High-temperature-resistant polyvinyl chloride adhesive tape and preparation process thereof

Abstract

The invention relates to the technical field of adhesive tapes, in particular to a high-temperature-resistant polyvinyl chloride adhesive tape and a preparation process thereof. The high-temperature-resistant polyvinyl chloride adhesive tape is composed of a flame-retardant polyvinyl chloride film and an adhesive layer, the flame-retardant polyvinyl chloride film comprises the following components: polyvinyl chloride resin, a flame-retardant plasticizer, a filler and a stabilizer, and the flame-retardant plasticizer has good plasticization and flame retardance and is beneficial to improving the processability, flexibility and flame retardance of polyvinyl chloride; the adhesive layer is formed by coating a flame-retardant polyvinyl chloride film with a modified acrylate pressure-sensitive adhesive, the modified acrylate pressure-sensitive adhesive is obtained by modifying an acrylate pressure-sensitive adhesive with a high-temperature-resistant composite filler, and the high-temperature-resistant composite filler has good heat resistance and mechanical properties; the heat resistance and the tensile strength of the acrylate pressure-sensitive adhesive are favorably improved, so that the high-temperature resistance and the peel strength of the high-temperature-resistant polyvinyl chloride adhesive tape are remarkably improved.

Description

Technical Field

[0001] The present invention relates to the technical field of adhesive tapes, and more particularly to a high temperature resistant polyvinyl chloride adhesive tape and a preparation process thereof. Background Art

[0002] PVC tape is a strip product made of PVC film as the main material and coated with pressure-sensitive adhesive on PVC film. It is suitable for wire and cable protection, such as wire joint winding, insulation damage repair, insulation protection of various motors and electronic parts such as transformers, motors, capacitors, and voltage stabilizers. It can also be used for bundling, fixing, overlapping, repairing, and sealing in industrial processes. Although PVC itself has certain flame retardant properties, in the preparation process of PVC tape, in order to ensure the processing performance and flexibility of the tape, a certain amount of plasticizer is usually added to the PVC. As the amount of plasticizer added increases, the chlorine content in the PVC tape also decreases, which in turn affects the flame retardant properties of the entire PVC tape, and thus the safety and reliability of the PVC tape during use cannot be guaranteed.

[0003] There are many types of pressure-sensitive adhesives commonly used in polyvinyl chloride tapes, such as acrylic pressure-sensitive adhesives, rubber-based pressure-sensitive adhesives, and polyurethane-based pressure-sensitive adhesives. Acrylic pressure-sensitive adhesives are polymer materials made by the polymerization of acrylic acid and its ester monomers. This type of pressure-sensitive adhesive can form effective adhesion with the surface of the adherend under slight pressure, and can quickly generate sufficient adhesion at room temperature without heating or using solvents. However, the tensile strength and high temperature resistance of ordinary acrylic pressure-sensitive adhesives are relatively low. In high temperature environments, the modulus and cohesive strength will drop sharply, becoming a nearly viscous body. When peeling, residual adhesive will appear on the surface of the adherend, which greatly limits its application in high temperature environments such as high temperature resistant shielding, electronic component taping fixation, and electronic component bonding. Summary of the invention

[0004] In view of the deficiencies in the prior art, the present invention provides a high temperature resistant polyvinyl chloride tape and a preparation process thereof.

[0005] A high temperature resistant polyvinyl chloride tape, the high temperature resistant polyvinyl chloride tape is composed of a flame retardant polyvinyl chloride film and an adhesive layer; The components of the flame retardant polyvinyl chloride film include: 86-110 parts by weight of polyvinyl chloride resin, 3-7 parts by weight of flame retardant plasticizer, 15-26 parts by weight of filler and 0.4-2 parts by weight of stabilizer; The raw materials of the flame retardant plasticizer include: 10 to 16 parts by weight of phosphorus oxychloride, 0.08 to 0.15 parts by weight of aluminum chloride and 75 to 100 parts by weight of epoxy fatty acid methyl ester; The adhesive layer is formed by coating a modified acrylic pressure-sensitive adhesive on a flame-retardant polyvinyl chloride film, wherein the modified acrylic pressure-sensitive adhesive comprises: 20 to 40 parts by weight of acrylic pressure-sensitive adhesive, 1 to 3 parts by weight of toluene diisocyanate and 0.1 to 0.5 parts by weight of a high-temperature resistant composite filler; The raw materials of the high temperature resistant composite filler include: a mixed solution, 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, wherein the mixed solution is obtained by mixing pretreated pine cone powder, pretreated nano silicon carbide and 50% ethanol solution in a mass ratio of (1-4): (2-9): (120-180), the amount of 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride is 1-10% of the mass of the mixed solution, and the amount of N-hydroxysuccinimide is 1-6% of the mass of the mixed solution; The pretreated pine cone powder is obtained by washing the pine cone powder with alcohol, washing with alkali and washing with acid; The pretreated nano-silicon carbide is obtained by subjecting the nano-silicon carbide to modification treatment using a modification solution.

