CN113512377B - High-viscosity weather-resistant hot melt adhesive and preparation method thereof - Google Patents

High-viscosity weather-resistant hot melt adhesive and preparation method thereof Download PDF

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CN113512377B
CN113512377B CN202110444644.XA CN202110444644A CN113512377B CN 113512377 B CN113512377 B CN 113512377B CN 202110444644 A CN202110444644 A CN 202110444644A CN 113512377 B CN113512377 B CN 113512377B
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titanium dioxide
hot melt
melt adhesive
polysiloxane
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CN113512377A (en
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李炳亮
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Foshan Gebang Polymer 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
    • C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
    • C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
    • C09J123/04—Homopolymers or copolymers of ethene
    • C09J123/08—Copolymers of ethene
    • C09J123/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
    • C09J123/0853—Vinylacetate
    • 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
    • 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
    • C08K2003/2237—Oxides; Hydroxides of metals of titanium
    • C08K2003/2241—Titanium dioxide
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention is applicable to the technical field of hot melt adhesives, and provides a high-viscosity weather-resistant hot melt adhesive and a preparation method thereof, wherein the hot melt adhesive comprises the following components in parts by weight: 50-70 parts of ethylene-vinyl acetate copolymer, 6-8 parts of modified titanium dioxide, 0.2-0.4 part of antioxidant, 10-14 parts of tackifier, 0.6-0.8 part of coupling agent, 1.2-1.4 parts of flatting agent, 0.6-0.8 part of plasticizer and 3-7 parts of filler; the ethylene-vinyl acetate copolymer is modified by the modified titanium dioxide, so that the hot melt adhesive has good weather resistance on the basis of high viscosity, and is beneficial to long-term use; and the titanium dioxide is modified by polysiloxane and diethylamino hydroxybenzoyl hexyl benzoate, so that the weather resistance of the hot melt adhesive is further improved.

Description

High-viscosity weather-resistant hot melt adhesive and preparation method thereof
Technical Field
The invention belongs to the technical field of hot melt adhesives, and particularly relates to a high-viscosity weather-resistant hot melt adhesive and a preparation method thereof.
Background
With the development of society, metal materials and reinforced plastics are more and more widely applied, and the metal materials have the advantages of electric conduction, heat conduction, high hardness, high strength, high density, high melting point, high toughness and the like; polyamide is one of the most widely used general engineering plastics, and has the advantages of unique low specific gravity, high tensile strength, wear resistance, good self-lubricating property, excellent impact toughness, and both rigidity and flexibility, thereby gaining attention of people. The application of direct bonding of metal and polyamide plastic is wider and wider, and the metal and polyamide plastic are more and more applied to the electronic and electrical industry, the mechanical industry and the like.
Due to the structural difference between metal and plastic, the properties of the two materials are greatly different, so that the interface bonding strength is low and the two materials are easy to fall off; therefore, the hot melt adhesive is usually used for assisting the combination of metal and plastic, is a plastic adhesive, has the physical state changed along with the temperature change within a certain temperature range and unchanged chemical characteristics, is non-toxic and tasteless, and belongs to an environment-friendly chemical product. The existing hot melt adhesive has general weather resistance while meeting high viscosity, is not beneficial to long-term use and is difficult to meet the use requirement.
Disclosure of Invention
The invention aims to provide a high-viscosity weather-resistant hot melt adhesive and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides a high-viscosity weather-resistant hot melt adhesive which comprises the following components in parts by weight:
50-70 parts of ethylene-vinyl acetate copolymer, 6-8 parts of modified titanium dioxide, 0.2-0.4 part of antioxidant, 10-14 parts of tackifier, 0.6-0.8 part of coupling agent, 1.2-1.4 parts of flatting agent, 0.6-0.8 part of plasticizer and 3-7 parts of filler.
Preferably, the composition comprises the following components in parts by weight:
55-70 parts of ethylene-vinyl acetate copolymer, 6.5-8 parts of modified titanium dioxide, 0.25-0.4 part of antioxidant, 11-14 parts of tackifier, 0.65-0.8 part of coupling agent, 1.25-1.4 parts of flatting agent, 0.65-0.8 part of plasticizer and 4-7 parts of filler.
Preferably, the composition comprises the following components in parts by weight:
55-65 parts of ethylene-vinyl acetate copolymer, 6.5-7.5 parts of modified titanium dioxide, 0.25-0.35 part of antioxidant, 11-13 parts of tackifier, 0.65-0.75 part of coupling agent, 1.25-1.35 parts of flatting agent, 0.65-0.75 part of plasticizer and 4-6 parts of filler.
