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CN108034392B - High-bonding-strength and anti-aging bonding agent and preparation method and application thereof - Google Patents

High-bonding-strength and anti-aging bonding agent and preparation method and application thereof Download PDF

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CN108034392B
CN108034392B CN201810043211.1A CN201810043211A CN108034392B CN 108034392 B CN108034392 B CN 108034392B CN 201810043211 A CN201810043211 A CN 201810043211A CN 108034392 B CN108034392 B CN 108034392B
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CN108034392A (en
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Changying New Material Yantai Co ltd
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Yantai Longain Electron 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
    • C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
    • C09J151/08—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
    • C08F283/006—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00
    • C08F283/008—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polymers provided for in C08G18/00 on to unsaturated polymers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/30—Low-molecular-weight compounds
    • C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
    • C08G18/348—Hydroxycarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
    • C08G18/4236—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups
    • C08G18/4238—Polycondensates having carboxylic or carbonic ester groups in the main chain containing only aliphatic groups derived from dicarboxylic acids and dialcohols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6633—Compounds of group C08G18/42
    • C08G18/6659—Compounds of group C08G18/42 with compounds of group C08G18/34
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/67—Unsaturated compounds having active hydrogen
    • C08G18/671—Unsaturated compounds having only one group containing active hydrogen
    • C08G18/672—Esters of acrylic or alkyl acrylic acid having only one group containing active hydrogen

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Polyurethanes Or Polyureas (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses a high-bonding-strength and anti-aging bonding agent which is prepared from the following raw materials in parts by weight: 60-80 parts of polyethylene glycol adipate; 25-35 parts of dimethyl biphenyl diisocyanate; 14-18 parts of a modifier; 0.04-0.06 part of dibutyltin dilaurate; 6-8 parts of dimethylolpropionic acid; 3-4 parts of gamma-aminopropyltriethoxysilane; 1-3 parts of hydroxypropyl methacrylate; 130-150 parts of water; 6-10 parts of alkali; 15-25 parts of vinyl monomer; 0.2-0.4 part of water-soluble initiator; the modifier is a mixture of isopropyl titanate and mercaptoethanol, and the weight ratio of the isopropyl titanate to the mercaptoethanol is 6-8: 1; the alkali is sodium hydroxide or potassium hydroxide. The adhesive provided by the invention has high bonding strength, is resistant to thermal aging and light aging, is not yellow, and can be used for preparing a reflective material. The preparation method of the adhesive is simple and easy to implement.

Description

High-bonding-strength and anti-aging bonding agent and preparation method and application thereof
The application is a divisional application of patent with application number of 201610604518.5, application date of 2016, 07, 28 and invention named as "a high-bonding-strength and aging-resistant adhesive and a preparation method thereof".
Technical Field
The invention belongs to the field of reflective materials, and particularly relates to a high-bonding-strength and aging-resistant bonding agent and application thereof in a reflective material.
Background
The reflecting material is widely applied to various road traffic safety facilities such as traffic sign lines, raised road signs, contour signs, traffic cones, anti-collision barrels and the like, and automobile license plates, clothes, shoes and hats, fire fighting, railways, water transportation, mining areas and the like, and can be divided into the reflecting material of the traffic signs, the reflecting material of the road sign lines, the raised road signs, the contour signs, the reflecting material for clothes and the like.
The long-term exposure of the retroreflective material to sunlight, especially in the summer with high temperature, imposes high requirements on the thermal and photoaging resistance of the binder used in the retroreflective material.
Disclosure of Invention
The first purpose of the invention is to provide a high-bonding-strength and aging-resistant adhesive;
the second object of the present invention is to provide a method for producing the above binder;
the third purpose of the invention is to provide the application of the adhesive in the reflecting material.
The above object of the present invention is achieved by the following technical solutions:
the high-bonding-strength and anti-aging bonding agent is prepared from the following raw materials in parts by weight: 60-80 parts of polyethylene glycol adipate; 25-35 parts of dimethyl biphenyl diisocyanate; 14-18 parts of a modifier; 0.04-0.06 part of dibutyltin dilaurate; 6-8 parts of dimethylolpropionic acid; 3-4 parts of gamma-aminopropyltriethoxysilane; 1-3 parts of hydroxypropyl methacrylate; 130-150 parts of water; 6-10 parts of alkali; 15-25 parts of vinyl monomer; 0.2-0.4 part of water-soluble initiator; the modifier is a mixture of isopropyl titanate and mercaptoethanol, and the weight ratio of the isopropyl titanate to the mercaptoethanol is 6-8: 1; the alkali is sodium hydroxide or potassium hydroxide.