[0006] Furthermore, the thickness of the flame retardant polyvinyl chloride film is 60 to 120 μm, and the thickness of the adhesive layer is 30 to 60 μm.

[0007] A process for preparing the high temperature resistant polyvinyl chloride tape according to claim 1, comprising the following steps: S1: Preparation of flame retardant plasticizer, heating and stirring phosphorus oxychloride, aluminum chloride and epoxy fatty acid methyl ester to react to obtain a mixed solution, and washing and rotary evaporating the mixed solution to obtain a flame retardant plasticizer; S2: Preparation of flame-retardant polyvinyl chloride film, mixing polyvinyl chloride resin, flame-retardant plasticizer, filler and stabilizer evenly and extruding into film to obtain flame-retardant polyvinyl chloride film; S3: Preparation of high temperature resistant composite filler, pine cone powder is washed with alcohol, alkali and acid to obtain pretreated pine cone powder, nano silicon carbide is pretreated with a modified solution to obtain pretreated nano silicon carbide, and the pretreated pine cone powder, pretreated nano silicon carbide, 50% ethanol solution by mass, 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide are heated and stirred to react to obtain a high temperature resistant composite filler; S4: Preparation and modification of acrylic pressure-sensitive adhesive, using n-butyl acrylate, methyl methacrylate, isooctyl acrylate, vinyl acetate, acrylic acid monomer, benzoyl peroxide and ethyl acetate as raw materials to prepare acrylic pressure-sensitive adhesive, and stirring and mixing acrylic pressure-sensitive adhesive, toluene diisocyanate and high-temperature resistant composite filler, and ultrasonically dispersing to obtain modified acrylic pressure-sensitive adhesive; S5: Preparation of high temperature resistant polyvinyl chloride tape, coating the modified acrylic pressure-sensitive adhesive on the flame retardant polyvinyl chloride film to form an adhesive layer, and drying to obtain the high temperature resistant polyvinyl chloride tape.

[0008] Furthermore, step S1 of preparing the flame retardant plasticizer specifically comprises the following steps: S1.1: 10-16 parts by weight of phosphorus oxychloride and 0.08-0.15 parts by weight of aluminum chloride are added to reactor A, and stirred for 3-8 minutes. Then, 75-100 parts by weight of epoxy fatty acid methyl ester are added to reactor A, and the mixture is heated to 56-64° C. and stirred for reaction for 2-4 hours to obtain a mixed solution; S1.2: After the mixed solution is washed with deionized water for 2 to 3 times, the mixed solution is dehydrated by a rotary evaporator at 60 to 75° C. to obtain a flame retardant plasticizer.

[0009] Furthermore, step S3 of preparing the high temperature resistant composite filler specifically comprises the following steps: S3.1: Wash, dry and crush the pine cones to obtain pine cone powder, immerse the pine cone powder in anhydrous ethanol for 15 to 30 minutes, filter and dry to obtain alcohol-washed pine cone powder, immerse the alcohol-washed pine cone powder in a sodium hydroxide solution with a mass fraction of 10 to 15% for 4 to 6 hours, filter, wash and dry to obtain alkali-washed pine cone powder; S3.2: immerse the pine cone powder after alkali washing in a 1-3% by mass glacial acetic acid aqueous solution and stir for 10-15 minutes, and obtain the pretreated pine cone powder after filtering, washing and drying; S3.3: drying the nano-silicon carbide in a blast drying oven at 100-120°C for 1-2 hours to remove surface moisture, drying and cooling the dried nano-silicon carbide, adding the dried nano-silicon carbide to the modified solution, stirring and reacting at 42-56°C for 1-3 hours, and then filtering, washing and drying to obtain pretreated nano-silicon carbide; S3.4: Mix the pretreated pine cone powder, pretreated nano-silicon carbide and 50% ethanol solution in a mass ratio of (1-4): (2-9): (120-180) to obtain a mixed solution. Then, add 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide to the mixed solution, and slowly stir the reaction at 60-80°C for 6-12h. Then, filter, wash and dry to obtain a high temperature resistant composite filler.

[0010] Furthermore, the modified solution is prepared by mixing 3-aminopropyltriethoxysilane and an ethanol solution with a volume fraction of 75% in a mass ratio of (1-5):100.

[0011] Furthermore, the mass ratio of the dried nano-silicon carbide to the modified solution is (1-5): (50-90).

