CN111057488A - Flame-retardant hot melt adhesive and preparation method thereof - Google Patents
Flame-retardant hot melt adhesive and preparation method thereof Download PDFInfo
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- CN111057488A CN111057488A CN201911423440.7A CN201911423440A CN111057488A CN 111057488 A CN111057488 A CN 111057488A CN 201911423440 A CN201911423440 A CN 201911423440A CN 111057488 A CN111057488 A CN 111057488A
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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
- 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
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- 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
- C09J145/00—Adhesives based on homopolymers or copolymers of compounds having no unsaturated aliphatic radicals in a side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic or in a heterocyclic system; Adhesives based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a flame-retardant hot melt adhesive which comprises the following components in percentage by weight: 25-35% of ethylene-vinyl acetate copolymer, 5-10% of polymerized terpene, 15-25% of hydrogenated aromatic modified alicyclic hydrocarbon resin, 19.5-25% of decabromodiphenylethane, 5-10% of zinc aluminate, 10-15% of Fischer-Tropsch wax and 0.3-0.5% of antioxidant. The invention also discloses a preparation method of the flame-retardant hot melt adhesive. The flame-retardant hot melt adhesive provided by the invention has good adhesive force on various electronic elements under the reasonable compounding action of the ethylene-vinyl acetate copolymer, the polymerized terpene, the hydrogenated aromatic modified alicyclic hydrocarbon resin, the decabromodiphenylethane, the zinc aluminate, the Fischer-Tropsch wax and the antioxidant, has good flame-retardant effect, can reach the UL94V-0 grade standard, can be applied to the assembly process of electronic and electric appliance parts, and can be produced in a large scale.
Description
Technical Field
The invention relates to the field of hot melt adhesives, in particular to a flame-retardant hot melt adhesive and a preparation method thereof.
Background
The hot melt adhesive is a plastic adhesive, the physical state of which changes along with the change of temperature within a certain temperature range, and the chemical property of which is unchanged, is nontoxic and tasteless, and belongs to an environment-friendly chemical product. The product is solid, so the product is convenient to package, transport and store, and has no solvent, pollution and toxicity; and the production process is simple, the added value is high, the bonding strength is high, the speed is high, and the like.
The general hot melt adhesive is prepared by melting and mixing raw materials such as high molecular polymer, rosin resin, petroleum resin, wax, antioxidant, filler and the like, wherein the components such as the high molecular polymer, the rosin resin, the petroleum resin, the wax and the like are all inflammable substances, so that the general hot melt adhesive has the common characteristics: is flammable. However, hot melt adhesives are used in various industries, and are extremely widely applied, and if the used hot melt adhesives are flammable, some potential safety hazards are inevitable, for example, electronic and electrical equipment often generates heat in the use process, and if flammable hot melt adhesives are used, the risk of fire is caused. Therefore, the hot melt adhesive with good flame retardant effect is urgently needed in some applications with higher fire protection requirements.
Disclosure of Invention
The flame-retardant hot melt adhesive and the preparation method thereof provided by the invention can be applied to the assembly process of electronic and electric parts and the like, have a good flame-retardant effect and can reach the UL94V-0 grade standard.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a flame-retardant hot melt adhesive, which comprises the following components in percentage by weight: 25-35% of ethylene-vinyl acetate copolymer, 5-10% of polymerized terpene, 15-25% of hydrogenated aromatic modified alicyclic hydrocarbon resin, 19.5-25% of decabromodiphenylethane, 5-10% of zinc aluminate, 10-15% of Fischer-Tropsch wax and 0.3-0.5% of antioxidant.
Furthermore, the melt index of the ethylene-vinyl acetate copolymer is 25-150 g/10min, wherein the vinyl acetate accounts for 28% of the mass of the ethylene-vinyl acetate copolymer.
Further, the polymeric terpene has a softening point of more than 100 ℃ and a weight average molecular weight of 1500-1800 g/mol.