Further, the vinyl monomer is methyl acrylate, methyl methacrylate, ethyl acrylate or ethyl methacrylate.
Further, the water-soluble initiator is potassium persulfate or ammonium persulfate.
Further, the modifier is a mixture of isopropyl titanate and mercaptoethanol, and the weight ratio of the isopropyl titanate to the mercaptoethanol is 7: 1.
The preparation method of the adhesive comprises the following steps:
step S1, uniformly mixing polyethylene glycol adipate, dimethyl biphenyl diisocyanate, a modifier and dibutyltin dilaurate, and reacting at 75-85 ℃ for 2-3 hours; the modifier is a mixture of isopropyl titanate and mercaptoethanol;
step S2, adding dimethylolpropionic acid and gamma-aminopropyltriethoxysilane, stirring uniformly, reacting for 1-2 hours at 65-75 ℃, and then adding hydroxypropyl methacrylate for reacting for 0.5-1.5 hours;
step S3, cooling to 20-30 ℃, adding water and alkali, and shearing and emulsifying to obtain emulsion;
and step S4, adding a vinyl monomer into the emulsion, uniformly mixing, adding a water-soluble initiator, and carrying out polymerization reaction at 75-85 ℃ for 3-5 hours to obtain the high-bonding-strength and anti-aging binder.
Further, step S1 is specifically: polyethylene glycol adipate, dimethyl biphenyl diisocyanate, a modifier and dibutyltin dilaurate are uniformly mixed and reacted for 2.5 hours at the temperature of 80 ℃.
Further, step S2 is specifically: adding dimethylolpropionic acid and gamma-aminopropyl triethoxysilane, stirring, reacting at 70 deg.C for 1.5 hr, and adding hydroxypropyl methacrylate for reacting for 1 hr.
Further, step S3 is specifically: cooling to 25 deg.C, adding water and alkali, and shearing and emulsifying to obtain emulsion.
Further, step S4 is specifically: adding vinyl monomer into the emulsion, mixing uniformly, adding water-soluble initiator, and carrying out polymerization reaction for 4 hours at 80 ℃.
The application of the binder in the reflecting material.
The invention has the advantages that:
the adhesive provided by the invention has high bonding strength, is resistant to thermal aging and light aging, is not yellow, and can be used for preparing a reflective material. The preparation method of the adhesive is simple and easy to implement.
Detailed Description
The following examples are given to further illustrate the essence of the present invention, but should not be construed as limiting the scope of the present invention. Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention.
Example 1: preparation of the Binder
The weight parts of the raw materials are as follows:
70 parts of polyethylene glycol adipate; 30 parts of dimethyl biphenyl diisocyanate; 16 parts of a modifier; 0.05 part of dibutyltin dilaurate; 7 parts of dimethylolpropionic acid; 3.5 parts of gamma-aminopropyl triethoxysilane; 2 parts of hydroxypropyl methacrylate; 140 parts of water; 8 parts of alkali; 20 parts of vinyl monomer; 0.3 part of water-soluble initiator; the modifier is a mixture of isopropyl titanate and mercaptoethanol, and the weight ratio of the isopropyl titanate to the mercaptoethanol is 7: 1; the base is sodium hydroxide. The vinyl monomer is methyl acrylate. The water-soluble initiator is potassium persulfate.
The preparation method comprises the following steps:
step S1, uniformly mixing polyethylene glycol adipate, dimethyl biphenyl diisocyanate, a modifier and dibutyltin dilaurate, and reacting at 80 ℃ for 2.5 hours; the modifier is a mixture of isopropyl titanate and mercaptoethanol;
step S2, adding dimethylolpropionic acid and gamma-aminopropyltriethoxysilane, stirring uniformly, reacting at 70 ℃ for 1.5 hours, and then adding hydroxypropyl methacrylate for reacting for 1 hour;
step S3, cooling to 25 ℃, adding water and alkali, and shearing and emulsifying to obtain emulsion;
and step S4, adding vinyl monomers into the emulsion, uniformly mixing, adding a water-soluble initiator, and carrying out polymerization reaction for 4 hours at 80 ℃ to obtain the adhesive.
