CN113583621A - High-temperature aging resistant glue for magic tape and manufacturing method thereof - Google Patents

High-temperature aging resistant glue for magic tape and manufacturing method thereof Download PDF

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Publication number
CN113583621A
CN113583621A CN202111072749.3A CN202111072749A CN113583621A CN 113583621 A CN113583621 A CN 113583621A CN 202111072749 A CN202111072749 A CN 202111072749A CN 113583621 A CN113583621 A CN 113583621A
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zinc oxide
stirring
double
shell hollow
parts
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CN202111072749.3A
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余建柱
余建荣
陈志坚
姜明华
余小郎
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Zhejiang Heyi Weaving Co ltd
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Zhejiang Heyi Weaving 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
    • C09J181/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur, with or without nitrogen, oxygen, or carbon only; Adhesives based on polysulfones; Adhesives based on derivatives of such polymers
    • C09J181/06—Polysulfones; Polyethersulfones
    • 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
    • C09J11/08—Macromolecular additives
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00—Properties
    • C08L2201/08—Stabilised against heat, light or radiation or oxydation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention provides a high-temperature aging resistant glue for magic tapes and a manufacturing method thereof, which comprises the steps of firstly carrying out modification treatment on double-shell hollow nano-zinc oxide by N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxysilane to obtain modified double-shell hollow nano-zinc oxide; then, adipic acid, 1, 4-cyclohexanediamine, modified double-shell hollow nano-zinc oxide and polyamino nano-silicon dioxide are used as raw materials, and a modified low-molecular polyamide is obtained through a polymerization reaction; and finally, mixing and melting the polyether sulfone resin, the modified low-molecular-weight polyamide, the rosin resin and the hydrogenated DCPD resin, cooling, adding dibutyl phthalate, and heating and stirring uniformly to obtain the modified low-molecular-weight polyamide resin. The glue for the magic tape has excellent high-temperature aging resistance and ultraviolet aging resistance, and has wide market prospect.

Description

High-temperature aging resistant glue for magic tape and manufacturing method thereof
Technical Field
The invention relates to the technical field of new materials, in particular to high-temperature-aging-resistant glue for a magic tape and a manufacturing method thereof.
Background
The magic tape is a common connecting auxiliary material, one surface of the magic tape is fine and soft fiber, and the other surface of the magic tape is hard barbed hair with hooks, and the magic tape is widely applied to the fields of clothes, shoes, sofas, automobile cushions, curtains, tents, various military products and the like.
On the basis of the common magic tape, hot melt adhesive can be applied to the back of the magic tape, and then a layer of oily release paper is attached to obtain the adhesive-backed magic tape. The hot melt adhesive is a solid soluble polymer which does not need a solvent and does not contain moisture, is solid at normal temperature, is heated and melted to a certain temperature to become liquid which can flow and has certain viscosity, and can be conveniently used for manufacturing the back adhesive magic tape.
Because many gum magic subsides service environment are abominable, expose under high temperature, ultraviolet condition for a long time, use can seriously influence the performance of gum magic subsides for a long time, lead to adhesive property to descend or even not stick completely to influence and use and experience and cause great incident even.
Patent CN110643311A discloses a special adhesive for magic tape with high temperature aging resistance, which is prepared by mixing composite elastomer, tackifying resin, softening agent, antioxidant, ultraviolet absorbent, pigment and the like. The high-temperature aging resistance of the special adhesive for the magic tape obtained by the patent technology is still not good enough, and the application requirements of special environmental conditions such as high temperature, outdoor and the like are difficult to meet.
Disclosure of Invention
The invention aims to provide a high-temperature aging resistant glue for a magic tape and a manufacturing method thereof, and the glue has an excellent high-temperature aging resistant effect.
In order to achieve the purpose, the invention is realized by the following scheme:
a method for manufacturing high-temperature aging resistant glue for magic tapes comprises the following specific steps:
(1) modifying double-shell hollow nano zinc oxide by N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane to obtain modified double-shell hollow nano zinc oxide;
(2) carrying out polymerization reaction on adipic acid, 1, 4-cyclohexanediamine, the modified double-shell hollow nano-zinc oxide prepared in the step (1) and polyamino nano-silicon dioxide serving as raw materials to prepare modified low-molecular-weight polyamide;
(3) and (3) mixing and melting polyether sulfone resin, the modified low-molecular-weight polyamide prepared in the step (2), rosin resin and hydrogenated DCPD resin, cooling, adding dibutyl phthalate, and heating and stirring uniformly to obtain the glue for the magic tape.