Preferably, the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.8-1: 1.
preferably, the tackifier is one of a phenolic resin, a xylene formaldehyde resin or a polyterpene resin.
Preferably, the plasticizer is one of dicyclohexyl phthalate, dibutyl phthalate or di-sec-octyl phthalate.
Preferably, the filler is one of calcium carbonate, talc or silica.
The preparation method of the high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) preparing modified titanium dioxide: firstly, crushing and grinding titanium dioxide, and then putting crushed titanium dioxide powder, polysiloxane and diethyl amino hydroxy benzoyl benzoic acid hexyl ester into a mixing tank, so that the total mass of the polysiloxane and the diethyl amino hydroxy benzoyl benzoic acid hexyl ester is 40-50% of the mass of the titanium dioxide powder, and the mass ratio of the polysiloxane to the diethyl amino hydroxy benzoyl benzoic acid hexyl ester is 1.3-1.5: 1, mixing and stirring at 60-70 ℃, uniformly stirring, drying and crushing to obtain modified titanium dioxide;
(2) weighing raw materials in parts by weight: the hot melt adhesive is prepared by the following steps of (1) inputting the weighed raw materials into a stirrer, uniformly stirring the raw materials, inputting the uniformly mixed materials into a screw extruder, and performing melt extrusion at the temperature of 110-120 ℃ to obtain the hot melt adhesive.
In summary, due to the adoption of the technical scheme, the method has the following beneficial effects:
the invention provides a high-viscosity weather-resistant hot melt adhesive and a preparation method thereof, wherein the ethylene-vinyl acetate copolymer is modified by modified titanium dioxide, so that the hot melt adhesive has good weather resistance on the basis of high viscosity, and is beneficial to long-term use; and the titanium dioxide is modified by polysiloxane and diethylamino hydroxybenzoyl hexyl benzoate, so that the thermal stability is further improved on the basis that the titanium dioxide has an excellent ultraviolet resistance function, and the weather resistance of the hot melt adhesive is further improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The existing hot melt adhesive has general weather resistance while meeting high viscosity, is not beneficial to long-term use and is difficult to meet the use requirement. The ethylene-vinyl acetate copolymer is modified by the modified titanium dioxide, so that the hot melt adhesive has good weather resistance on the basis of high viscosity, and is beneficial to long-term use.
Example 1
A preparation method of a high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) preparing modified titanium dioxide: firstly, crushing and grinding titanium dioxide, sieving the crushed titanium dioxide with a 200-mesh sieve, then putting the crushed titanium dioxide powder, polysiloxane and diethyl amino hydroxy benzoyl benzoate into a mixing tank, wherein the total mass of the polysiloxane and the diethyl amino hydroxy benzoyl benzoate is 40% of the mass of the titanium dioxide powder, and the mass ratio of the polysiloxane to the diethyl amino hydroxy benzoyl benzoate is 1.3: 1, mixing and stirring at 60 ℃ until the rotating speed is 180r/min, stirring for 60min, then drying, crushing and sieving with a 150-mesh sieve to obtain modified titanium dioxide;
(2) weighing raw materials in corresponding weight: 500g of ethylene-vinyl acetate copolymer, 60g of modified titanium dioxide, 2g of antioxidant, 100g of tackifier, 6g of coupling agent, 12g of flatting agent, 6g of plasticizer and 30g of filler; the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.8: 1, the tackifier is phenolic resin, the coupling agent is a titanate coupling agent, the leveling agent is a modified polysiloxane type leveling agent, the plasticizer is dicyclohexyl phthalate, and the filler is calcium carbonate; and then inputting the weighed raw materials into a stirrer, uniformly stirring, inputting the uniformly mixed materials into a screw extruder, and melting and extruding at the temperature of 110 ℃ to obtain the hot melt adhesive.