[0012] Furthermore, step S4 of preparing and modifying the acrylic pressure-sensitive adhesive specifically comprises the following steps: S4.1: 10 to 24 parts by weight of n-butyl acrylate, 16 to 29 parts by weight of methyl methacrylate, 7 to 18 parts by weight of isooctyl acrylate, 1 to 3 parts by weight of vinyl acetate, 0.5 to 2 parts by weight of acrylic acid monomer, 0.1 to 0.5 parts by weight of benzoyl peroxide and 25 to 50 parts by weight of ethyl acetate are added to reactor B, and the mixture is continuously stirred and heated to 75 to 90° C. under a nitrogen atmosphere, and the mixture is kept warm for reaction for 3 to 5 hours. After the reaction is completed, the mixture is cooled and discharged to obtain an acrylic pressure-sensitive adhesive; S4.2: Take 20 to 40 parts by weight of acrylic pressure-sensitive adhesive, 1 to 3 parts by weight of toluene diisocyanate and 0.1 to 0.5 parts by weight of high-temperature resistant composite filler, stir and mix, and ultrasonically disperse for 20 to 60 minutes to obtain a modified acrylic pressure-sensitive adhesive.

[0013] Furthermore, the filler is at least one of calcium carbonate, white carbon black, glass fiber or talc.

[0014] Furthermore, the stabilizer is at least one of stearic acid, zinc stearate or calcium stearate.

[0015] Compared with the prior art, the present invention has at least the following advantages: 1. In the present invention, by reacting epoxy fatty acid methyl ester with phosphorus oxychloride, the chlorine atom in the phosphorus oxychloride molecule reacts with the oxygen atom in the epoxy group by a nucleophilic reaction, and the chlorine atom in the phosphorus oxychloride combines with the oxygen atom in the epoxy group, resulting in the ring opening of the epoxy group, and then the epoxy fatty acid methyl ester after the ring opening further undergoes a substitution reaction with the chloride ion in the phosphorus oxychloride. After phosphorus oxychloride is introduced into the epoxy fatty acid methyl ester, the obtained flame retardant plasticizer has good flame retardant properties, ensuring that the flame retardant plasticizer has a plasticizing effect on polyvinyl chloride while improving the flame retardant properties of polyvinyl chloride.

[0016] 2. In the present invention, pine cone powder and nano-silicon carbide are pretreated respectively, and then a dehydration condensation reaction is carried out with the pretreated pine cone powder and the pretreated nano-silicon carbide as raw materials. In the dehydration condensation reaction, the carboxyl groups on the surface of the pretreated pine cone powder are first activated by 1-ethyl-(3-dimethylaminopropyl)carbodiimide hydrochloride, and then the activated pretreated pine cone powder reacts with N-hydroxysuccinimide to generate an intermediate, and the intermediate can condense with the amino groups on the surface of the pretreated nano-silicon carbide to form an amide bond, thereby generating a high-temperature resistant composite filler. The pine cone powder and nano-silicon carbide cooperate with each other in the composite system of the high-temperature resistant composite filler, and have a significant synergistic effect in tensile strength and high temperature resistance, so that the generated high-temperature resistant composite filler has good heat resistance and mechanical properties.

[0017] 3. In the present invention, the acrylic pressure-sensitive adhesive is modified by using a high-temperature resistant composite filler, which is not only beneficial to improving the cross-linked network structure and cohesive strength of the acrylic pressure-sensitive adhesive, increasing the degree of mutual entanglement of the acrylic pressure-sensitive adhesive, promoting the interface interaction between the high-temperature resistant composite filler and acrylate, and improving the bonding effect of the acrylic pressure-sensitive adhesive on the bonded material, but also helps to improve the overall heat resistance of the acrylic pressure-sensitive adhesive, thereby significantly improving the high-temperature resistance, bonding effect and peel strength of the high-temperature resistant polyvinyl chloride tape. DETAILED DESCRIPTION