Further, the hydrogenated aromatic-modified alicyclic hydrocarbon resin has a softening point of 100 ℃ and an aromaticity of 8 to 10% at 110 ℃.
Furthermore, the decabromodiphenylethane is white powder, the average particle size is less than or equal to 5 mu m, and the content of bromine is more than or equal to 81 percent.
Further, the fineness of the zinc aluminate is 1000-1250 mesh.
Further, the melting point of the Fischer-Tropsch wax is 110-118 ℃, and the melt viscosity of the Fischer-Tropsch wax is 9-16mPa.
The second aspect of the invention provides a preparation method of the flame-retardant hot melt adhesive, which comprises the following steps:
step 1, adding Fischer-Tropsch wax and an antioxidant under stirring, and melting the Fischer-Tropsch wax at 120-130 ℃;
step 2, after complete melting, putting the ethylene-vinyl acetate copolymer, the polymerized terpene and the hydrogenated aromatic modified alicyclic hydrocarbon resin into a stirring kettle in sequence for melting, setting the temperature of the stirring kettle to be 120-130 ℃ and the stirring speed to be 80-100 r/min;
step 3, sequentially putting the decabromodiphenylethane and the zinc aluminate into the stirring kettle, and continuously stirring for 30 minutes;
step 4, obtaining a mixture after uniformly stirring, vacuumizing the stirring kettle, setting the temperature of the stirring kettle to be 110 ℃, and stopping vacuumizing after the temperature in the stirring kettle is reduced to 110 ℃;
and 5, heating the granulation system to be turned on, preheating for 30 minutes, then enabling the mixture in the stirring kettle to enter the granulation system through a pipeline, and granulating and discharging.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
the flame-retardant hot melt adhesive provided by the invention has good adhesive force on various electronic elements under the reasonable compounding action of the ethylene-vinyl acetate copolymer, the polymerized terpene, the hydrogenated aromatic modified alicyclic hydrocarbon resin, the decabromodiphenylethane, the zinc aluminate, the Fischer-Tropsch wax and the antioxidant, has good flame-retardant effect, can reach the UL94V-0 grade standard, can be applied to the assembly process of electronic and electric appliance parts, and can be produced in a large scale.
Detailed Description
The invention provides a flame-retardant hot melt adhesive and a preparation method thereof.
The present invention will be described in detail and specifically with reference to the following examples to facilitate better understanding of the present invention, but the following examples do not limit the scope of the present invention.
Example one
The embodiment provides a preferable flame-retardant hot melt adhesive, which comprises the following components in percentage by weight:
example two
The embodiment provides a preferable flame-retardant hot melt adhesive, which comprises the following components in percentage by weight:
EXAMPLE III
The embodiment provides a preferable flame-retardant hot melt adhesive, which comprises the following components in percentage by weight:
example four
The embodiment provides a preparation method of the flame-retardant hot melt adhesive, which comprises the following steps:
step 1, adding Fischer-Tropsch wax and an antioxidant under stirring, and melting the Fischer-Tropsch wax at 120-130 ℃;
step 2, after complete melting, sequentially putting the ethylene-vinyl acetate copolymer, the polymerized terpene and the hydrogenated aromatic modified alicyclic hydrocarbon resin into a stirring kettle for melting, setting the temperature of the stirring kettle to be 100-120 ℃, and the stirring speed to be 80-100 r/min;
step 3, sequentially putting decabromodiphenylethane and zinc aluminate into a stirring kettle, and continuously stirring for 30 minutes;
step 4, obtaining a mixture after uniformly stirring, vacuumizing the stirring kettle, setting the temperature of the stirring kettle to be 110 ℃, and stopping vacuumizing after the temperature in the stirring kettle is reduced to 110 ℃;
and 5, heating the granulation system to be turned on, preheating for 30 minutes, then enabling the mixture in the stirring kettle to enter the granulation system through a pipeline, and granulating and discharging.
