt extrusion by the extruder, cooling and solidifying by 7 ℃ cold air to form a strip-shaped extrusion adhesive tape, cutting the extrusion adhesive tape, and winding the cut extrusion adhesive tape onto a winding drum to obtain a self-adhesive tape finished product.
Example 3
The preparation method of the flame-retardant rebound silicon rubber self-adhesive tape comprises the following steps:
s1, preparing modified silicon rubber
Weighing: adding 72g of 9, 10-dihydro-9-oxo-10-phenanthrene phosphate, 250mL of toluene and 1g of azodiisobutyronitrile into a three-neck flask protected by nitrogen, stirring, raising the temperature of the three-neck flask to 90 ℃, dropwise adding 118mL of 45wt% methyl vinyl diethoxysilane/toluene solution into the three-neck flask, carrying out heat preservation reaction for 9h after the dropwise addition is finished, keeping the temperature of the three-neck flask at 90 ℃, and carrying out reduced pressure distillation to remove toluene to obtain an intermediate I;
weighing: 48g of intermediate I, 84g of methyl vinyl diethoxysilane, 20g of triethoxysilane and 840mL of ethanol are added into a three-neck flask, 2M hydrochloric acid is added into the three-neck flask, the pH=5 of the system is regulated, the temperature of the three-neck flask is increased to 60 ℃, the temperature is kept for 6 hours, the temperature of the three-neck flask is increased to 75 ℃, the solvent is distilled off under reduced pressure, then the solid is washed to be neutral by purified water, and then is washed by absolute ethyl alcohol, and then is transferred into an oven with the temperature of 80 ℃ to be dried to constant weight, thus obtaining the modified silicon rubber.
S2, preparing modified aluminum hydroxide
Adding KH-570 and absolute ethyl alcohol into a beaker according to the dosage ratio of 1g to 2mL, and uniformly mixing to obtain a modified liquid;
weighing: adding 20g of nano aluminum hydroxide, 70mL of absolute ethyl alcohol and 10mL of 10-16wt% sodium hydroxide solution into a three-neck flask, after ultrasonic dispersion for 50min, fixing the three-neck flask on an iron stand table with mechanical stirring, raising the temperature of the three-neck flask to 65 ℃, dropwise adding 30mL of modified solution into the three-neck flask, carrying out heat preservation reaction for 5h after dropwise adding, carrying out suction filtration, washing a filter cake with purified water to be neutral, then pumping, transferring the filter cake into a drying box with the temperature of 80 ℃, and drying to constant weight, thus obtaining the modified aluminum hydroxide.
S3, preparing a kneading material
Setting the temperature of a kneader at 180 ℃, the rotating speed of the rollers at 40r/min, and the pressure between the rollers of the kneader at 50MPa;
weighing: 1200g of methyl silicone rubber, 140g of nano silicon oxide powder and 140g of hydroxyl silicone oil are added into a kneader, kneading is carried out for 30min, 350g of modified silicone rubber and 170g of modified aluminum hydroxide are added into the kneader, kneading is carried out for 15min, 50g of diethyl sulfide and 50g of diisopropyl sulfide are added into the kneader, and kneading is carried out for 24min, thus obtaining the kneaded material.
S4, preparing self-adhesive tape
Transferring the kneaded material into an extruder while the kneaded material is hot, setting the temperature of the extruder to 220 ℃, carrying out melt extrusion by the extruder, cooling and solidifying by 8 ℃ cold air to form a strip-shaped extrusion adhesive tape, cutting the extrusion adhesive tape, and winding the cut extrusion adhesive tape onto a winding drum to obtain a self-adhesive tape finished product.
Comparative example 1
The present comparative example differs from example 1 in that the modified silicone rubber of step S1 was omitted without the addition of intermediate I.
Comparative example 2
The present comparative example differs from example 1 in that step S2 is eliminated and the modified aluminum hydroxide in step S3 is replaced by nano aluminum hydroxide in equal amount.
Comparative example 3
The comparative example differs from example 1 in that the preparation method of the kneadate in step S3 is: weighing: 1000g of methyl silicone rubber, 120g of nano silicon oxide powder, 80g of hydroxyl silicone oil, 250g of modified silicone rubber, 130g of modified aluminum hydroxide and 60g of diethyl sulfide are added into a kneader and kneaded for 48min to obtain a kneaded material
Performance test:
the finished self-adhesive tapes prepared in examples 1 to 3 and comparative examples 1 to 3 were tested for their combustion performance, self-adhesive performance, tensile strength, elongation at break and rebound resilience, wherein the tensile strength and elongation at break of the test specimens were determined with reference to the standard GB/T30776-2014 test method for tensile strength and elongation at break of adhesive tapes; the rebound resilience is measured according to the standard GB/T1681-2009 "determination of rebound resilience of vulcanized rubber"; self-adhesion performance the self-adhesion force of the sample is measured according to the standard GB/T4851-2014 test method for adhesive tape holding viscosity; the combustion performance of the test sample is measured according to the combustion performance reference standard GB/T10707-2008 'determination of rubber combustion performance', and the flame retardant grade of the test sample is judged according to the standard UL94, and the specific test results are shown in the following table:
data analysis:
in the preparation process of the self-adhesive tape, the methyl silicone rubber is doped and mixed after the modified silicone rubber and the aluminum hydroxide are synthesized, and the mixing process of the kneading materials is optimized, so that the tensile strength of the self-adhesive tape reaches 5.2MPa, the stretch-break elongation reaches 362.3%, the rebound resilience reaches 61.7%, the self-adhesive force reaches 9.2N/cm, the flame retardant grade reaches V-0, and all detection data are superior to those of comparative examples 1-3, thereby indicating that the self-adhesive tape prepared by the invention has good tensile property, rebound resilience, self-adhesive force and flame retardant property.
The foregoing is merely illustrative and explanatory of the invention, as it is well within the scope of the invention as claimed, as it relates to various modifications, additions and substitutions for those skilled in the art, without departing from the inventive concept and without departing from the scope of the invention as defined in the accompanying claims.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.