Example 2: preparation of the Binder
The weight parts of the raw materials are as follows:
60 parts of polyethylene glycol adipate; 25 parts of dimethyl biphenyl diisocyanate; 14 parts of a modifier; 0.04 part of dibutyltin dilaurate; 6 parts of dimethylolpropionic acid; 3 parts of gamma-aminopropyltriethoxysilane; 1 part of hydroxypropyl methacrylate; 130 parts of water; 6 parts of alkali; 15 parts of vinyl monomer; 0.2 part of water-soluble initiator; the modifier is a mixture of isopropyl titanate and mercaptoethanol, and the weight ratio of the isopropyl titanate to the mercaptoethanol is 6: 1; the base is sodium hydroxide. The vinyl monomer is methyl acrylate. The water-soluble initiator is potassium persulfate.
The preparation method comprises the following steps:
step S1, uniformly mixing polyethylene glycol adipate, dimethyl biphenyl diisocyanate, a modifier and dibutyltin dilaurate, and reacting at 80 ℃ for 2.5 hours; the modifier is a mixture of isopropyl titanate and mercaptoethanol;
step S2, adding dimethylolpropionic acid and gamma-aminopropyltriethoxysilane, stirring uniformly, reacting at 70 ℃ for 1.5 hours, and then adding hydroxypropyl methacrylate for reacting for 1 hour;
step S3, cooling to 25 ℃, adding water and alkali, and shearing and emulsifying to obtain emulsion;
and step S4, adding vinyl monomers into the emulsion, uniformly mixing, adding a water-soluble initiator, and carrying out polymerization reaction for 4 hours at 80 ℃ to obtain the adhesive.
Example 3: preparation of the Binder
The weight parts of the raw materials are as follows:
80 parts of polyethylene glycol adipate; 35 parts of dimethyl biphenyl diisocyanate; 18 parts of a modifier; 0.06 part of dibutyltin dilaurate; 8 parts of dimethylolpropionic acid; 4 parts of gamma-aminopropyltriethoxysilane; 3 parts of hydroxypropyl methacrylate; 150 parts of water; 10 parts of alkali; 25 parts of vinyl monomer; 0.4 part of water-soluble initiator; the modifier is a mixture of isopropyl titanate and mercaptoethanol, and the weight ratio of the isopropyl titanate to the mercaptoethanol is 8: 1; the base is sodium hydroxide. The vinyl monomer is methyl acrylate. The water-soluble initiator is potassium persulfate.
The preparation method comprises the following steps:
step S1, uniformly mixing polyethylene glycol adipate, dimethyl biphenyl diisocyanate, a modifier and dibutyltin dilaurate, and reacting at 80 ℃ for 2.5 hours; the modifier is a mixture of isopropyl titanate and mercaptoethanol;
step S2, adding dimethylolpropionic acid and gamma-aminopropyltriethoxysilane, stirring uniformly, reacting at 70 ℃ for 1.5 hours, and then adding hydroxypropyl methacrylate for reacting for 1 hour;
step S3, cooling to 25 ℃, adding water and alkali, and shearing and emulsifying to obtain emulsion;
and step S4, adding vinyl monomers into the emulsion, uniformly mixing, adding a water-soluble initiator, and carrying out polymerization reaction for 4 hours at 80 ℃ to obtain the adhesive.
Example 4: preparation of the Binder
The weight parts of the raw materials are as follows:
70 parts of polyethylene glycol adipate; 30 parts of dimethyl biphenyl diisocyanate; 16 parts of a modifier; 0.05 part of dibutyltin dilaurate; 7 parts of dimethylolpropionic acid; 3.5 parts of gamma-aminopropyl triethoxysilane; 2 parts of hydroxypropyl methacrylate; 140 parts of water; 8 parts of alkali; 20 parts of vinyl monomer; 0.3 part of water-soluble initiator; the modifier is a mixture of isopropyl titanate and mercaptoethanol, and the weight ratio of the isopropyl titanate to the mercaptoethanol is 6: 1; the base is sodium hydroxide. The vinyl monomer is methyl acrylate. The water-soluble initiator is potassium persulfate.