Verification examples
In this verification embodiment, the performance indexes of the flame-retardant hot melt adhesive provided in the first to third embodiments include viscosity, softening point, and flame-retardant test, and the following method is adopted:
1. viscosity of the oil
The melt viscosity of the hot-melt adhesive was determined by means of a Brookfield DV-2+ PRO type rotary viscometer, with a spindle of 27# and a rotational speed of 20 rpm, according to HG/T3660-1999 determination of the melt viscosity of the hot-melt adhesive.
2. Softening point
The softening point test method refers to GB/T15332-94 method for determining the softening point of hot melt adhesive by the ring and ball method.
3. Flame retardancy
Preparing a small strip sample: 127mm in length, 12.7mm in width and 3-13mm in thickness, 10 samples (2 sets) were prepared for each hot melt adhesive product, 5 samples were tested after being left at 23 ℃ for 48 hours at 50% RH, and 5 samples were tested after being left at 70 ℃ for 7 days.
In a non-ventilated test chamber, the specimen was held by a holder at a distance of 6.4mm from the upper end of the specimen, with the longitudinal axis of the specimen held vertical, with the lower end of the specimen at a distance of 9.5mm from the tip and 305mm from the surface of the dried absorbent cotton, the bunsen burner was ignited and adjusted to produce a blue flame 19mm high, the bunsen burner flame was placed at the lower end of the specimen, ignited for 10 seconds, then the flame was removed at a distance of at least 152mm from the specimen, and the flaming combustion time of the specimen was recorded. If the flame of the sample is extinguished within 30 seconds after the flame is removed, the bunsen burner must be moved to the lower part of the sample again, the sample is ignited for 10 seconds, then the flame of the bunsen burner is moved again, the flame-lasting time of the flaming combustion and flameless combustion of the sample is recorded, if the sample drops one grain, the sample is dropped on absorbent cotton 305mm below the sample, whether the absorbent cotton is ignited or not is judged, and the flame-retardant grade is judged according to the following standard.
UL94V-0 level requirements:
a No sample still had a flame burning for more than 10 seconds (flaming combustion time) after the test flame was removed.
B, for each set of 5 samples, after 10 times of ignition, the total time of combustion with the flame does not exceed 50 seconds
No sample was burned onto the fixture (including flaming and glowing)
D, without any sample, burning the melted liquid drops to drip and ignite the absorbent cotton below.
Without any sample, red-emitting combustion continued for more than 30 seconds (flameless combustion time) after the second removal of the test flame.
Table 1 test results of relevant indexes of flame retardant hot melt adhesive provided in examples one to three
As can be seen from Table 1, the products of examples 1-3 have good adhesive strength and flame retardant properties, and can reach the UL94V-0 rating standard.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (8)
1. The flame-retardant hot melt adhesive is characterized by comprising the following components in percentage by weight: 25-35% of ethylene-vinyl acetate copolymer, 5-10% of polymerized terpene, 15-25% of hydrogenated aromatic modified alicyclic hydrocarbon resin, 19.5-25% of decabromodiphenylethane, 5-10% of zinc aluminate, 10-15% of Fischer-Tropsch wax and 0.3-0.5% of antioxidant.
2. The flame-retardant hot melt adhesive according to claim 1, wherein the ethylene-vinyl acetate copolymer has a melt index of 25 to 150g/10min, and the mass of vinyl acetate in the ethylene-vinyl acetate copolymer is 28%.
3. The flame-retardant hot melt adhesive according to claim 1, wherein the polymerized terpene has a softening point of greater than 100 ℃ and a weight-average molecular weight of 1500-.
4. The flame-retardant hot melt adhesive according to claim 1, wherein the hydrogenated aromatic-modified alicyclic hydrocarbon resin has a softening point of 100 ℃ and an aromaticity of 8 to 10%.