[0018] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be described clearly and completely below. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0019] Example 1 A preparation process of a high temperature resistant polyvinyl chloride tape comprises the following steps: S1: Preparation of flame retardant plasticizer, S1.1: 16 parts by weight of phosphorus oxychloride and 0.15 parts by weight of aluminum chloride were added to reactor A, stirred and mixed for 8 minutes, and then 100 parts by weight of epoxy fatty acid methyl ester were added to reactor A, heated to 64° C. and stirred for reaction for 3 hours to obtain a mixed solution; S1.2: After the mixed solution was washed with deionized water for three times, the mixed solution was dehydrated by a rotary evaporator at 65°C to obtain a flame retardant plasticizer; S2: Preparation of flame retardant polyvinyl chloride film, 110 parts by weight of polyvinyl chloride resin, 7 parts by weight of flame retardant plasticizer, 26 parts by weight of calcium carbonate and 1.4 parts by weight of calcium stearate were added to a mixer in sequence for mixing and mixing. The mixture was uniformly mixed and sent to an extruder for extrusion into a film to obtain a flame retardant polyvinyl chloride film with a thickness of 100 μm. S3: Preparation of high temperature resistant composite fillers, S3.1: Wash, dry and crush the pine cones to obtain pine cone powder, immerse the pine cone powder in anhydrous ethanol for 30 minutes, filter and dry to obtain alcohol-washed pine cone powder, immerse the alcohol-washed pine cone powder in a 10% sodium hydroxide solution for 6 hours, filter, wash and dry to obtain alkali-washed pine cone powder; S3.2: The pine cone powder after alkali washing is immersed in a 1% by mass acetic acid aqueous solution and stirred for 15 minutes, and then filtered, washed and dried to obtain pretreated pine cone powder; S3.3: Dry the nano-silicon carbide in a 100°C forced air drying oven for 2 hours to remove surface moisture, dry and cool the dried nano-silicon carbide, add the dried nano-silicon carbide to a modified solution, the modified solution is prepared by 3-aminopropyltriethoxysilane and 75% ethanol solution in a mass ratio of 5:100, the mass ratio of the dried nano-silicon carbide to the modified solution is 1:50, stir and react at 45°C for 3 hours, then filter, wash and dry to obtain pretreated nano-silicon carbide; S3.4: Pretreated pine cone powder, pretreated nano silicon carbide and 50% ethanol solution are mixed uniformly in a mass ratio of 1:4:120 to obtain a mixed solution. Subsequently, 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide are added to the mixed solution, wherein the amount of 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride added is 10% of the mass of the mixed solution, and the amount of N-hydroxysuccinimide added is 6% of the mass of the mixed solution. The mixture is slowly stirred and reacted at 75°C for 12 hours. Subsequently, the mixture is filtered, washed and dried to obtain a high temperature resistant composite filler. S4: Preparation and modification of acrylic pressure-sensitive adhesive, S4.1: 18 parts by weight of n-butyl acrylate, 24 parts by weight of methyl methacrylate, 13 parts by weight of isooctyl acrylate, 3 parts by weight of vinyl acetate, 1 part by weight of acrylic acid monomer, 0.5 parts by weight of benzoyl peroxide and 50 parts by weight of ethyl acetate are added to reactor B, and the mixture is heated to 80° C. under a nitrogen atmosphere with continuous stirring. The mixture is kept warm for reaction for 5 hours. After the reaction is completed, the mixture is cooled and discharged to obtain an acrylic pressure-sensitive adhesive; S4.2: Take 40 parts by weight of acrylic pressure-sensitive adhesive, 3 parts by weight of toluene diisocyanate and 0.5 parts by weight of high-temperature resistant composite filler, stir and mix, and ultrasonically disperse for 40 minutes to obtain a modified acrylic pressure-sensitive adhesive; S5: Preparation of high temperature resistant polyvinyl chloride tape, The modified acrylic pressure-sensitive adhesive was coated on the flame-retardant polyvinyl chloride film by using an applicator to form an adhesive layer with a thickness of 60 μm, and then dried at 100° C. for 1 h to obtain a high-temperature resistant polyvinyl chloride tape.