Example 2
A preparation method of a high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) preparing modified titanium dioxide: firstly, crushing and grinding titanium dioxide, sieving the crushed titanium dioxide with a 200-mesh sieve, then putting the crushed titanium dioxide powder, polysiloxane and diethyl amino hydroxy benzoyl benzoate into a mixing tank, wherein the total mass of the polysiloxane and the diethyl amino hydroxy benzoyl benzoate is 50% of the mass of the titanium dioxide powder, and the mass ratio of the polysiloxane to the diethyl amino hydroxy benzoyl benzoate is 1.3: 1, mixing and stirring at 70 ℃ until the rotating speed is 200r/min, stirring for 80min, drying, crushing and sieving with a 150-mesh sieve to obtain modified titanium dioxide;
(2) weighing raw materials in corresponding weight: 700g of ethylene-vinyl acetate copolymer, 80g of modified titanium dioxide, 4g of antioxidant, 140g of tackifier, 8g of coupling agent, 14g of flatting agent, 8g of plasticizer and 70g of filler; the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 1: 1, the tackifier is xylene formaldehyde resin, the coupling agent is a titanate coupling agent, the leveling agent is a modified polysiloxane type leveling agent, the plasticizer is dibutyl phthalate, and the filler is talcum powder; and then inputting the weighed raw materials into a stirrer, uniformly stirring, inputting the uniformly mixed materials into a screw extruder, and carrying out melt extrusion at the temperature of 120 ℃ to obtain the hot melt adhesive.
Example 3
A preparation method of a high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) preparing modified titanium dioxide: firstly, crushing and grinding titanium dioxide, sieving the crushed titanium dioxide with a 200-mesh sieve, then putting the crushed titanium dioxide powder, polysiloxane and diethyl amino hydroxy benzoyl benzoate into a mixing tank, wherein the total mass of the polysiloxane and the diethyl amino hydroxy benzoyl benzoate is 45% of the mass of the titanium dioxide powder, and the mass ratio of the polysiloxane to the diethyl amino hydroxy benzoyl benzoate is 1.3: 1, mixing and stirring at 65 ℃ until the rotating speed is 190r/min, stirring for 70min, drying, crushing and sieving with a 150-mesh sieve to obtain modified titanium dioxide;
(2) weighing raw materials in corresponding weight: 550g of ethylene-vinyl acetate copolymer, 65g of modified titanium dioxide, 2.5g of antioxidant, 110g of tackifier, 6.5g of coupling agent, 12.5g of leveling agent, 6.5g of plasticizer and 40g of filler; the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.9: 1, the tackifier is polyterpene resin, the coupling agent is a titanate coupling agent, the leveling agent is a modified polysiloxane type leveling agent, the plasticizer is di-sec-octyl phthalate, and the filler is silicon dioxide; and then inputting the weighed raw materials into a stirrer, uniformly stirring, inputting the uniformly mixed materials into a screw extruder, and carrying out melt extrusion at the temperature of 115 ℃ to obtain the hot melt adhesive.
Example 4
A preparation method of a high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) preparing modified titanium dioxide: firstly, crushing and grinding titanium dioxide, sieving the crushed titanium dioxide with a 200-mesh sieve, then putting the crushed titanium dioxide powder, polysiloxane and diethyl amino hydroxy benzoyl benzoate into a mixing tank, wherein the total mass of the polysiloxane and the diethyl amino hydroxy benzoyl benzoate is 45% of the mass of the titanium dioxide powder, and the mass ratio of the polysiloxane to the diethyl amino hydroxy benzoyl benzoate is 1.3: 1, mixing and stirring at 65 ℃ until the rotating speed is 190r/min, stirring for 70min, drying, crushing and sieving with a 150-mesh sieve to obtain modified titanium dioxide;
(2) weighing raw materials in corresponding weight: 600g of ethylene-vinyl acetate copolymer, 70g of modified titanium dioxide, 3g of antioxidant, 120g of tackifier, 7g of coupling agent, 13g of flatting agent, 7g of plasticizer and 50g of filler; the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.9: 1, the tackifier is phenolic resin, the coupling agent is a titanate coupling agent, the leveling agent is a modified polysiloxane type leveling agent, the plasticizer is dicyclohexyl phthalate, and the filler is silicon dioxide; and then inputting the weighed raw materials into a stirrer, uniformly stirring, inputting the uniformly mixed materials into a screw extruder, and carrying out melt extrusion at the temperature of 115 ℃ to obtain the hot melt adhesive.