The preparation method comprises the following steps:
step S1, uniformly mixing polyethylene glycol adipate, dimethyl biphenyl diisocyanate, a modifier and dibutyltin dilaurate, and reacting at 80 ℃ for 2.5 hours; the modifier is a mixture of isopropyl titanate and mercaptoethanol;
step S2, adding dimethylolpropionic acid and gamma-aminopropyltriethoxysilane, stirring uniformly, reacting at 70 ℃ for 1.5 hours, and then adding hydroxypropyl methacrylate for reacting for 1 hour;
step S3, cooling to 25 ℃, adding water and alkali, and shearing and emulsifying to obtain emulsion;
and step S4, adding vinyl monomers into the emulsion, uniformly mixing, adding a water-soluble initiator, and carrying out polymerization reaction for 4 hours at 80 ℃ to obtain the adhesive.
Example 5: preparation of the Binder
The weight parts of the raw materials are as follows:
70 parts of polyethylene glycol adipate; 30 parts of dimethyl biphenyl diisocyanate; 16 parts of a modifier; 0.05 part of dibutyltin dilaurate; 7 parts of dimethylolpropionic acid; 3.5 parts of gamma-aminopropyl triethoxysilane; 2 parts of hydroxypropyl methacrylate; 140 parts of water; 8 parts of alkali; 20 parts of vinyl monomer; 0.3 part of water-soluble initiator; the modifier is a mixture of isopropyl titanate and mercaptoethanol, and the weight ratio of the isopropyl titanate to the mercaptoethanol is 8: 1; the base is sodium hydroxide. The vinyl monomer is methyl acrylate. The water-soluble initiator is potassium persulfate.
The preparation method comprises the following steps:
step S1, uniformly mixing polyethylene glycol adipate, dimethyl biphenyl diisocyanate, a modifier and dibutyltin dilaurate, and reacting at 80 ℃ for 2.5 hours; the modifier is a mixture of isopropyl titanate and mercaptoethanol;
step S2, adding dimethylolpropionic acid and gamma-aminopropyltriethoxysilane, stirring uniformly, reacting at 70 ℃ for 1.5 hours, and then adding hydroxypropyl methacrylate for reacting for 1 hour;
step S3, cooling to 25 ℃, adding water and alkali, and shearing and emulsifying to obtain emulsion;
and step S4, adding vinyl monomers into the emulsion, uniformly mixing, adding a water-soluble initiator, and carrying out polymerization reaction for 4 hours at 80 ℃ to obtain the adhesive.
Example 6: comparative examples
The weight parts of the raw materials are as follows:
70 parts of polyethylene glycol adipate; 30 parts of dimethyl biphenyl diisocyanate; 16 parts of a modifier; 0.05 part of dibutyltin dilaurate; 7 parts of dimethylolpropionic acid; 3.5 parts of gamma-aminopropyl triethoxysilane; 2 parts of hydroxypropyl methacrylate; 140 parts of water; 8 parts of alkali; 20 parts of vinyl monomer; 0.3 part of water-soluble initiator; the modifier is a mixture of isopropyl titanate and mercaptoethanol, and the weight ratio of the isopropyl titanate to the mercaptoethanol is 5: 1; the base is sodium hydroxide. The vinyl monomer is methyl acrylate. The water-soluble initiator is potassium persulfate.
The preparation method comprises the following steps:
step S1, uniformly mixing polyethylene glycol adipate, dimethyl biphenyl diisocyanate, a modifier and dibutyltin dilaurate, and reacting at 80 ℃ for 2.5 hours; the modifier is a mixture of isopropyl titanate and mercaptoethanol;
step S2, adding dimethylolpropionic acid and gamma-aminopropyltriethoxysilane, stirring uniformly, reacting at 70 ℃ for 1.5 hours, and then adding hydroxypropyl methacrylate for reacting for 1 hour;
step S3, cooling to 25 ℃, adding water and alkali, and shearing and emulsifying to obtain emulsion;
and step S4, adding vinyl monomers into the emulsion, uniformly mixing, adding a water-soluble initiator, and carrying out polymerization reaction for 4 hours at 80 ℃ to obtain the adhesive.
Example 7: comparative examples
The weight parts of the raw materials are as follows:
70 parts of polyethylene glycol adipate; 30 parts of dimethyl biphenyl diisocyanate; 16 parts of a modifier; 0.05 part of dibutyltin dilaurate; 7 parts of dimethylolpropionic acid; 3.5 parts of gamma-aminopropyl triethoxysilane; 2 parts of hydroxypropyl methacrylate; 140 parts of water; 8 parts of alkali; 20 parts of vinyl monomer; 0.3 part of water-soluble initiator; the modifier is a mixture of isopropyl titanate and mercaptoethanol, and the weight ratio of the isopropyl titanate to the mercaptoethanol is 9: 1; the base is sodium hydroxide. The vinyl monomer is methyl acrylate. The water-soluble initiator is potassium persulfate.