[0020] Example 2 A preparation process of a high temperature resistant polyvinyl chloride tape comprises the following steps: S1: Preparation of flame retardant plasticizer, S1.1: 16 parts by weight of phosphorus oxychloride and 0.15 parts by weight of aluminum chloride were added to reactor A, stirred and mixed for 8 minutes, and then 100 parts by weight of epoxy fatty acid methyl ester were added to reactor A, heated to 56° C. and stirred for reaction for 4 hours to obtain a mixed solution; S1.2: After the mixed solution was washed with deionized water for three times, the mixed solution was dehydrated by a rotary evaporator at 75°C to obtain a flame retardant plasticizer; S2: Preparation of flame retardant polyvinyl chloride film, 110 parts by weight of polyvinyl chloride resin, 7 parts by weight of flame retardant plasticizer, 26 parts by weight of calcium carbonate and 1.4 parts by weight of calcium stearate were added to a mixer in sequence for mixing and mixing. The mixture was uniformly mixed and sent to an extruder for extrusion into a film to obtain a flame retardant polyvinyl chloride film with a thickness of 100 μm. S3: Preparation of high temperature resistant composite fillers, S3.1: Wash, dry and crush the pine cones to obtain pine cone powder, immerse the pine cone powder in anhydrous ethanol for 30 minutes, filter and dry to obtain alcohol-washed pine cone powder, immerse the alcohol-washed pine cone powder in a 10% sodium hydroxide solution for 6 hours, filter, wash and dry to obtain alkali-washed pine cone powder; S3.2: The pine cone powder after alkali washing is immersed in a 1% by mass acetic acid aqueous solution and stirred for 15 minutes, and then filtered, washed and dried to obtain pretreated pine cone powder; S3.3: Dry the nano-silicon carbide in a 120°C forced air drying oven for 1 hour to remove surface moisture, dry and cool the dried nano-silicon carbide, add the dried nano-silicon carbide to a modified solution, the modified solution is prepared by 3-aminopropyltriethoxysilane and 75% ethanol solution in a mass ratio of 5:100, the mass ratio of the dried nano-silicon carbide to the modified solution is 1:50, stir and react at 56°C for 1 hour, then filter, wash and dry to obtain pretreated nano-silicon carbide; S3.4: Pretreated pine cone powder, pretreated nano silicon carbide and 50% ethanol solution are mixed uniformly in a mass ratio of 1:4:120 to obtain a mixed solution. Subsequently, 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide are added to the mixed solution, wherein the amount of 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride added is 10% of the mass of the mixed solution, and the amount of N-hydroxysuccinimide added is 6% of the mass of the mixed solution. The mixture is slowly stirred and reacted at 60°C for 12 hours. Subsequently, the mixture is filtered, washed and dried to obtain a high temperature resistant composite filler. S4: Preparation and modification of acrylic pressure-sensitive adhesive, S4.1: 18 parts by weight of n-butyl acrylate, 24 parts by weight of methyl methacrylate, 13 parts by weight of isooctyl acrylate, 3 parts by weight of vinyl acetate, 1 part by weight of acrylic acid monomer, 0.5 parts by weight of benzoyl peroxide and 50 parts by weight of ethyl acetate are added to reactor B, and the mixture is heated to 90° C. under a nitrogen atmosphere with continuous stirring for 3 hours. After the reaction is completed, the mixture is cooled and discharged to obtain an acrylic pressure-sensitive adhesive; S4.2: 40 parts by weight of acrylic pressure-sensitive adhesive, 3 parts by weight of toluene diisocyanate and 0.5 parts by weight of high-temperature resistant composite filler are mixed and ultrasonically dispersed for 60 minutes to obtain a modified acrylic pressure-sensitive adhesive; S5: Preparation of high temperature resistant polyvinyl chloride tape, The modified acrylic pressure-sensitive adhesive was coated on the flame-retardant polyvinyl chloride film by using an applicator to form an adhesive layer with a thickness of 60 μm, and then dried at 100° C. for 1 h to obtain a high-temperature resistant polyvinyl chloride tape.

[0021] Example 3 A preparation process of a high temperature resistant polyvinyl chloride tape comprises the following steps: S1: Preparation of flame retardant plasticizer, S1.1: 10 parts by weight of phosphorus oxychloride and 0.1 parts by weight of aluminum chloride were added to reactor A, stirred and mixed for 8 minutes, and then 75 parts by weight of epoxy fatty acid methyl ester were added to reactor A, heated to 64° C. and stirred for reaction for 3 hours to obtain a mixed solution; S1.2: After the mixed solution was washed with deionized water for three times, the mixed solution was dehydrated by a rotary evaporator at 65°C to obtain a flame retardant plasticizer; S2: Preparation of flame retardant polyvinyl chloride film, 110 parts by weight of polyvinyl chloride resin, 3 parts by weight of flame retardant plasticizer, 26 parts by weight of calcium carbonate and 0.8 parts by weight of calcium stearate were added to a mixer in sequence and mixed evenly, and then fed to an extruder and extruded into a film to obtain a flame retardant polyvinyl chloride film with a thickness of 100 μm; S3: Preparation of high temperature resistant composite fillers, S3.1: Wash, dry and crush the pine cones to obtain pine cone powder, immerse the pine cone powder in anhydrous ethanol for 30 minutes, filter and dry to obtain alcohol-washed pine cone powder, immerse the alcohol-washed pine cone powder in a 10% sodium hydroxide solution for 6 hours, filter, wash and dry to obtain alkali-washed pine cone powder; S3.2: The pine cone powder after alkali washing is immersed in a 1% by mass acetic acid aqueous solution and stirred for 15 minutes, and then filtered, washed and dried to obtain pretreated pine cone powder; S3.3: Dry the nano-silicon carbide in a 100°C forced air drying oven for 2 hours to remove surface moisture, dry and cool the dried nano-silicon carbide, add the dried nano-silicon carbide to a modified solution, the modified solution is prepared by 3-aminopropyltriethoxysilane and 75% ethanol solution in a mass ratio of 5:100, the mass ratio of the dried nano-silicon carbide to the modified solution is 3:80, stir and react at 45°C for 3 hours, then filter, wash and dry to obtain pretreated nano-silicon carbide; S3.4: Pretreated pine cone powder, pretreated nano silicon carbide and 50% ethanol solution are mixed uniformly in a mass ratio of 2:5:150 to obtain a mixed solution. Subsequently, 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide are added to the mixed solution, wherein the amount of 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride added is 8% of the mass of the mixed solution, and the amount of N-hydroxysuccinimide added is 5% of the mass of the mixed solution. The mixture is stirred slowly at 75°C for 12 hours, and then filtered, washed and dried to obtain a high temperature resistant composite filler. S4: Preparation and modification of acrylic pressure-sensitive adhesive, S4.1: 18 parts by weight of n-butyl acrylate, 24 parts by weight of methyl methacrylate, 13 parts by weight of isooctyl acrylate, 3 parts by weight of vinyl acetate, 1 part by weight of acrylic acid monomer, 0.5 parts by weight of benzoyl peroxide and 50 parts by weight of ethyl acetate are added to reactor B, and the mixture is heated to 80° C. under a nitrogen atmosphere with continuous stirring. The mixture is kept warm for reaction for 5 hours. After the reaction is completed, the mixture is cooled and discharged to obtain an acrylic pressure-sensitive adhesive; S4.2: 40 parts by weight of acrylic pressure-sensitive adhesive, 3 parts by weight of toluene diisocyanate and 0.2 parts by weight of high-temperature resistant composite filler are mixed and ultrasonically dispersed for 40 minutes to obtain a modified acrylic pressure-sensitive adhesive; S5: Preparation of high temperature resistant polyvinyl chloride tape, The modified acrylic pressure-sensitive adhesive was coated on the flame-retardant polyvinyl chloride film by using an applicator to form an adhesive layer with a thickness of 60 μm, and then dried at 100° C. for 1 h to obtain a high-temperature resistant polyvinyl chloride tape.