Preferably, the specific method of step (1) is as follows, in parts by weight: adding 1 part of double-shell hollow nano-zinc oxide into 5-7 parts of N- (beta-aminoethyl) -gamma-aminopropylmethyldimethoxysilane, stirring and reacting for 7-9 hours at 85-95 ℃, and centrifuging to obtain a precipitate, thus obtaining the modified double-shell hollow nano-zinc oxide.
Preferably, in the step (1), the preparation method of the double-shell hollow nano zinc oxide comprises the following steps: firstly, adding 0.5-0.6 part of zinc nitrate hexahydrate, 0.4-0.5 part of urea and 0.1-0.15 part of potassium citrate monohydrate into 100 parts of deionized water, and stirring for 20-30 minutes to obtain a mixed solution; and then transferring the mixed solution into an oven, preserving heat for 4 hours at 100 ℃, cooling to room temperature, transferring into the oven again, preserving heat for 4 hours at 110 ℃, and centrifuging to obtain the double-shell hollow nano zinc oxide.
Preferably, the specific method of step (2) is as follows, in parts by weight: preheating 100 parts of adipic acid to 120-130 ℃; then, under the protection of nitrogen, slowly dropwise adding 25-35 parts of 1, 4-cyclohexanediamine, and then slowly adding 4-6 parts of modified double-shell hollow nano-zinc oxide and 2-3 parts of polyamino nano-silicon dioxide; then heating to 220-230 ℃ while stirring, and keeping the temperature and stirring for 3-4 hours; and finally, keeping the temperature unchanged, reducing the pressure to 0.01Mpa, performing polycondensation for 0.5 hour, removing water and unreacted 1, 4-cyclohexanediamine, cooling to 130-140 ℃, and discharging to obtain the modified low-molecular polyamide.
Preferably, in the step (2), the preparation method of the polyamino nano-silica comprises the following steps: adding 1 part of n-butyl titanate into 20-25 parts of absolute ethyl alcohol, uniformly stirring and dispersing, then adding 0.5 part of diethylenetriamine and 0.43 part of methyl acrylate, dropwise adding ammonia water with the mass concentration of 20-25%, stirring for 4-5 hours, then transferring to a rotary evaporator, and treating for 4-5 hours at the temperature of 150-170 ℃ and under the pressure of 0.08-0.09 MPa to obtain the polyamino loaded nano silicon dioxide powder.
Preferably, in the step (3), the mass ratio of the polyether sulfone resin, the modified low-molecular polyamide, the rosin resin, the hydrogenated DCPD resin and the dibutyl phthalate is 100: 20-30: 10-20: 6-9: 5 to 7.
Preferably, in the step (3), the process conditions of the mixing and melting are as follows: mixing and melting for 5-7 minutes at 200-220 ℃.
Preferably, in the step (3), the temperature is reduced to 35-45 ℃, and then dibutyl phthalate is added; the technological conditions of heating and stirring are as follows: mixing and stirring for 30-40 minutes at 200-220 ℃.
In addition, the invention also claims a high-temperature aging resistant glue for magic tapes prepared by the preparation method.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) firstly, carrying out modification treatment on double-shell hollow nano zinc oxide by N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane to obtain modified double-shell hollow nano zinc oxide; then, adipic acid, 1, 4-cyclohexanediamine, modified double-shell hollow nano-zinc oxide and polyamino nano-silicon dioxide are used as raw materials, and a modified low-molecular polyamide is obtained through a polymerization reaction; and finally, mixing and melting the polyether sulfone resin, the modified low-molecular polyamide, the rosin resin and the hydrogenated DCPD resin, cooling, adding dibutyl phthalate, heating and uniformly stirring to obtain the glue for the magic tape.
