CN109439240A - A kind of preparation method of heat resistant type PP hot melt adhesive - Google Patents
A kind of preparation method of heat resistant type PP hot melt adhesive Download PDFInfo
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- CN109439240A CN109439240A CN201811370216.1A CN201811370216A CN109439240A CN 109439240 A CN109439240 A CN 109439240A CN 201811370216 A CN201811370216 A CN 201811370216A CN 109439240 A CN109439240 A CN 109439240A
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- resistant type
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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
- C09J151/06—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 homopolymers or copolymers of aliphatic hydrocarbons containing only one carbon-to-carbon double bond
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention provides a kind of preparation methods of heat resistant type PP hot melt adhesive, comprising the following steps: S1. prepares graft polypropylene；S2. amino-acid modified graft polypropylene is prepared；S3. by ethyl orthosilicate and methacrylic acid-β-hydroxypropyl acrylate, fully reacting, then deionized water is added, hydrochloric acid and ethyl alcohol are hydrolyzed, and benzoyl peroxide then is added by nitrogen, methyl methacrylate and ethyl acetate, it is condensed back reaction, hybrid collosol is obtained, is being aged, drying, obtains hybrid composite material；S4. after the obtained amino-acid modified graft polypropylene of step S2 and antioxidant being mixed, it is added in mixer and mixes, then the hybrid composite material of terpene phenolic resin and step S3 preparation is added, it is heated to after terpene phenolic resin resin melts completely, it is added, polyethylene wax and naphthenic oil, after mixing discharge, packaging, obtains heat resistant type polyolefin hot-melt.The Good Heat-resistance for the hot melt adhesive that the present invention is prepared.
Description
Technical field
The present invention relates to polyolefin hot-melt fields, and in particular to a kind of preparation method of heat resistant type PP hot melt adhesive.
Background technique
Polypropylene (PP) has nonpolarity, viscosity low (can mix people's high amount of inorganic filler), stability and water resistance preferably (full
And high molecular material), many advantages, such as color is shallow transparent, cheap, prepare hot melt adhesive, coating and composite material for building
Very good material.But since PP is nonpolar molecule, relative molecular mass is smaller, structure is irregular and cohesive force is lower, leads
Cause its hydrophily, antistatic property, mechanical property and heat resistance poor, application range is restricted, will by graft-modification method
On polar monomer graft to the strand of polymer, increase its reactivity, functionality and polarity, is macromolecule material in recent years
One of the hot research problem in material field.Maleic anhydride inoculated polypropylene can significantly improve the polarity and reactivity using branch
Improve the performance of PP, but maleic anhydride inoculated polypropylene is in twin-screw extrusion production process, used grafted monomers
Maleic anhydride has stronger acidity, easily corrodes board, and have stronger irritation to human body.
Summary of the invention
Technical problems to be solved: the object of the present invention is to provide a kind of preparation method of heat resistant type PP hot melt adhesive, preparations
The Good Heat-resistance of obtained hot melt adhesive.
A kind of technical solution: preparation method of heat resistant type PP hot melt adhesive, comprising the following steps:
S1. by polypropylene, glycidyl methacrylate, styrene and cumyl peroxide 100-150:1- in mass ratio
2:3-6:0.15-0.25 adding twin-screw extrude after mixing, reactive extrursion, pelletizing, drying, purification are grafted
Polypropylene；
S2. by 1,6-aminocaprolc acid and graft polypropylene are added twin-screw extrude in the ratio of 1:100, and reactive extrursion is cut
Grain, is dried to obtain amino-acid modified graft polypropylene；
S3. by ethyl orthosilicate and methacrylic acid-β-hydroxypropyl acrylate, then deionized water, hydrochloric acid and ethyl alcohol is added in fully reacting
It is hydrolyzed, the pH for controlling solution is 3-4, and benzoyl peroxide, methyl methacrylate and acetic acid then is added by nitrogen
Ethyl ester is condensed back reaction, obtains hybrid collosol, be aged, and dries, obtains hybrid composite material；
S4. it after mixing the obtained amino-acid modified graft polypropylene of step S2 and antioxidant, is added in mixer and mixes, so
The hybrid composite material of terpene phenolic resin and step S3 preparation is added afterwards, is heated to terpene phenolic resin resin and melts completely
Afterwards, it is added, polyethylene wax and naphthenic oil, after mixing discharge, packaging obtains heat resistant type polyolefin hot-melt.