[0022] Comparative Example 1 Compared with Example 1, the difference of Comparative Example 1 is that step S1 is removed, the flame retardant plasticizer in step S2 is replaced by epoxy fatty acid methyl ester, and the other steps remain unchanged to prepare a flame retardant polyvinyl chloride film, which is recorded as Comparative Example 1.

[0023] According to GB / T 2406-2022 and GB / T 1040.1-2018 standards, the flame retardant polyvinyl chloride films in Examples 1-3 and Comparative Example 1 were respectively subjected to oxygen index tests and tensile strength tests, and the test results are shown in Table 1.

[0024] Table 1:

[0025] As shown in Table 1, the flame retardant polyvinyl chloride films in Examples 1-3 have oxygen indexes greater than 32%, and have better flame retardant properties than the flame retardant polyvinyl chloride film in Comparative Example 1, and the difference in tensile strength and elongation at break test results between Examples 1-3 and Comparative Example 1 is not significant. This indicates that the use and addition of flame retardant plasticizers will not affect the original plasticizing effect of epoxy fatty acid methyl ester on polyvinyl chloride, and can ensure that the flame retardant plasticizers plasticize polyvinyl chloride while improving the flame retardant properties of polyvinyl chloride, thereby improving the flame retardant properties of the flame retardant polyvinyl chloride film.

[0026] Comparative Example 2 Compared with Example 1, the difference of Comparative Example 2 is that step S3.4 is removed, the high temperature resistant composite filler in step S4.2 is replaced with nano silicon carbide, and the other steps remain unchanged to prepare a high temperature resistant polyvinyl chloride tape, which is recorded as Comparative Example 2.

[0027] Comparative Example 3 Compared with Example 1, the difference of Comparative Example 3 is that step S3.4 is removed, the high temperature resistant composite filler in step S4.2 is replaced with pretreated pine cone powder, and the other steps remain unchanged to prepare a high temperature resistant polyvinyl chloride tape, which is recorded as Comparative Example 3.

[0028] Comparative Example 4 Compared with Example 1, the difference of Comparative Example 4 is that step S3.4 is removed, and the high-temperature resistant composite filler in step S4.2 is replaced by a mixed powder, and the mixed powder is prepared by mixing pretreated pine cone powder and nano-silicon carbide in a mass ratio of 1:4. The other steps remain unchanged to prepare a high-temperature resistant polyvinyl chloride tape, which is recorded as Comparative Example 4.

[0029] Comparative Example 5 Compared with Example 1, the difference of Comparative Example 5 is that step S4.2 is removed, the modified acrylate pressure-sensitive adhesive in step S5 is replaced by acrylate pressure-sensitive adhesive, and the other steps remain unchanged to prepare a high-temperature resistant polyvinyl chloride tape, which is recorded as Comparative Example 5.

[0030] The high temperature resistant polyvinyl chloride tapes prepared in Examples 1-3 and Comparative Examples 2-5 were tested as follows. The test results are shown in Table 2: Mechanical properties: tensile strength test according to GB / T 1040.1-2018 standard; 180° peel strength: tested according to GB / T 2792-2014; Adhesion performance: tested according to GB / T 4851-2014; High temperature resistance: stick the high temperature resistant polyvinyl chloride tape on the mirror stainless steel plate, then place it in a constant temperature oven at 150°C. After 2 hours, take out the mirror stainless steel plate and hot peel off the high temperature resistant polyvinyl chloride tape on the mirror stainless steel plate. Check the damage of the adhesive layer and the residual glue on the mirror stainless steel plate. There are five levels: overall glue transfer, serious residual glue, a small amount of residual glue, shadow, and no residual glue.