The preparation method comprises the following steps:
step S1, uniformly mixing polyethylene glycol adipate, dimethyl biphenyl diisocyanate, a modifier and dibutyltin dilaurate, and reacting at 80 ℃ for 2.5 hours; the modifier is a mixture of isopropyl titanate and mercaptoethanol;
step S2, adding dimethylolpropionic acid and gamma-aminopropyltriethoxysilane, stirring uniformly, reacting at 70 ℃ for 1.5 hours, and then adding hydroxypropyl methacrylate for reacting for 1 hour;
step S3, cooling to 25 ℃, adding water and alkali, and shearing and emulsifying to obtain emulsion;
and step S4, adding vinyl monomers into the emulsion, uniformly mixing, adding a water-soluble initiator, and carrying out polymerization reaction for 4 hours at 80 ℃ to obtain the adhesive.
Example 8: effects of the embodiment
The performance of the binders prepared in examples 1 to 7 were tested separately, and the test methods were as follows.
And (3) aging resistance testing: under ultraviolet irradiation and at the temperature of 70 ℃ for 1000 hours, testing the tensile strength and the yellowing resistance grade, and measuring the thermal aging resistance by using the tensile strength; the light aging resistance is measured by a yellowing resistance grade, and an SFJJ-2000C type standard light source box (Shanghai Lin New electronics Co., Ltd.) is used for testing the yellowing resistance grade.
Tensile strength: implementing the GB/T528-1998 standard; an LJ-5000N tensile machine (Chengde tester factory) with the test conditions of room temperature 25 deg.C, air humidity 55% and loading speed of 100 mm/min.
Peel strength: executing GB/T2791-1995 standard, adopting PET material to make bonding, testing 24-hour final bonding strength, and making material width be 2.5 cm; the test conditions of the tensile machine are that the room temperature is 25 ℃, the air humidity is 55 percent, and the loading speed of the tensile machine is 100 mm/min; LJ-5000N tensile machine (Chengde tester).
The test results are given in the following table:
grade of resistance to yellowing Peel strength/(N/2.5 cm) Tensile strength (70 ℃, 1000h)/MPa
Example 1 4.8 68 28
Example 2 4.5 63 25
Example 3 4.6 65 26
Example 4 4.5 64 25
Example 5 4.6 65 26
Example 6 2.8 55 18
Example 7 2.9 56 19
The results show that the adhesive provided by the invention has high bonding strength, heat aging resistance, light aging resistance and no yellowing, and can be used for preparing a reflective material. The preparation method of the adhesive is simple and easy to implement. In addition, potassium hydroxide may also be used as the base in the examples; the vinyl monomer may also be methyl methacrylate, ethyl acrylate or ethyl methacrylate; ammonium persulfate may also be used as the water-soluble initiator. The above-described embodiments are intended to illustrate the substance of the present invention, but are not intended to limit the scope of the present invention. It will be understood by those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof without departing from the true spirit and scope of the invention.