(2) The main raw material of the invention is polyether sulfone resin, which provides better cohesiveness and high temperature resistance effect, while the modified low molecular polyamide contains abundant amino groups and the like, which can form hydrogen bonds with polyether sulfone resin, thus playing a role in improving the cohesiveness, high temperature aging resistance and ultraviolet aging resistance of the product. In addition, when the modified low-molecular-weight polyamide is prepared, the modified double-shell hollow nano-zinc oxide and the polyamino nano-silicon dioxide are added, the reaction can be performed in the generation process of the polyamide, and the double-shell hollow nano-zinc oxide and the nano-silicon dioxide have nano sizes, so that the improvement of high temperature resistance, ultraviolet resistance and caking property is facilitated, and the anti-aging effect is achieved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A method for manufacturing high-temperature aging resistant glue for magic tapes comprises the following specific steps:
(1) adding 1g of double-shell hollow nano-zinc oxide into 5g of N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxysilane, stirring and reacting for 7 hours at 95 ℃, centrifuging and taking precipitate to obtain the modified double-shell hollow nano-zinc oxide;
(2) 100g of adipic acid are preheated to 130 ℃; then under the protection of nitrogen, slowly dripping 25g of 1, 4-cyclohexanediamine, and slowly adding 6g of modified double-shell hollow nano-zinc oxide and 2g of polyamino nano-silicon dioxide; then heating to 230 ℃ while stirring, preserving heat and stirring for 3 hours; finally, keeping the temperature unchanged, reducing the pressure to 0.01Mpa, performing polycondensation for 0.5 hour, removing water and unreacted 1, 4-cyclohexanediamine, cooling to 140 ℃, and discharging to obtain the modified low-molecular polyamide;
(3) and finally, mixing and melting 25g of polyether sulfone resin, 5g of modified low-molecular polyamide, 5g of rosin resin and 1.5g of hydrogenated DCPD resin at 200 ℃ for 7 minutes, cooling to 35 ℃, adding 1.75g of dibutyl phthalate, mixing and stirring at 220 ℃ for 30 minutes to obtain the glue for the magic tape.
In the step (1), the preparation method of the double-shell hollow nano zinc oxide comprises the following steps: firstly, 0.6g of zinc nitrate hexahydrate, 0.4g of urea and 0.15g of potassium citrate monohydrate are added into 100g of deionized water, and stirred for 20 minutes to obtain a mixed solution; and then transferring the mixed solution into an oven, preserving heat for 4 hours at 100 ℃, cooling to room temperature, transferring into the oven again, preserving heat for 4 hours at 110 ℃, and centrifuging to obtain the double-shell hollow nano zinc oxide.
In the step (2), the preparation method of the polyamino nano silicon dioxide comprises the following steps: firstly, adding 1g of n-butyl titanate into 20g of absolute ethyl alcohol, uniformly stirring and dispersing, then adding 0.5g of diethylenetriamine and 0.43g of methyl acrylate, dropwise adding ammonia water with the mass concentration of 25%, stirring for 4 hours, then transferring to a rotary evaporator, and treating for 5 hours at the temperature of 170 ℃ and under the pressure of 0.008Mpa to obtain the polyamino loaded nano silicon dioxide powder.
Example 2
A method for manufacturing high-temperature aging resistant glue for magic tapes comprises the following specific steps:
(1) adding 1g of double-shell hollow nano-zinc oxide into 7g of N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxysilane, stirring and reacting for 9 hours at 85 ℃, centrifuging and taking precipitate to obtain the modified double-shell hollow nano-zinc oxide;
(2) 100g of adipic acid are preheated to 120 ℃; then under the protection of nitrogen, slowly dripping 35g of 1, 4-cyclohexanediamine, and slowly adding 4g of modified double-shell hollow nano-zinc oxide and 3g of polyamino nano-silicon dioxide; then heating to 220 ℃ while stirring, preserving heat and stirring for 4 hours; finally, keeping the temperature unchanged, reducing the pressure to 0.01Mpa, performing polycondensation for 0.5 hour, removing water and unreacted 1, 4-cyclohexanediamine, cooling to 130 ℃, and discharging to obtain the modified low-molecular polyamide;
(3) and finally, mixing and melting 25g of polyether sulfone resin, 7.5g of modified low-molecular-weight polyamide, 2.5g of rosin resin and 1.8g of hydrogenated DCPD resin at 220 ℃ for 5 minutes, cooling to 45 ℃, adding 1g of dibutyl phthalate, and mixing and stirring at 200 ℃ for 40 minutes to obtain the glue for the magic tape.