Claims (7)

1. The flame-retardant rebound silicone rubber self-adhesive tape is characterized by comprising the following raw materials in parts by weight: 100-120 parts of methyl silicone rubber, 25-35 parts of modified silicone rubber, 13-17 parts of modified aluminum hydroxide, 12-14 parts of nano silicon oxide powder, 8-14 parts of hydroxyl silicone oil and 6-10 parts of cross-linking agent;
the self-adhesive tape is processed by the following steps:
s1, adding 9, 10-dihydro-9-oxo-10-phenanthrene phosphate, toluene and an initiator into a three-neck flask protected by nitrogen, stirring, raising the temperature of the three-neck flask to 80-90 ℃, dropwise adding 45wt% of methylvinyldiethoxysilane/toluene solution into the three-neck flask, and carrying out heat preservation reaction for 8-9h after the dropwise addition is completed, so as to obtain an intermediate I;
s2, adding the intermediate I, methyl vinyl diethoxysilane, triethoxysilane and ethanol into a three-neck flask, uniformly mixing, adding hydrochloric acid into the three-neck flask, adjusting the pH value of the system to be 3-5, raising the temperature of the three-neck flask to 50-60 ℃, carrying out heat preservation reaction for 5-6 hours, and carrying out aftertreatment to obtain modified silicone rubber;
s3, adding the methyl silicone rubber, the nano silicon oxide powder and the hydroxyl silicone oil into a kneader, kneading for 20-30min, adding the modified silicone rubber and the modified aluminum hydroxide into the kneader, kneading for 10-15min, adding the cross-linking agent into the kneader, and kneading for 18-24min to obtain a kneaded material;
s4, transferring the kneaded material into an extruder while the kneaded material is hot, setting the temperature of the extruder to be 200-220 ℃, performing melt extrusion through the extruder, cooling and solidifying to form a strip-shaped extrusion adhesive tape, cutting the extrusion adhesive tape, and winding the cut extrusion adhesive tape onto a winding drum to obtain a self-adhesive tape finished product;
the preparation method of the modified aluminum hydroxide comprises the following steps: adding nano aluminum hydroxide, absolute ethyl alcohol and sodium hydroxide solution into a three-neck flask, performing ultrasonic dispersion for 30-50min, fixing the three-neck flask on an iron stand with mechanical stirring, raising the temperature of the three-neck flask to 55-65 ℃, dropwise adding a modified solution into the three-neck flask, and performing heat preservation reaction for 3-5h after the dropwise addition is completed, so as to obtain modified aluminum hydroxide, wherein the modified solution consists of KH-570 and absolute ethyl alcohol according to the dosage ratio of 1g to 2 mL.
2. The flame retardant resilient silicone rubber self adhesive tape of claim 1, wherein the cross-linking agent is one or more of diethyl sulfide, diisopropyl sulfide.
3. The flame retardant resilient silicone rubber self adhesive tape of claim 1, wherein in step S1 the 9, 10-dihydro-9-oxo-10-phenanthrene phosphate, 45wt% methylvinyldiethoxysilane/toluene solution, toluene and initiator are used in a ratio of 7.2g:11.8g:25ml:0.1g, said initiator being azobisisobutyronitrile.
4. The flame retardant resilient silicone rubber self adhesive tape of claim 1, wherein the amount ratio of intermediate I, methylvinyldiethoxysilane, triethoxysilane to ethanol in step S2 is 2.4g:4.2g:1g:42ml, and the concentration of hydrochloric acid is 1-2M.
5. The flame-retardant rebound silicone rubber self-adhesive tape of claim 1, wherein the dosage ratio of the nano aluminum hydroxide, the absolute ethyl alcohol, the sodium hydroxide solution and the modifying solution is 2g to 7ml to 1ml to 3ml, and the mass concentration of the sodium hydroxide solution is 10-16%.
6. The flame-retardant resilient silicone rubber self-adhesive tape according to claim 1, wherein in step S3, the kneader temperature is 160-180 ℃, the drum rotation speed is 30-40r/min, and the pressure between the kneader drums is 40-50MPa.
7. A method of preparing a flame retardant resilient silicone rubber self adhesive tape according to any one of claims 1 to 6, comprising the steps of:
adding methyl silicone rubber, nano silicon oxide powder and hydroxyl silicone oil into a kneader, kneading for 20-30min, adding modified silicone rubber and modified aluminum hydroxide into the kneader, kneading for 10-15min, adding a cross-linking agent into the kneader, and kneading for 18-24min to obtain a kneaded material;
transferring the kneaded material into an extruder while the kneaded material is hot, setting the temperature of the extruder to be 200-220 ℃, performing melt extrusion through the extruder, cooling and solidifying to form a strip-shaped extrusion adhesive tape, cutting the extrusion adhesive tape, and winding the cut extrusion adhesive tape onto a winding drum to obtain a self-adhesive tape finished product.
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CN113980609A (en) * 2021-12-13 2022-01-28 成都硅宝科技股份有限公司 High-self-adhesion silicon rubber self-adhesive tape and preparation method thereof
CN116376474A (en) * 2023-04-21 2023-07-04 奎达高分子材料科技(宜兴)有限公司 Anti-aging photovoltaic adhesive film based on PVB material and preparation process thereof

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