CN113881369B - Special high-temperature-resistant hot melt adhesive for automobile filter and preparation method thereof - Google Patents
Special high-temperature-resistant hot melt adhesive for automobile filter and preparation method thereof Download PDFInfo
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- CN113881369B CN113881369B CN202111259774.2A CN202111259774A CN113881369B CN 113881369 B CN113881369 B CN 113881369B CN 202111259774 A CN202111259774 A CN 202111259774A CN 113881369 B CN113881369 B CN 113881369B
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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
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- 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)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a special high-temperature-resistant hot melt adhesive for an automobile filter and a preparation method thereof, relating to the technical field of hot melt adhesives, and the key points of the technical scheme are as follows: the composition comprises the following components in parts by weight: 100 parts of base resin, 45-75 parts of tackifier, 9-25 parts of regulator, 0.1-1 part of antioxidant and 9-18 parts of filler; the base resin is an ethylene-vinyl acetate copolymer; the tackifier is a mixture of petroleum resin and ethylene isodecanoate cross-linked polymer; the regulator is microcrystalline wax. According to the invention, the water-soluble ethylene isodecanoate cross-linked polymer is mixed with the petroleum resin to be used as the tackifier, the double-ring structure of the ethylene isodecanoate cross-linked polymer can be well fused with the microcrystalline wax and the petroleum resin, the cracking and elution phenomena can be effectively reduced particularly in a high-temperature environment with certain humidity, and the ethylene isodecanoate cross-linked polymer has good heat resistance and water resistance.
Description
Technical Field
The invention relates to the technical field of hot melt adhesives, in particular to a special high-temperature-resistant hot melt adhesive for an automobile filter and a preparation method thereof.
Background
The hot melt adhesive is a plastic adhesive, is in a solid state at normal temperature, can be quickly bonded after being heated and melted, is mainly applied to the aspects of binding automobiles, furniture, textiles, books and periodicals and the like, and is commonly EVA (ethylene vinyl acetate) and TPR (thermal plastic rubber) hot melt adhesives.
The existing EVA hot melt adhesive is generally composed of base resin, tackifier, regulator and antioxidant, wherein the base resin can be ethylene-vinyl acetate copolymer, the tackifier can be rosin and derivatives thereof and petroleum resin, such as petroleum resin C5 and C9, and the regulator is generally microcrystalline wax or paraffin wax. However, the existing EVA hot melt adhesive is easy to crack and elute after washing, and especially in an environment with high temperature and certain humidity, such as an automobile filter, the natural crack and shedding phenomenon is obvious, which seriously affects the service life of the automobile filter.
Therefore, how to research and design a special high-temperature-resistant hot melt adhesive for an automobile filter and a preparation method thereof are problems which are urgently needed to be solved at present.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide the special high-temperature-resistant hot melt adhesive for the automobile filter and the preparation method thereof, which can effectively reduce the occurrence of cracks and elution phenomena in a high-temperature environment with certain humidity and have good heat resistance and water resistance; compared with the traditional preparation process, the whole preparation process does not need to be subjected to melting dehydration treatment, so that the required temperature condition is lower than the traditional preparation temperature, and no toxic gas or substance is generated in the whole preparation process.
The technical purpose of the invention is realized by the following technical scheme:
the first aspect provides a special high-temperature-resistant hot melt adhesive for an automobile filter, which comprises the following components in parts by weight: 100 parts of base resin, 45-75 parts of tackifier, 9-25 parts of regulator, 0.1-1 part of antioxidant and 9-18 parts of filler;
the base resin is an ethylene-vinyl acetate copolymer;
the tackifier is a mixture of petroleum resin and an ethylene isodecanoate cross-linked polymer;
the regulator is microcrystalline wax.
Preferably, the mixing mass ratio of the petroleum resin to the ethylene isodecanoate crosslinked polymer is 5-10: 1.
preferably, the mixing mass ratio of the petroleum resin to the ethylene isodecanoate crosslinked polymer is 5: 1.
preferably, the antioxidant is antioxidant 264 or antioxidant 1010.
Preferably, the filler is silica.
Preferably, the composition consists of the following components in parts by weight: 100 parts of base resin, 65 parts of tackifier, 25 parts of regulator, 1 part of antioxidant and 9 parts of filler.
In a second aspect, a preparation method of the special high-temperature-resistant hot melt adhesive for the automobile filter in the first aspect is provided, and the preparation method comprises the following steps:
s1: respectively heating the base resin, the tackifier, the regulator, the antioxidant and the filler to 120 ℃ for 100-;
s2: mixing the spare materials of the base resin, the tackifier, the regulator, the antioxidant and the filler prepared in the step S1, and stirring the mixture for 2 to 3 hours at the rotating speed of 400-600r/min at the temperature of between 85 and 95 ℃ until no obvious air bubbles, cracks or concave-convex parts exist on the surface of the mixture to obtain a mixture;
s3: dehydrating the mixture heated to the temperature of 130-;
s4: and melting and extruding the finished product material, and cooling, molding and cooling the extruded product to obtain the special high-temperature-resistant hot melt adhesive for the automobile filter.