Further, extrusion reaction temperature is 180-190 DEG C in the step S1, and screw speed takes 200-350r/min, is squeezed out
Time is 60-180s；
Further, in the step S2 wherein each barrel temperature of double screw extruder be respectively 160,180,200,200,190,
180℃。
Further, ethyl orthosilicate and methacrylic acid-β-hydroxypropyl acrylate react 60- at 50-60 DEG C in the step S3
150min.Further, ethyl orthosilicate in the step S3, methacrylic acid-β-hydroxypropyl acrylate and methyl methacrylate
Molar ratio is 1:1:1.
Further, amino-acid modified graft polypropylene in the step S3, hybrid composite material, antioxidant, terpenes phenolic aldehyde
Resin, polyethylene wax, the mass ratio of naphthenic oil are 100-150:25-40:2-4:20-30:1-5:5-10.
The utility model has the advantages that of the invention has the advantage that first through inorganic SiO2The addition of component substantially increases hot melt adhesive
Heat resistance, while also improving energy required when strand is broken in thermal histories in hot melt adhesive；Grafted monomers into
After row grafting modification, grafting molecules chain has longer length, therefore is provided with higher mechanical property, while epoxy is opened
The chemical bond that ring is formed compares the chemical bond more hydrolysis that acid anhydrides open loop is formed, therefore is broken after also obtaining higher aging
Elongation retention rate.
Specific embodiment
Embodiment 1
A kind of preparation method of heat resistant type PP hot melt adhesive, comprising the following steps:
S1. by polypropylene, glycidyl methacrylate, styrene and cumyl peroxide 100:1:6 in mass ratio:
0.15 adds twin-screw extrude after mixing, reactive extrursion, pelletizing, drying, purification, and extrusion reaction temperature is 180 DEG C,
Screw speed takes 200r/min, finds time as 180s, obtains graft polypropylene；
S2. by 1,6-aminocaprolc acid and graft polypropylene are added twin-screw extrude in the ratio of 1:100, and reactive extrursion is cut
Grain, each barrel temperature of double screw extruder is respectively 160,180,200,200,190,180 DEG C, is dried to obtain amino-acid modified connect
Branch polypropylene；
S3. by ethyl orthosilicate and methacrylic acid-β-hydroxypropyl acrylate, 60min is reacted at 50 DEG C, deionized water is then added,
Hydrochloric acid and ethyl alcohol are hydrolyzed, and the pH for controlling solution is 3, and benzoyl peroxide, methyl methacrylate then is added by nitrogen
Ester and ethyl acetate, condensing reflux reaction, ethyl orthosilicate, methacrylic acid-β-hydroxypropyl acrylate and methyl methacrylate rub
You obtain hybrid collosol, are being aged, dry, obtain hybrid composite material than being 1:1:1；
S4. it after mixing the obtained amino-acid modified graft polypropylene of step S2 and antioxidant, is added in mixer and mixes, so
The hybrid composite material of terpene phenolic resin and step S3 preparation is added afterwards, is heated to terpene phenolic resin resin and melts completely
Afterwards, it is added, polyethylene wax and naphthenic oil, after mixing discharge, amino-acid modified graft polypropylene, hybrid composite material resists
Oxidant, terpene phenolic resin, polyethylene wax, the mass ratio of naphthenic oil are 100:25:4:30:1:5, and packaging obtains heat resistant type
Polyolefin hot-melt.
Embodiment 2
A kind of preparation method of heat resistant type PP hot melt adhesive, comprising the following steps:
S1. by polypropylene, glycidyl methacrylate, styrene and cumyl peroxide 150:2:3 in mass ratio:
0.25 adds twin-screw extrude after mixing, reactive extrursion, pelletizing, drying, purification, and extrusion reaction temperature is 190 DEG C,
Screw speed takes 350r/min, finds time as 60s, obtains graft polypropylene；
S2. by 1,6-aminocaprolc acid and graft polypropylene are added twin-screw extrude in the ratio of 1:100, and reactive extrursion is cut
Grain, each barrel temperature of double screw extruder is respectively 160,180,200,200,190,180 DEG C, is dried to obtain amino-acid modified connect
Branch polypropylene；
S3. by ethyl orthosilicate and methacrylic acid-β-hydroxypropyl acrylate, 150min is reacted at 60 DEG C, deionized water is then added,
Hydrochloric acid and ethyl alcohol are hydrolyzed, and the pH for controlling solution is 4, and benzoyl peroxide, methyl methacrylate then is added by nitrogen
Ester and ethyl acetate, condensing reflux reaction, ethyl orthosilicate, methacrylic acid-β-hydroxypropyl acrylate and methyl methacrylate rub
You obtain hybrid collosol, are being aged, dry, obtain hybrid composite material than being 1:1:1；
S4. it after mixing the obtained amino-acid modified graft polypropylene of step S2 and antioxidant, is added in mixer and mixes, so
The hybrid composite material of terpene phenolic resin and step S3 preparation is added afterwards, is heated to terpene phenolic resin resin and melts completely
Afterwards, it is added, polyethylene wax and naphthenic oil, after mixing discharge, amino-acid modified graft polypropylene, hybrid composite material resists
Oxidant, terpene phenolic resin, polyethylene wax, the mass ratio of naphthenic oil are 150:40:2:20:5:10, and packaging obtains heat resistant type
Polyolefin hot-melt.