In the step (1), the preparation method of the double-shell hollow nano zinc oxide comprises the following steps: firstly, 0.5g of zinc nitrate hexahydrate, 0.5g of urea and 0.1g of potassium citrate monohydrate are added into 100g of deionized water, and stirred for 30 minutes to obtain a mixed solution; and then transferring the mixed solution into an oven, preserving heat for 4 hours at 100 ℃, cooling to room temperature, transferring into the oven again, preserving heat for 4 hours at 110 ℃, and centrifuging to obtain the double-shell hollow nano zinc oxide.
In the step (2), the preparation method of the polyamino nano silicon dioxide comprises the following steps: firstly, adding 1g of n-butyl titanate into 25g of absolute ethyl alcohol, uniformly stirring and dispersing, then adding 0.5g of diethylenetriamine and 0.43g of methyl acrylate, dropwise adding ammonia water with the mass concentration of 20%, stirring and treating for 5 hours, then transferring to a rotary evaporator, and treating for 4 hours at the temperature of 150 ℃ and under the pressure of 0.09Mpa to obtain the polyamino loaded nano silicon dioxide powder.
Example 3
A method for manufacturing high-temperature aging resistant glue for magic tapes comprises the following specific steps:
(1) adding 1g of double-shell hollow nano-zinc oxide into 6g of N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxysilane, stirring and reacting for 8 hours at 90 ℃, centrifuging and taking precipitate to obtain the modified double-shell hollow nano-zinc oxide;
(2) 100g of adipic acid were preheated to 125 ℃; then, under the protection of nitrogen, slowly adding 1, 4-cyclohexanediamine in a dropwise manner, and then slowly adding 5g of modified double-shell hollow nano-zinc oxide and 2.5g of polyamino nano-silicon dioxide; then heating to 225 ℃ while stirring, and keeping the temperature and stirring for 3.5 hours; finally, keeping the temperature unchanged, reducing the pressure to 0.01Mpa, performing polycondensation for 0.5 hour, removing water and unreacted 1, 4-cyclohexanediamine, cooling to 135 ℃, and discharging to obtain the modified low-molecular polyamide;
(3) and finally, mixing and melting 20g of polyether sulfone resin, 5g of modified low-molecular polyamide, 3g of rosin resin and 1.6g of hydrogenated DCPD resin at 210 ℃ for 6 minutes, cooling to 40 ℃, adding 1.2g of dibutyl phthalate, and mixing and stirring at 210 ℃ for 35 minutes to obtain the glue for the magic tape. The mass ratio of the polyether sulfone resin to the modified low-molecular polyamide to the rosin resin to the hydrogenated DCPD resin to the dibutyl phthalate is 100: 25: 15: 8: 6.
in the step (1), the preparation method of the double-shell hollow nano zinc oxide comprises the following steps: firstly, 0.55g of zinc nitrate hexahydrate, 0.45g of urea and 0.12g of potassium citrate monohydrate are added into 100g of deionized water, and stirred for 25 minutes to obtain a mixed solution; and then transferring the mixed solution into an oven, preserving heat for 4 hours at 100 ℃, cooling to room temperature, transferring into the oven again, preserving heat for 4 hours at 110 ℃, and centrifuging to obtain the double-shell hollow nano zinc oxide.
In the step (2), the preparation method of the polyamino nano silicon dioxide comprises the following steps: adding 1g of n-butyl titanate into 22g of absolute ethyl alcohol, uniformly stirring and dispersing, then adding 0.5g of diethylenetriamine and 0.43g of methyl acrylate, dropwise adding ammonia water with the mass concentration of 22%, stirring for 4.5 hours, then transferring to a rotary evaporator, and treating for 4.5 hours at 160 ℃ and 0.08MPa to obtain the polyamino loaded nano silicon dioxide powder.