[0031] Table 2:

[0032] As shown in Table 2, the tensile strength, 180° peel strength and holding force test results of the high temperature resistant polyvinyl chloride adhesive in Examples 1-3 are better than those of the high temperature resistant polyvinyl chloride adhesive in Comparative Examples 2-5, and after high temperature treatment and hot peeling, the high temperature resistant polyvinyl chloride adhesive in Examples 1-3 has no residual adhesive or dark shadow, and the high temperature resistance effect is also significantly better than that of the high temperature resistant polyvinyl chloride adhesive in Comparative Examples 2-5. It shows that compared with the use of adding pine cone powder, nano silicon carbide or a mixed powder of pine cone powder and nano silicon carbide, the use of high temperature resistant composite fillers to modify the acrylic pressure sensitive adhesive is more conducive to improving the tensile strength, high temperature resistance and adhesion effect of the high temperature resistant polyvinyl chloride adhesive.

[0033] It should be understood that those skilled in the art can make improvements or changes based on the above description, and all such improvements and changes should fall within the scope of protection of the appended claims of the present invention. Parts not described in detail in this specification belong to the prior art known to those skilled in the art.

Claims

1. A high temperature resistant polyvinyl chloride tape, characterized in that: High temperature resistant polyvinyl chloride tape is composed of flame retardant polyvinyl chloride film and adhesive layer; The components of the flame retardant polyvinyl chloride film include: 86-110 parts by weight of polyvinyl chloride resin, 3-7 parts by weight of flame retardant plasticizer, 15-26 parts by weight of filler and 0.4-2 parts by weight of stabilizer; The raw materials of the flame retardant plasticizer include: 10 to 16 parts by weight of phosphorus oxychloride, 0.08 to 0.15 parts by weight of aluminum chloride and 75 to 100 parts by weight of epoxy fatty acid methyl ester; The adhesive layer is formed by coating a modified acrylic pressure-sensitive adhesive on a flame-retardant polyvinyl chloride film, wherein the modified acrylic pressure-sensitive adhesive comprises: 20 to 40 parts by weight of acrylic pressure-sensitive adhesive, 1 to 3 parts by weight of toluene diisocyanate and 0.1 to 0.5 parts by weight of a high-temperature resistant composite filler; The raw materials of the high temperature resistant composite filler include: a mixed solution, 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide, wherein the mixed solution is obtained by mixing pretreated pine cone powder, pretreated nano silicon carbide and 50% ethanol solution in a mass ratio of (1-4): (2-9): (120-180), the amount of 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride is 1-10% of the mass of the mixed solution, and the amount of N-hydroxysuccinimide is 1-6% of the mass of the mixed solution; The pretreated pine cone powder is obtained by washing the pine cone powder with alcohol, washing with alkali and washing with acid; The pretreated nano-silicon carbide is obtained by subjecting the nano-silicon carbide to modification treatment using a modification solution.

2. A high temperature resistant polyvinyl chloride tape according to claim 1, characterized in that: The thickness of the flame retardant polyvinyl chloride film is 60 to 120 μm, and the thickness of the adhesive layer is 30 to 60 μm.

3. A process for preparing the high temperature resistant polyvinyl chloride tape according to claim 1, characterized in that: The steps include: S1: Preparation of flame retardant plasticizer, heating and stirring phosphorus oxychloride, aluminum chloride and epoxy fatty acid methyl ester to react to obtain a mixed solution, and washing and rotary evaporating the mixed solution to obtain a flame retardant plasticizer; S2: Preparation of flame-retardant polyvinyl chloride film, mixing polyvinyl chloride resin, flame-retardant plasticizer, filler and stabilizer evenly and extruding into film to obtain flame-retardant polyvinyl chloride film; S3: Preparation of high temperature resistant composite filler, pine cone powder is washed with alcohol, alkali and acid to obtain pretreated pine cone powder, nano silicon carbide is pretreated with modified solution to obtain pretreated nano silicon carbide, pretreated pine cone powder, pretreated nano silicon carbide, 50% ethanol solution by mass, 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide are heated and stirred to react to obtain high temperature resistant composite filler; S4: Preparation and modification of acrylic pressure-sensitive adhesive, using n-butyl acrylate, methyl methacrylate, isooctyl acrylate, vinyl acetate, acrylic acid monomer, benzoyl peroxide and ethyl acetate as raw materials to prepare acrylic pressure-sensitive adhesive, and stirring and mixing acrylic pressure-sensitive adhesive, toluene diisocyanate and high-temperature resistant composite filler, and ultrasonically dispersing to obtain modified acrylic pressure-sensitive adhesive; S5: Preparation of high temperature resistant polyvinyl chloride tape, coating the modified acrylic pressure-sensitive adhesive on the flame retardant polyvinyl chloride film to form an adhesive layer, and drying to obtain the high temperature resistant polyvinyl chloride tape.