Example 5
A preparation method of a high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) preparing modified titanium dioxide: firstly, crushing and grinding titanium dioxide, sieving the crushed titanium dioxide with a 200-mesh sieve, then putting the crushed titanium dioxide powder, polysiloxane and diethyl amino hydroxy benzoyl benzoate into a mixing tank, wherein the total mass of the polysiloxane and the diethyl amino hydroxy benzoyl benzoate is 45% of the mass of the titanium dioxide powder, and the mass ratio of the polysiloxane to the diethyl amino hydroxy benzoyl benzoate is 1.3: 1, mixing and stirring at 65 ℃ until the rotating speed is 190r/min, stirring for 70min, drying, crushing and sieving with a 150-mesh sieve to obtain modified titanium dioxide;
(2) weighing raw materials in corresponding weight: 650g of ethylene-vinyl acetate copolymer, 75g of modified titanium dioxide, 3.5g of antioxidant, 130g of tackifier, 7.5g of coupling agent, 13.5g of leveling agent, 7.5g of plasticizer and 60g of filler; the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.9: 1, the tackifier is phenolic resin, the coupling agent is a titanate coupling agent, the leveling agent is a modified polysiloxane type leveling agent, the plasticizer is dicyclohexyl phthalate, and the filler is silicon dioxide; and then inputting the weighed raw materials into a stirrer, uniformly stirring, inputting the uniformly mixed materials into a screw extruder, and carrying out melt extrusion at the temperature of 115 ℃ to obtain the hot melt adhesive.
Example 6
A preparation method of a high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) preparing modified titanium dioxide: firstly, crushing and grinding titanium dioxide, sieving the crushed titanium dioxide with a 200-mesh sieve, then putting the crushed titanium dioxide powder, polysiloxane and diethyl amino hydroxy benzoyl benzoate into a mixing tank, wherein the total mass of the polysiloxane and the diethyl amino hydroxy benzoyl benzoate is 45% of the mass of the titanium dioxide powder, and the mass ratio of the polysiloxane to the diethyl amino hydroxy benzoyl benzoate is 1.3: 1, mixing and stirring at 65 ℃ until the rotating speed is 190r/min, stirring for 70min, drying, crushing and sieving with a 150-mesh sieve to obtain modified titanium dioxide;
(2) weighing raw materials in corresponding weight: 600g of ethylene-vinyl acetate copolymer, 70g of modified titanium dioxide, 3g of antioxidant, 120g of tackifier, 7g of coupling agent, 13g of leveling agent, 7g of plasticizer and 50g of filler; the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.9: 1, the tackifier is polyterpene resin, the coupling agent is a titanate coupling agent, the leveling agent is a modified polysiloxane type leveling agent, the plasticizer is dicyclohexyl phthalate, and the filler is silicon dioxide; and then inputting the weighed raw materials into a stirrer, uniformly stirring, inputting the uniformly mixed materials into a screw extruder, and carrying out melt extrusion at the temperature of 115 ℃ to obtain the hot melt adhesive.
Example 7
A preparation method of a high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) preparing modified titanium dioxide: firstly, crushing and grinding titanium dioxide, sieving the crushed titanium dioxide with a 200-mesh sieve, then putting the crushed titanium dioxide powder, polysiloxane and diethyl amino hydroxy benzoyl benzoate into a mixing tank, wherein the total mass of the polysiloxane and the diethyl amino hydroxy benzoyl benzoate is 45% of the mass of the titanium dioxide powder, and the mass ratio of the polysiloxane to the diethyl amino hydroxy benzoyl benzoate is 1.3: 1, mixing and stirring at 65 ℃ until the rotating speed is 190r/min, stirring for 70min, drying, crushing and sieving with a 150-mesh sieve to obtain modified titanium dioxide;
(2) weighing raw materials in corresponding weight: 600g of ethylene-vinyl acetate copolymer, 70g of modified titanium dioxide, 3g of antioxidant, 120g of tackifier, 7g of coupling agent, 13g of flatting agent, 7g of plasticizer and 50g of filler; the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.9: 1, the tackifier is polyterpene resin, the coupling agent is a titanate coupling agent, the leveling agent is a modified polysiloxane type leveling agent, the plasticizer is dicyclohexyl phthalate, and the filler is calcium carbonate; and then inputting the weighed raw materials into a stirrer, uniformly stirring, inputting the uniformly mixed materials into a screw extruder, and carrying out melt extrusion at the temperature of 115 ℃ to obtain the hot melt adhesive.