Comparative example 1
A manufacturing method of glue for a magic tape comprises the following specific steps:
(1) 100g of adipic acid are preheated to 130 ℃; then under the protection of nitrogen, slowly dripping 25g of 1, 4-cyclohexanediamine, heating to 230 ℃ while stirring, and keeping the temperature and stirring for 3 hours; finally, keeping the temperature unchanged, reducing the pressure to 0.01Mpa, performing polycondensation for 0.5 hour, removing water and unreacted 1, 4-cyclohexanediamine, cooling to 140 ℃, and discharging to obtain the low-molecular polyamide;
(2) mixing and melting 25g of polyether sulfone resin, 5g of low-molecular polyamide, 5g of rosin resin and 1.5g of hydrogenated DCPD resin at 200 ℃ for 7 minutes, cooling to 35 ℃, adding 1.75g of dibutyl phthalate, mixing and stirring at 220 ℃ for 30 minutes to obtain the glue for the magic tape.
After melting the glue for magic tapes obtained in examples 1-3 or comparative example 1 at 175 ℃, the glue is prepared into a glue sample for standby.
1. Initial tack test: refer to GB/T4852 & 2002-2The gluing amount of the adhesive tape is uniformly coated on the back surface of a magic tape with the thickness of 25mm multiplied by 250 mm. Wherein, the test method adopts a method A: the angle of the inclined plane is 30 degrees by the inclined plane rolling ball method. The magic tape is fixed on the inclined plane with the side coated with the glue sample facing upwards, and the rolling ball device is horizontally fixed on the test board. And rolling the test steel ball from small to large sequentially from the rolling-assisting section at the position of 10cm of the inclined plane, and recording the maximum ball number which can be stuck by the glue sample, namely the initial sticking force. After 5 tests on each sample, the results are averaged as shown in Table 1.
2. Tack-holding test: reference GB/T4851-1998 pressure-sensitive adhesive tape holding adhesion testTest method, mixing glue sample at 25g/m2The gluing amount of the adhesive tape is uniformly coated on the back surface of a magic tape with the thickness of 25mm multiplied by 100 mm. Dividing a steel plate for testing into a test plate and a loading plate, pasting the surface of the magic tape coated with the glue sample on the test plate in parallel with the longitudinal direction of the plate, sticking the magic tape on the test plate, pressing the magic tape back and forth for three times at the speed of 300mm/min by using a press roller, and then placing the magic tape for 20 minutes. The test plate was vertically fixed to a test stand, and a 1kg weight was attached to one end of the load plate to record the time at which the sample completely separated. After 5 tests on each sample, the results are averaged as shown in Table 1.
3.180 ° peel strength test: referring to GB/T2792-1998 test method for 180 DEG peeling strength of pressure-sensitive adhesive tape, samples of the adhesive are 25g/m2The gluing amount of the adhesive tape is uniformly coated on the back surface of a magic tape with the thickness of 25mm multiplied by 250 mm. And (3) sticking one surface of the magic tape coated with the glue sample to the cleaned test board, pressing the surface of the magic tape back and forth three times at the speed of 300mm/min by using a press roller, and standing for 20 minutes after no air bubbles exist at the bonding position of the test sample and the test board. The test piece was peeled from the test plate at 180 ℃ by a peeling machine at a speed of 300mm/min, and the 180 ℃ peel strength was calculated by recording a curve by an instrument. After 5 tests on each sample, the results are averaged as shown in Table 1.
4. Ultraviolet light aging resistance test: the light source adopts a UVB313 ultraviolet lamp, the illumination and condensation temperatures are respectively 60 ℃ and 40 ℃, the time is respectively 4 hours and 4 hours, and the illumination and condensation are alternately carried out for 1000 hours. The yellowing index (delta YI) after thermo-oxidative aging resistance and ultraviolet light aging resistance is tested according to GB2409-80 Plastic yellow index test method.
TABLE 1 Performance test results
Initial viscosity (ball) Tackiness (h) 180 degree peel strength (kN/m) Ultraviolet light aging resistant delta YI
Example 1 25# 77 0.96 0.15
Example 2 24# 72 0.94 0.19
Example 3 24# 73 0.91 0.13
Comparative example 1 15# 48 0.53 0.32
As can be seen from Table 1, the initial tack number of the glue for hook and loop fasteners obtained in examples 1 to 3 has a long lasting tack, a high 180-degree peel strength, and excellent high temperature aging resistance and ultraviolet aging resistance.