4. The process for preparing a high temperature resistant polyvinyl chloride tape according to claim 3, characterized in that: Step S1: Preparation of flame retardant plasticizer, specifically comprising the following steps: S1.1: 10-16 parts by weight of phosphorus oxychloride and 0.08-0.15 parts by weight of aluminum chloride are added to reactor A, and stirred for 3-8 minutes. Then, 75-100 parts by weight of epoxy fatty acid methyl ester are added to reactor A, and the mixture is heated to 56-64° C. and stirred for reaction for 2-4 hours to obtain a mixed solution; S1.2: After the mixed solution is washed with deionized water for 2 to 3 times, the mixed solution is dehydrated by a rotary evaporator at 60 to 75° C. to obtain a flame retardant plasticizer.

5. The process for preparing a high temperature resistant polyvinyl chloride tape according to claim 3, characterized in that: Step S3: Preparation of high temperature resistant composite filler, specifically comprising the following steps: S3.1: Wash, dry and crush the pine cones to obtain pine cone powder, immerse the pine cone powder in anhydrous ethanol for 15 to 30 minutes, filter and dry to obtain alcohol-washed pine cone powder, immerse the alcohol-washed pine cone powder in a sodium hydroxide solution with a mass fraction of 10 to 15% for 4 to 6 hours, filter, wash and dry to obtain alkali-washed pine cone powder; S3.2: immerse the pine cone powder after alkali washing in a 1-3% by mass glacial acetic acid aqueous solution and stir for 10-15 minutes, and obtain the pretreated pine cone powder after filtering, washing and drying; S3.3: drying the nano-silicon carbide in a blast drying oven at 100-120°C for 1-2 hours to remove surface moisture, drying and cooling the dried nano-silicon carbide, adding the dried nano-silicon carbide to the modified solution, stirring and reacting at 42-56°C for 1-3 hours, and then filtering, washing and drying to obtain pretreated nano-silicon carbide; S3.4: Mix the pretreated pine cone powder, pretreated nano-silicon carbide and 50% ethanol solution in a mass ratio of (1-4): (2-9): (120-180) to obtain a mixed solution. Then, add 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride and N-hydroxysuccinimide to the mixed solution, and slowly stir the mixture at 60-80°C for 6-12h. Then, filter, wash and dry to obtain a high temperature resistant composite filler.

6. The process for preparing a high temperature resistant polyvinyl chloride tape according to claim 5, characterized in that: The modified solution is prepared by mixing 3-aminopropyltriethoxysilane and an ethanol solution with a volume fraction of 75% in a mass ratio of (1-5):

100.

7. The process for preparing a high temperature resistant polyvinyl chloride tape according to claim 5, characterized in that: The mass ratio of the dried nano-silicon carbide to the modified solution is (1-5): (50-90).

8. The process for preparing a high temperature resistant polyvinyl chloride tape according to claim 3, characterized in that: Step S4 preparation and modification of acrylic pressure-sensitive adhesive, specifically comprising the following steps: S4.1: 10 to 24 parts by weight of n-butyl acrylate, 16 to 29 parts by weight of methyl methacrylate, 7 to 18 parts by weight of isooctyl acrylate, 1 to 3 parts by weight of vinyl acetate, 0.5 to 2 parts by weight of acrylic acid monomer, 0.1 to 0.5 parts by weight of benzoyl peroxide and 25 to 50 parts by weight of ethyl acetate are added to reactor B, and the mixture is continuously stirred and heated to 75 to 90° C. under a nitrogen atmosphere, and the mixture is kept warm for reaction for 3 to 5 hours. After the reaction is completed, the mixture is cooled and discharged to obtain an acrylic pressure-sensitive adhesive; S4.2: Take 20 to 40 parts by weight of acrylic pressure-sensitive adhesive, 1 to 3 parts by weight of toluene diisocyanate and 0.1 to 0.5 parts by weight of high-temperature resistant composite filler, stir and mix, and ultrasonically disperse for 20 to 60 minutes to obtain a modified acrylic pressure-sensitive adhesive.

9. The process for preparing a high temperature resistant polyvinyl chloride tape according to claim 3, characterized in that: The filler is at least one of calcium carbonate, white carbon black, glass fiber or talcum powder.

10. The process for preparing a high temperature resistant polyvinyl chloride tape according to claim 3, characterized in that: The stabilizer is at least one of stearic acid, zinc stearate or calcium stearate.

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