5. The flame-retardant hot melt adhesive according to claim 1, wherein the decabromodiphenylethane is white powder with an average particle size of not more than 5 μm, and the bromine content of not less than 81%.
6. The flame-retardant hot melt adhesive according to claim 1, wherein the fineness of the zinc aluminate is 1000-1250 mesh.
7. The flame-retardant hot melt adhesive according to claim 1, wherein the melting point of the Fischer-Tropsch wax is 110 ℃ to 118 ℃, and the melt viscosity of the Fischer-Tropsch wax is 9 to 16mPa.s at 140 ℃.
8. The preparation method of the flame-retardant hot melt adhesive according to any one of claims 1 to 7, characterized by comprising the following steps:
step 1, adding Fischer-Tropsch wax and an antioxidant under stirring, and melting the Fischer-Tropsch wax at the temperature of 120-130 ℃;
step 2, after complete melting, putting the ethylene-vinyl acetate copolymer, the polymerized terpene and the hydrogenated aromatic modified alicyclic hydrocarbon resin into a stirring kettle in sequence for melting, setting the temperature of the stirring kettle to be 120-130 ℃ and the stirring speed to be 80-100 r/min;
step 3, sequentially putting the decabromodiphenylethane and the zinc aluminate into the stirring kettle, and continuously stirring for 30 minutes;
step 4, obtaining a mixture after uniformly stirring, vacuumizing the stirring kettle, setting the temperature of the stirring kettle to be 110 ℃, and stopping vacuumizing after the temperature in the stirring kettle is reduced to 110 ℃;
and 5, heating the granulation system to be turned on, preheating for 30 minutes, then enabling the mixture in the stirring kettle to enter the granulation system through a pipeline, and granulating and discharging.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911423440.7A CN111057488A (en) | 2019-12-31 | 2019-12-31 | Flame-retardant hot melt adhesive and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201911423440.7A CN111057488A (en) | 2019-12-31 | 2019-12-31 | Flame-retardant hot melt adhesive and preparation method thereof |
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| CN111057488A true CN111057488A (en) | 2020-04-24 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117304869A (en) * | 2023-11-29 | 2023-12-29 | 拓迪化学(上海)股份有限公司 | Flame-retardant transparent hot-melt pressure-sensitive adhesive and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104531007A (en) * | 2014-12-23 | 2015-04-22 | 安徽助成信息科技有限公司 | Flame-retardant EVA (ethylene-vinyl acetate) hot-melt adhesive |
| CN108130021A (en) * | 2017-12-22 | 2018-06-08 | 广州宝之泰电子科技有限公司 | A kind of co-extrusion type high fire-retardance hot melt adhesive and preparation method thereof |
| CN109943257A (en) * | 2019-03-28 | 2019-06-28 | 广州市隆创新材料有限公司 | Halogen-free flame-retardant hot-melt optical adhesive and preparation method thereof |
-
2019
- 2019-12-31 CN CN201911423440.7A patent/CN111057488A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104531007A (en) * | 2014-12-23 | 2015-04-22 | 安徽助成信息科技有限公司 | Flame-retardant EVA (ethylene-vinyl acetate) hot-melt adhesive |
| CN108130021A (en) * | 2017-12-22 | 2018-06-08 | 广州宝之泰电子科技有限公司 | A kind of co-extrusion type high fire-retardance hot melt adhesive and preparation method thereof |
| CN109943257A (en) * | 2019-03-28 | 2019-06-28 | 广州市隆创新材料有限公司 | Halogen-free flame-retardant hot-melt optical adhesive and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117304869A (en) * | 2023-11-29 | 2023-12-29 | 拓迪化学(上海)股份有限公司 | Flame-retardant transparent hot-melt pressure-sensitive adhesive and preparation method and application thereof |
| CN117304869B (en) * | 2023-11-29 | 2024-02-27 | 拓迪化学(上海)股份有限公司 | Flame-retardant transparent hot-melt pressure-sensitive adhesive and preparation method and application thereof |
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