Example 8
A preparation method of a high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) preparing modified titanium dioxide: firstly, crushing and grinding titanium dioxide, sieving the crushed titanium dioxide with a 200-mesh sieve, then putting the crushed titanium dioxide powder, polysiloxane and diethyl amino hydroxy benzoyl benzoate into a mixing tank, wherein the total mass of the polysiloxane and the diethyl amino hydroxy benzoyl benzoate is 45% of the mass of the titanium dioxide powder, and the mass ratio of the polysiloxane to the diethyl amino hydroxy benzoyl benzoate is 1.3: 1, mixing and stirring at 65 ℃ until the rotating speed is 190r/min, stirring for 70min, drying, crushing and sieving with a 150-mesh sieve to obtain modified titanium dioxide;
(2) weighing raw materials in corresponding weight: 600g of ethylene-vinyl acetate copolymer, 70g of modified titanium dioxide, 3g of antioxidant, 120g of tackifier, 7g of coupling agent, 13g of flatting agent, 7g of plasticizer and 50g of filler; the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.9: 1, the tackifier is polyterpene resin, the coupling agent is a titanate coupling agent, the leveling agent is a modified polysiloxane type leveling agent, the plasticizer is dicyclohexyl phthalate, and the filler is talcum powder; and then inputting the weighed raw materials into a stirrer, uniformly stirring, inputting the uniformly mixed materials into a screw extruder, and carrying out melt extrusion at the temperature of 115 ℃ to obtain the hot melt adhesive.
Example 9
A preparation method of a high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) preparing modified titanium dioxide: firstly, crushing and grinding titanium dioxide, sieving the crushed titanium dioxide with a 200-mesh sieve, then putting the crushed titanium dioxide powder, polysiloxane and diethyl amino hydroxy benzoyl benzoate into a mixing tank, wherein the total mass of the polysiloxane and the diethyl amino hydroxy benzoyl benzoate is 45% of the mass of the titanium dioxide powder, and the mass ratio of the polysiloxane to the diethyl amino hydroxy benzoyl benzoate is 1.35: 1, mixing and stirring at 65 ℃ until the rotating speed is 190r/min, stirring for 70min, drying, crushing and sieving with a 150-mesh sieve to obtain modified titanium dioxide;
(2) weighing raw materials in corresponding weight: 600g of ethylene-vinyl acetate copolymer, 70g of modified titanium dioxide, 3g of antioxidant, 120g of tackifier, 7g of coupling agent, 13g of flatting agent, 7g of plasticizer and 50g of filler; the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.9: 1, the tackifier is polyterpene resin, the coupling agent is a titanate coupling agent, the leveling agent is a modified polysiloxane type leveling agent, the plasticizer is dicyclohexyl phthalate, and the filler is talcum powder; and then inputting the weighed raw materials into a stirrer, uniformly stirring, inputting the uniformly mixed materials into a screw extruder, and carrying out melt extrusion at the temperature of 115 ℃ to obtain the hot melt adhesive.
Example 10
A preparation method of a high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) preparing modified titanium dioxide: firstly, crushing and grinding titanium dioxide, sieving the crushed titanium dioxide with a 200-mesh sieve, then putting the crushed titanium dioxide powder, polysiloxane and diethyl amino hydroxy benzoyl benzoate into a mixing tank, wherein the total mass of the polysiloxane and the diethyl amino hydroxy benzoyl benzoate is 45% of the mass of the titanium dioxide powder, and the mass ratio of the polysiloxane to the diethyl amino hydroxy benzoyl benzoate is 1.4: 1, mixing and stirring at 65 ℃ until the rotating speed is 190r/min, stirring for 70min, drying, crushing and sieving with a 150-mesh sieve to obtain modified titanium dioxide;
(2) weighing raw materials in corresponding weight: 600g of ethylene-vinyl acetate copolymer, 70g of modified titanium dioxide, 3g of antioxidant, 120g of tackifier, 7g of coupling agent, 13g of flatting agent, 7g of plasticizer and 50g of filler; the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.9: 1, the tackifier is polyterpene resin, the coupling agent is a titanate coupling agent, the leveling agent is a modified polysiloxane type leveling agent, the plasticizer is dicyclohexyl phthalate, and the filler is talcum powder; and then inputting the weighed raw materials into a stirrer, uniformly stirring, inputting the uniformly mixed materials into a screw extruder, and carrying out melt extrusion at the temperature of 115 ℃ to obtain the hot melt adhesive.