Preferably, the cooling temperature of the extruded product before shaping is 80-100 ℃.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention provides a special high-temperature-resistant hot melt adhesive for an automobile filter, which is characterized in that a water-soluble ethylene isodecanoate cross-linked polymer and petroleum resin are mixed to serve as a tackifier, the double-ring structure of the ethylene isodecanoate cross-linked polymer can be well fused with microcrystalline wax and petroleum resin, the occurrence of cracks and elution can be effectively reduced especially in a high-temperature environment with certain humidity, and the high-temperature-resistant hot melt adhesive has good heat resistance and water resistance;
2. according to the preparation method of the special high-temperature-resistant hot melt adhesive for the automobile filter, provided by the invention, the raw materials are subjected to melting stirring, heating mixing stirring and heating dehydration stirring under a certain humidity condition, so that a finished product material with good cross-linking fusion of the raw materials can be obtained, and compared with the traditional preparation process, the whole preparation process does not need melting dehydration treatment, so that the required temperature condition is lower than the traditional preparation temperature, and no toxic gas or substance is generated in the whole preparation process.
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 below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
Examples
First, experimental design
The parts by weight of each component in each test example and comparative example are shown in table 1:
TABLE 1 parts by weight of the respective ingredients in the test examples and comparative examples
1. Test examples 1 to 4 and comparative example 1 were prepared by the following method:
s1: respectively heating the base resin, the tackifier, the regulator, the antioxidant and the filler to 120 ℃, stirring and mixing until the water content is kept below 5%, and then cooling to 80 ℃ to obtain the corresponding spare material.
S2: and (4) mixing the prepared basic resin, the tackifier, the regulator, the antioxidant and the filler in the step S1, and stirring at the rotating speed of 600r/min for 3 hours at the temperature of 95 ℃ until no obvious air bubbles, cracks or concave-convex parts exist on the surface, so as to obtain a mixture.
S3: and dehydrating the mixture heated to 150 ℃ for 1h at the rotating speed of 3500r/min in a vacuum environment to obtain a finished product.
S4: melting and extruding the finished product material, and cooling, molding and cooling the extruded product to obtain the special high-temperature-resistant hot melt adhesive for the automobile filter; the cooling temperature before the extruded product is molded is 100 ℃.
2. Comparative example 2 was prepared using the following method:
s101: heating a reaction kettle, weighing the wax and the antioxidant in the formula, adding the wax and the antioxidant into the reaction kettle, heating, controlling the temperature and continuously stirring until the wax is completely melted; the temperature is controlled to be 120-160 ℃, and the rotating speed is 60 r/min.
S201: vacuumizing the reaction kettle for protection, controlling the temperature in the reaction kettle to be 120 ℃, then adding the EVA resin, and continuing stirring until the EVA resin is completely melted.
S301: adding a tackifier and a filler into the reaction kettle, continuously heating, and stirring until the raw materials are completely melted; the heating temperature is 120-160 ℃, and the stirring speed is increased to 80 r/min.
S401: cooling, extruding and packaging to obtain the EVA hot melt adhesive.
Second, experimental verification
The finished hot melt adhesives prepared in the experimental examples 1-4 and the comparative examples 1-2 were washed with water at 40 ℃ and 40% humidity, at 100 ℃ and 70% humidity for 2 hours, respectively, and then the elution ratio and the crack ratio were counted.
When the elution ratio and the crack ratio are unified, the laser gridding treatment is carried out on the surface of the finished hot melt adhesive, and the size of a unit grid is 1mm multiplied by 1 mm; if the unit grids are washed and shed, the elution value of the corresponding unit grid is recorded as 1, otherwise, the elution value is 0; if the unit grid has a crack phenomenon, recording the crack value of the corresponding unit grid as 1, otherwise, recording the crack value as 0; and dividing the total elution value and the total crack value by the number of the unit grids to obtain the corresponding elution ratio and crack ratio.
The softening point is not reached yet at 40 ℃, so that the bonding fastness test is not carried out; and the adhesion fastness test was performed for each experimental example and comparative example under the conditions of 100 c and 70% humidity. The results of the elution ratio, crack ratio and adhesion fastness tests are shown in table 2.
TABLE 2 elution ratio, crack ratio and bond Strength test results
As can be seen from tables 1 and 2, in examples 1 to 3, the water-soluble ethylene isodecanoate crosspolymer was mixed with petroleum resin as a tackifier, and the elution ratio and the crack ratio were significantly reduced compared to those of the same petroleum resin and ethylene isodecanoate crosspolymer alone as a tackifier, particularly at higher temperatures and higher humidity. In addition, the elution rate and the crack rate of the EVA hot melt adhesive provided by the invention are obviously lower than those of the existing EVA hot melt adhesive. In addition, the EVA hot melt adhesive provided by the invention is obviously higher in bonding fastness than the EVA hot melt adhesive with the same share of petroleum resin and ethylene isodecanoate crosslinked polymer which are independently used as the tackifier, and is higher than the existing EVA hot melt adhesive.