Claims (9)

1.一种高粘结强度、耐老化的粘结剂，其特征在于，通过如下重量份的原料制备而成：聚己二酸乙二醇酯，60～80份；二甲基联苯二异氰酸酯，25～35份；改性剂，14～18份；二月桂酸二丁基锡，0.04～0.06份；二羟甲基丙酸，6～8份；γ-氨基丙基三乙氧基硅烷，3～4份；甲基丙烯酸羟丙酯，1～3份；水，130～150份；碱，6～10份；乙烯基单体，15～25份；水溶性引发剂，0.2～0.4份；所述改性剂为钛酸异丙酯和巯基乙醇的混合物，二者重量份之比为6～8:1。1. a high bonding strength, anti-aging binder, is characterized in that, is prepared from the raw material of following parts by weight: polyethylene adipate, 60～80 parts; dimethyl biphenyl diphenyl Isocyanate, 25-35 parts; Modifier, 14-18 parts; Dibutyltin dilaurate, 0.04-0.06 parts; Dimethylolpropionic acid, 6-8 parts; γ-Aminopropyltriethoxysilane, 3-4 parts; hydroxypropyl methacrylate, 1-3 parts; water, 130-150 parts; alkali, 6-10 parts; vinyl monomer, 15-25 parts; water-soluble initiator, 0.2-0.4 parts The modifier is a mixture of isopropyl titanate and mercaptoethanol, and the ratio of the two parts by weight is 6-8:1. 2.根据权利要求1所述的高粘结强度、耐老化的粘结剂，其特征在于：所述乙烯基单体为丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯或甲基丙烯酸乙酯。2. The high bonding strength, aging-resistant adhesive of claim 1, wherein the vinyl monomer is methyl acrylate, methyl methacrylate, ethyl acrylate or ethyl methacrylate ester. 3.根据权利要求1所述的高粘结强度、耐老化的粘结剂，其特征在于：所述水溶性引发剂为过硫酸钾或过硫酸铵；所述碱为氢氧化钠或氢氧化钾。3. The high bonding strength, aging-resistant binder according to claim 1, wherein the water-soluble initiator is potassium persulfate or ammonium persulfate; the alkali is sodium hydroxide or hydroxide Potassium. 4.权利要求1～3任一所述粘结剂的制备方法，其特征在于，包括如下步骤：4. the preparation method of any described binder of claim 1～3, is characterized in that, comprises the steps: 步骤S1，将聚己二酸乙二醇酯、二甲基联苯二异氰酸酯、改性剂和二月桂酸二丁基锡混合均匀，加热反应；Step S1, mixing polyethylene adipate, dimethylbiphenyl diisocyanate, modifier and dibutyltin dilaurate uniformly, and heating for reaction; 步骤S2，加入二羟甲基丙酸、γ-氨基丙基三乙氧基硅烷搅拌均匀，加热反应，然后再加入甲基丙烯酸羟丙酯继续反应；Step S2, adding dimethylolpropionic acid and γ-aminopropyl triethoxysilane, stirring evenly, heating for reaction, and then adding hydroxypropyl methacrylate to continue the reaction; 步骤S3，温度降至20～30℃后，再加入水和碱，剪切乳化得乳液；In step S3, after the temperature is lowered to 20-30°C, water and alkali are added, and an emulsion is obtained by shearing and emulsification; 步骤S4，向乳液中添加乙烯基单体，混合均匀后再添加水溶性引发剂，聚合反应后即得所述高粘结强度、耐老化的粘结剂。In step S4, vinyl monomers are added to the emulsion, and the water-soluble initiator is added after mixing evenly. 5.根据权利要求4所述的制备方法，其特征在于，步骤S1中加热反应条件为75～85℃下反应2～3小时。5 . The preparation method according to claim 4 , wherein the heating reaction condition in step S1 is 75-85° C. for 2-3 hours. 6 . 6.根据权利要求4所述的制备方法，其特征在于，步骤S2具体为：加入二羟甲基丙酸、γ-氨基丙基三乙氧基硅烷搅拌均匀，65～75℃反应1～2小时，再加入甲基丙烯酸羟丙酯反应0.5～1.5小时。6 . The preparation method according to claim 4 , wherein step S2 is specifically: adding dimethylolpropionic acid and γ-aminopropyltriethoxysilane, stirring evenly, and reacting at 65-75° C. for 1-2 hours, then add hydroxypropyl methacrylate to react for 0.5-1.5 hours. 7.根据权利要求4所述的制备方法，其特征在于，步骤S3具体为：温度降至25℃后，再加入水和碱，剪切乳化得乳液。7 . The preparation method according to claim 4 , wherein step S3 is specifically as follows: after the temperature is lowered to 25° C., water and alkali are added, and an emulsion is obtained by shearing and emulsification. 8 . 8.根据权利要求4所述的制备方法，其特征在于，步骤S4具体为：向乳液中添加乙烯基单体，混合均匀后再添加水溶性引发剂，75～85℃下聚合反应3～5小时即得。8 . The preparation method according to claim 4 , wherein step S4 is specifically as follows: adding vinyl monomers to the emulsion, adding a water-soluble initiator after mixing evenly, and performing a polymerization reaction for 3 to 5 at 75 to 85° C. 9 . Get it in hours. 9.如权利要求1～3任一项所述的粘结剂在反光材料中的应用。9. The application of the binder according to any one of claims 1 to 3 in reflective materials.
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