Example 11
A preparation method of a high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) preparing modified titanium dioxide: firstly, crushing and grinding titanium dioxide, sieving the crushed titanium dioxide by a 200-mesh sieve, then putting the crushed titanium dioxide powder, polysiloxane and diethyl amino hydroxy benzoyl benzoate into a mixing tank, wherein the total mass of the polysiloxane and the diethyl amino hydroxy benzoyl benzoate is 45% of the mass of the titanium dioxide powder, and the mass ratio of the polysiloxane to the diethyl amino hydroxy benzoyl benzoate is 1.45: 1, mixing and stirring at 65 ℃ until the rotating speed is 190r/min, stirring for 70min, drying, crushing and sieving with a 150-mesh sieve to obtain modified titanium dioxide;
(2) weighing raw materials in corresponding weight: 600g of ethylene-vinyl acetate copolymer, 70g of modified titanium dioxide, 3g of antioxidant, 120g of tackifier, 7g of coupling agent, 13g of flatting agent, 7g of plasticizer and 50g of filler; the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.9: 1, the tackifier is polyterpene resin, the coupling agent is a titanate coupling agent, the leveling agent is a modified polysiloxane type leveling agent, the plasticizer is dicyclohexyl phthalate, and the filler is talcum powder; and then inputting the weighed raw materials into a stirrer, uniformly stirring, inputting the uniformly mixed materials into a screw extruder, and carrying out melt extrusion at the temperature of 115 ℃ to obtain the hot melt adhesive.
Example 12
A preparation method of a high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) preparing modified titanium dioxide: firstly, crushing and grinding titanium dioxide, sieving the crushed titanium dioxide with a 200-mesh sieve, then putting the crushed titanium dioxide powder, polysiloxane and diethyl amino hydroxy benzoyl benzoate into a mixing tank, wherein the total mass of the polysiloxane and the diethyl amino hydroxy benzoyl benzoate is 45% of the mass of the titanium dioxide powder, and the mass ratio of the polysiloxane to the diethyl amino hydroxy benzoyl benzoate is 1.5: 1, mixing and stirring at 65 ℃ until the rotating speed is 190r/min, stirring for 70min, drying, crushing and sieving with a 150-mesh sieve to obtain modified titanium dioxide;
(2) weighing raw materials in corresponding weight: 600g of ethylene-vinyl acetate copolymer, 70g of modified titanium dioxide, 3g of antioxidant, 120g of tackifier, 7g of coupling agent, 13g of leveling agent, 7g of plasticizer and 50g of filler; the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.9: 1, the tackifier is polyterpene resin, the coupling agent is a titanate coupling agent, the leveling agent is a modified polysiloxane type leveling agent, the plasticizer is dicyclohexyl phthalate, and the filler is talcum powder; and then inputting the weighed raw materials into a stirrer, uniformly stirring, inputting the uniformly mixed materials into a screw extruder, and carrying out melt extrusion at the temperature of 115 ℃ to obtain the hot melt adhesive.
Comparative example 1
A preparation method of a high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) weighing raw materials in parts by weight: 60 parts of ethylene-vinyl acetate copolymer, 7 parts of titanium dioxide, 0.3 part of antioxidant, 12 parts of tackifier, 0.7 part of coupling agent, 1.3 parts of flatting agent, 0.7 part of plasticizer and 5 parts of filler; the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.9: 1, the tackifier is polyterpene resin, the coupling agent is a titanate coupling agent, the leveling agent is a modified polysiloxane type leveling agent, the plasticizer is dicyclohexyl phthalate, and the filler is talcum powder; and then inputting the weighed raw materials into a stirrer, uniformly stirring, inputting the uniformly mixed materials into a screw extruder, and carrying out melt extrusion at the temperature of 115 ℃ to obtain the hot melt adhesive.
Comparative example 2
A preparation method of a high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) weighing raw materials in corresponding weight: 600g of ethylene-vinyl acetate copolymer, 0.30g of antioxidant, 120g of tackifier, 7g of coupling agent, 13g of flatting agent, 7g of plasticizer and 50g of filler; the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.9: 1, the tackifier is polyterpene resin, the coupling agent is a titanate coupling agent, the leveling agent is a modified polysiloxane type leveling agent, the plasticizer is dicyclohexyl phthalate, and the filler is talcum powder; and then inputting the weighed raw materials into a stirrer, uniformly stirring, inputting the uniformly mixed materials into a screw extruder, and carrying out melt extrusion at the temperature of 115 ℃ to obtain the hot melt adhesive.