The research process also carries out single adjustment on the ratio of each component, and the obtained contrast effect is less different from the effect. However, the mixing ratio of the petroleum resin and the ethylene isodecanoate cross-linked polymer has large influence difference, and the ratio with the best effect is 5: 1, when the ethylene isodecanoate cross-linked polymer accounts for a relatively large amount, the non-water-soluble performance of the hot melt adhesive can be influenced, and when the ethylene isodecanoate cross-linked polymer accounts for a relatively small amount, the water resistance and the bonding performance of the hot melt adhesive are not obviously reflected.
In conclusion, the water-soluble ethylene isodecanoate cross-linked polymer is mixed with the petroleum resin to be used as the tackifier, and a large number of experimental verifications and comparative analyses are carried out to research out a reasonable component proportion, so that the double-ring structure of the ethylene isodecanoate cross-linked polymer can be well fused with the microcrystalline wax and the petroleum resin, the cracking and elution phenomena can be effectively reduced particularly in a high-temperature environment with certain humidity, and the tackifier has good heat resistance and water resistance.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. The high-temperature-resistant hot melt adhesive special for the automobile filter is characterized by comprising the following components in parts by weight: 100 parts of base resin, 45-75 parts of tackifier, 9-25 parts of regulator, 0.1-1 part of antioxidant and 9-18 parts of filler;
the base resin is an ethylene-vinyl acetate copolymer;
the tackifier is a mixture of petroleum resin and an ethylene isodecanoate cross-linked polymer;
the regulator is microcrystalline wax;
the mixing mass ratio of the petroleum resin to the ethylene isodecanoate cross-linked polymer is 5: 1.
2. the high-temperature-resistant hot melt adhesive special for the automobile filter as claimed in claim 1, wherein the antioxidant is antioxidant 264 or antioxidant 1010.
3. The special high-temperature-resistant hot melt adhesive for the automobile filter as claimed in claim 1, wherein the filler is silicon dioxide.
4. The special high-temperature-resistant hot melt adhesive for the automobile filter as claimed in any one of claims 1 to 3, which is characterized by comprising the following components in parts by weight: 100 parts of base resin, 65 parts of tackifier, 25 parts of regulator, 1 part of antioxidant and 9 parts of filler.
5. The preparation method of the special high-temperature-resistant hot melt adhesive for the automobile filter as claimed in any one of claims 1 to 4, characterized by comprising the following steps:
s1: respectively heating the base resin, the tackifier, the regulator, the antioxidant and the filler to 120 ℃ for 100-;
s2: mixing the prepared basic resin, tackifier, regulator, antioxidant and filler at S1, and stirring at 85-95 deg.C at a rotation speed of 400-;
s3: dehydrating the mixture heated to the temperature of 130-;
s4: and melting and extruding the finished product material, and cooling, molding and cooling the extruded product to obtain the special high-temperature-resistant hot melt adhesive for the automobile filter.
6. The method as set forth in claim 5, wherein the cooling temperature of the extruded product before molding is 80 to 100 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111259774.2A CN113881369B (en) | 2021-10-28 | 2021-10-28 | Special high-temperature-resistant hot melt adhesive for automobile filter and preparation method thereof |
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| CN202111259774.2A CN113881369B (en) | 2021-10-28 | 2021-10-28 | Special high-temperature-resistant hot melt adhesive for automobile filter and preparation method thereof |
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| CN113881369A CN113881369A (en) | 2022-01-04 |
| CN113881369B true CN113881369B (en) | 2022-09-06 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10219215A (en) * | 1997-02-12 | 1998-08-18 | Sekisui Chem Co Ltd | Hot melt adhesive composition |
| CN102108269A (en) * | 2009-12-24 | 2011-06-29 | 上海理日化工新材料有限公司 | Ethylene-vinylacetate copolymer resin hot melt adhesive with high melting point, fast curing and low viscosity |
| CN111019559A (en) * | 2018-10-10 | 2020-04-17 | 上海灿盾实业有限公司 | EVA hot melt adhesive for rapid box sealing and preparation method thereof |
| CN111944456A (en) * | 2020-09-04 | 2020-11-17 | 上海路嘉胶粘剂有限公司 | EVA edge sealing hot melt adhesive without adhesive line and with low adhesive coating amount and preparation method thereof |
-
2021
- 2021-10-28 CN CN202111259774.2A patent/CN113881369B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10219215A (en) * | 1997-02-12 | 1998-08-18 | Sekisui Chem Co Ltd | Hot melt adhesive composition |
| CN102108269A (en) * | 2009-12-24 | 2011-06-29 | 上海理日化工新材料有限公司 | Ethylene-vinylacetate copolymer resin hot melt adhesive with high melting point, fast curing and low viscosity |
| CN111019559A (en) * | 2018-10-10 | 2020-04-17 | 上海灿盾实业有限公司 | EVA hot melt adhesive for rapid box sealing and preparation method thereof |
| CN111944456A (en) * | 2020-09-04 | 2020-11-17 | 上海路嘉胶粘剂有限公司 | EVA edge sealing hot melt adhesive without adhesive line and with low adhesive coating amount and preparation method thereof |
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| CN113881369A (en) | 2022-01-04 |
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