Comparative example 1 the modified low molecular polyamide was replaced with the low molecular polyamide, and the high temperature aging resistance of the obtained adhesive for hook and loop fasteners was remarkably deteriorated.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (9)

1. The manufacturing method of the high-temperature aging resistant glue for the magic tape is characterized by comprising the following specific steps of:
(1) modifying double-shell hollow nano zinc oxide by N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane to obtain modified double-shell hollow nano zinc oxide;
(2) carrying out polymerization reaction on adipic acid, 1, 4-cyclohexanediamine, the modified double-shell hollow nano-zinc oxide prepared in the step (1) and polyamino nano-silicon dioxide serving as raw materials to prepare modified low-molecular-weight polyamide;
(3) and (3) mixing and melting polyether sulfone resin, the modified low-molecular-weight polyamide prepared in the step (2), rosin resin and hydrogenated DCPD resin, cooling, adding dibutyl phthalate, and heating and stirring uniformly to obtain the glue for the magic tape.
2. The manufacturing method according to claim 1, wherein the specific method of step (1) is as follows in parts by weight: adding 1 part of double-shell hollow nano-zinc oxide into 5-7 parts of N- (beta-aminoethyl) -gamma-aminopropylmethyldimethoxysilane, stirring and reacting for 7-9 hours at 85-95 ℃, and centrifuging to obtain a precipitate, thus obtaining the modified double-shell hollow nano-zinc oxide.
3. The manufacturing method according to claim 1, wherein in the step (1), the double-shell hollow nano zinc oxide is prepared by the following steps in parts by weight: adding 0.5-0.6 part of zinc nitrate hexahydrate, 0.4-0.5 part of urea and 0.1-0.15 part of potassium citrate monohydrate into 100 parts of deionized water, and stirring for 20-30 minutes to obtain a mixed solution; and then transferring the mixed solution into an oven, preserving heat for 4 hours at 100 ℃, cooling to room temperature, transferring into the oven again, preserving heat for 4 hours at 110 ℃, and centrifuging to obtain the double-shell hollow nano zinc oxide.
4. The manufacturing method according to claim 1, wherein the specific method of step (2) is as follows in parts by weight: preheating 100 parts of adipic acid to 120-130 ℃; then, under the protection of nitrogen, slowly dropwise adding 25-35 parts of 1, 4-cyclohexanediamine, and then slowly adding 4-6 parts of modified double-shell hollow nano-zinc oxide and 2-3 parts of polyamino nano-silicon dioxide; then heating to 220-230 ℃ while stirring, and keeping the temperature and stirring for 3-4 hours; and finally, keeping the temperature unchanged, reducing the pressure to 0.01Mpa, performing polycondensation for 0.5 hour, removing water and unreacted 1, 4-cyclohexanediamine, cooling to 130-140 ℃, and discharging to obtain the modified low-molecular polyamide.
5. The method according to claim 1, wherein in the step (2), the polyamino nanosilica is prepared by the following method in parts by weight: adding 1 part of n-butyl titanate into 20-25 parts of absolute ethyl alcohol, stirring and dispersing uniformly, then adding 0.5 part of diethylenetriamine and 0.43 part of methyl acrylate, dropwise adding ammonia water with the mass concentration of 20-25%, stirring for 4-5 hours, then transferring to a rotary evaporator, and treating for 4-5 hours at the temperature of 150-170 ℃ and under the pressure of 0.008-0.09 MPa to obtain the polyamino loaded nano silicon dioxide powder.
6. The production method according to claim 1, wherein in the step (3), the mass ratio of the polyether sulfone resin, the modified low-molecular polyamide, the rosin resin, the hydrogenated DCPD resin and the dibutyl phthalate is 100: 20-30: 10-20: 6-9: 5 to 7.
7. The manufacturing method according to claim 1, wherein in the step (3), the process conditions of the mixing and melting are as follows: mixing and melting for 5-7 minutes at 200-220 ℃.
8. The preparation method according to claim 1, wherein in the step (3), the temperature is reduced to 35-45 ℃, and dibutyl phthalate is added; the technological conditions of heating and stirring are as follows: mixing and stirring for 30-40 minutes at 200-220 ℃.
9. A high temperature aging resistant glue for magic tapes prepared by the preparation method of any one of claims 1 to 8.
CN202111072749.3A 2021-09-14 2021-09-14 High-temperature aging resistant glue for magic tape and manufacturing method thereof Withdrawn CN113583621A (en)

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Application publication date: 20211102