Comparative example 3
A preparation method of a high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) preparing modified titanium dioxide: firstly, crushing and grinding titanium dioxide, sieving with a 200-mesh sieve, then putting the crushed titanium dioxide powder and polysiloxane into a mixing tank to enable the mass of the polysiloxane to be 45% of that of the titanium dioxide powder, mixing and stirring at 65 ℃ to enable the rotating speed to be 190r/min, stirring for 70min, then drying, crushing and sieving with a 150-mesh sieve to obtain modified titanium dioxide;
(2) weighing raw materials in corresponding weight: 600g of ethylene-vinyl acetate copolymer, 70g of modified titanium dioxide, 3g of antioxidant, 120g of tackifier, 7g of coupling agent, 13g of flatting agent, 7g of plasticizer and 50g of filler; the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.9: 1, the tackifier is polyterpene resin, the coupling agent is a titanate coupling agent, the leveling agent is a modified polysiloxane type leveling agent, the plasticizer is dicyclohexyl phthalate, and the filler is talcum powder; and then inputting the weighed raw materials into a stirrer, uniformly stirring, inputting the uniformly mixed materials into a screw extruder, and carrying out melt extrusion at the temperature of 115 ℃ to obtain the hot melt adhesive.
Comparative example 4
A preparation method of a high-viscosity weather-resistant hot melt adhesive specifically comprises the following steps:
(1) preparing modified titanium dioxide: firstly, crushing and grinding titanium dioxide, sieving with a 200-mesh sieve, then putting the crushed titanium dioxide powder and diethyl amino hydroxy benzoyl benzoic acid hexyl ester into a mixing tank, so that the mass of the diethyl amino hydroxy benzoyl benzoic acid hexyl ester is 45% of that of the titanium dioxide powder, mixing and stirring at 65 ℃ so that the rotating speed is 190r/min, stirring for 70min, then drying, crushing and sieving with a 150-mesh sieve to obtain modified titanium dioxide;
(2) weighing raw materials in corresponding weight: 600g of ethylene-vinyl acetate copolymer, 70g of modified titanium dioxide, 3g of antioxidant, 120g of tackifier, 7g of coupling agent, 13g of flatting agent, 7g of plasticizer and 50g of filler; the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.9: 1, the tackifier is polyterpene resin, the coupling agent is a titanate coupling agent, the leveling agent is a modified polysiloxane type leveling agent, the plasticizer is dicyclohexyl phthalate, and the filler is talcum powder; and then inputting the weighed raw materials into a stirrer, uniformly stirring, inputting the uniformly mixed materials into a screw extruder, and carrying out melt extrusion at the temperature of 115 ℃ to obtain the hot melt adhesive.
1. And (3) testing the instant metal adhesion force: step 1: taking a sample of 25.4 × 150mm, generally 1 Pcs; and 2, step: adhering transparent adhesive to PET surfaces at two ends of a sample, reserving a half, and adhering 2Pcs of a tinned wire and bare copper with specifications of 0.35mm multiplied by 0.30mm to the transparent adhesive in parallel with the trimming edge of the sample; and step 3: pressing at 170 deg.C at a speed of 1.5m/min and a pressure of 0.4mpa.s, and standing for 5 min; and 4, step 4: 2cm of metal wires are pulled open and placed on an upper chuck of a tensile machine, a sample film is placed on a lower chuck, and the span between the chucks of the tensile machine is set to be 20mm (the speed is 100 mm/min); and 5: the testing stroke is 50-70mm, the average force displayed by the tensile machine is recorded, the force is the metal bonding force (g/0.3mm) of the tested sample, and when the metal bonding force is more than or equal to 26g/0.3mm, the product reaches the qualified standard.
2. 85%, 145 ℃, 24 hour metal adhesion test: step 1: taking a sample of 25.4 × 150mm, generally 1 Pcs; step 2: adhering transparent adhesive to PET surfaces at two ends of a sample, reserving a half, and adhering 2Pcs of a tinned wire and bare copper with specifications of 0.35mm multiplied by 0.30mm to the transparent adhesive in parallel with the trimming edge of the sample; and step 3: pressing at 170 deg.C at speed of 1.5m/min and pressure of 0.4mpa.s, and placing in oven at 85% and 145 deg.C for 24 hr; and 4, step 4: 2cm of metal wires are pulled open and placed on an upper chuck of a tensile machine, a sample film is placed on a lower chuck, and the span between the chucks of the tensile machine is set to be 20mm (the speed is 100 mm/min); and 5: the testing stroke is 50-70mm, the average force displayed by the tensile machine is recorded, the force is the metal bonding force (g/0.3mm) of the tested sample, and when the metal bonding force is more than or equal to 30g/0.3mm, the product reaches the qualified standard.
3. Salt spray 96 hours metal adhesion test: putting the test sample into a salt spray machine (the salt water proportion is that 250g of salt is added into 5000ml of water) for 96 hours, wherein the conductor of the test sample must be completely exposed and cannot be laminated or shielded, after the salt spray is finished, measuring the value of the metal adhesion force by using an instant metal adhesion force test scheme, and when the metal adhesion force is more than or equal to 25g/0.3mm, the product reaches the qualified standard.
The results of the performance tests of examples 1-12 and comparative examples 1-4 are as follows:
TABLE 1
Figure BDA0003036349930000131
Figure BDA0003036349930000141
In summary, the following steps: the invention provides a high-viscosity weather-resistant hot melt adhesive and a preparation method thereof, wherein the ethylene-vinyl acetate copolymer is modified by modified titanium dioxide, so that the hot melt adhesive has good weather resistance on the basis of high viscosity, and is beneficial to long-term use; and the titanium dioxide is modified by polysiloxane and diethylamino hydroxybenzoyl hexyl benzoate, so that the thermal stability is further improved on the basis that the titanium dioxide has an excellent ultraviolet resistance function, and the weather resistance of the hot melt adhesive is further improved.
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 (8)

1. The high-viscosity weather-resistant hot melt adhesive is characterized by comprising the following components in parts by weight:
50-70 parts of ethylene-vinyl acetate copolymer, 6-8 parts of modified titanium dioxide, 0.2-0.4 part of antioxidant, 10-14 parts of tackifier, 0.6-0.8 part of coupling agent, 1.2-1.4 parts of flatting agent, 0.6-0.8 part of plasticizer and 3-7 parts of filler;
preparing modified titanium dioxide: firstly, crushing and grinding titanium dioxide, and then putting crushed titanium dioxide powder, polysiloxane and diethyl amino hydroxy benzoyl benzoic acid hexyl ester into a mixing tank, so that the total mass of the polysiloxane and the diethyl amino hydroxy benzoyl benzoic acid hexyl ester is 40-50% of the mass of the titanium dioxide powder, and the mass ratio of the polysiloxane to the diethyl amino hydroxy benzoyl benzoic acid hexyl ester is 1.3-1.5: 1, mixing and stirring at the temperature of 60-70 ℃, uniformly stirring, drying and crushing to obtain the modified titanium dioxide.
2. The high-viscosity weather-resistant hot melt adhesive as claimed in claim 1, which comprises the following components in parts by weight:
55-70 parts of ethylene-vinyl acetate copolymer, 6.5-8 parts of modified titanium dioxide, 0.25-0.4 part of antioxidant, 11-14 parts of tackifier, 0.65-0.8 part of coupling agent, 1.25-1.4 parts of flatting agent, 0.65-0.8 part of plasticizer and 4-7 parts of filler.
3. The high-viscosity weather-resistant hot melt adhesive as claimed in claim 2, which comprises the following components in parts by weight:
55-65 parts of ethylene-vinyl acetate copolymer, 6.5-7.5 parts of modified titanium dioxide, 0.25-0.35 part of antioxidant, 11-13 parts of tackifier, 0.65-0.75 part of coupling agent, 1.25-1.35 parts of flatting agent, 0.65-0.75 part of plasticizer and 4-6 parts of filler.
4. The high-viscosity weather-resistant hot melt adhesive as claimed in claim 1, wherein the antioxidant is a mixture of ascorbyl palmitate and tert-butyl hydroquinone, and the mass ratio of the ascorbyl palmitate to the tert-butyl hydroquinone is 0.8-1: 1.
5. the high-viscosity weather-resistant hot melt adhesive as claimed in claim 1, wherein the tackifier is one of phenolic resin, xylene formaldehyde resin or polyterpene resin.
6. The high-viscosity weather-resistant hot melt adhesive according to claim 1, wherein the plasticizer is one of dicyclohexyl phthalate, dibutyl phthalate or di-sec-octyl phthalate.
7. A high-viscosity weather-resistant hot melt adhesive as claimed in claim 1, wherein the filler is one of calcium carbonate, talc and silica.
8. The preparation method of the high-viscosity weather-resistant hot melt adhesive as claimed in any one of claims 1 to 7, which is characterized by comprising the following steps:
(1) weighing raw materials in parts by weight: the hot melt adhesive is prepared by the following steps of (1) inputting the weighed raw materials into a stirrer, uniformly stirring the raw materials, inputting the uniformly mixed materials into a screw extruder, and performing melt extrusion at the temperature of 110-120 ℃ to obtain the hot melt adhesive.
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