Embodiment 3
A kind of preparation method of heat resistant type PP hot melt adhesive, comprising the following steps:
S1. by polypropylene, glycidyl methacrylate, styrene and cumyl peroxide 120:1:5 in mass ratio:
0.18 adds twin-screw extrude after mixing, reactive extrursion, pelletizing, drying, purification, and extrusion reaction temperature is 180 DEG C,
Screw speed takes 240r/min, finds time as 90s, obtains graft polypropylene；
S2. by 1,6-aminocaprolc acid and graft polypropylene are added twin-screw extrude in the ratio of 1:100, and reactive extrursion is cut
Grain, each barrel temperature of double screw extruder is respectively 160,180,200,200,190,180 DEG C, is dried to obtain amino-acid modified connect
Branch polypropylene；
S3. by ethyl orthosilicate and methacrylic acid-β-hydroxypropyl acrylate, 90min is reacted at 50 DEG C, deionized water is then added,
Hydrochloric acid and ethyl alcohol are hydrolyzed, and the pH for controlling solution is 3, and benzoyl peroxide, methyl methacrylate then is added by nitrogen
Ester and ethyl acetate, condensing reflux reaction, ethyl orthosilicate, methacrylic acid-β-hydroxypropyl acrylate and methyl methacrylate rub
You obtain hybrid collosol, are being aged, dry, obtain hybrid composite material than being 1:1:1；
S4. it after mixing the obtained amino-acid modified graft polypropylene of step S2 and antioxidant, is added in mixer and mixes, so
The hybrid composite material of terpene phenolic resin and step S3 preparation is added afterwards, is heated to terpene phenolic resin resin and melts completely
Afterwards, it is added, polyethylene wax and naphthenic oil, after mixing discharge, amino-acid modified graft polypropylene, hybrid composite material resists
Oxidant, terpene phenolic resin, polyethylene wax, the mass ratio of naphthenic oil are 120:28:4:28:4:6, and packaging obtains heat resistant type
Polyolefin hot-melt.
Embodiment 4
A kind of preparation method of heat resistant type PP hot melt adhesive, comprising the following steps:
S1. by polypropylene, glycidyl methacrylate, styrene and cumyl peroxide 140:2:4 in mass ratio:
0.22 adds twin-screw extrude after mixing, reactive extrursion, pelletizing, drying, purification, and extrusion reaction temperature is 190 DEG C,
Screw speed takes 320r/min, finds time as 120s, obtains graft polypropylene；
S2. by 1,6-aminocaprolc acid and graft polypropylene are added twin-screw extrude in the ratio of 1:100, and reactive extrursion is cut
Grain, each barrel temperature of double screw extruder is respectively 160,180,200,200,190,180 DEG C, is dried to obtain amino-acid modified connect
Branch polypropylene；
S3. by ethyl orthosilicate and methacrylic acid-β-hydroxypropyl acrylate, 120min is reacted at 60 DEG C, deionized water is then added,
Hydrochloric acid and ethyl alcohol are hydrolyzed, and the pH for controlling solution is 4, and benzoyl peroxide, methyl methacrylate then is added by nitrogen
Ester and ethyl acetate, condensing reflux reaction, ethyl orthosilicate, methacrylic acid-β-hydroxypropyl acrylate and methyl methacrylate rub
You obtain hybrid collosol, are being aged, dry, obtain hybrid composite material than being 1:1:1；
S4. it after mixing the obtained amino-acid modified graft polypropylene of step S2 and antioxidant, is added in mixer and mixes, so
The hybrid composite material of terpene phenolic resin and step S3 preparation is added afterwards, is heated to terpene phenolic resin resin and melts completely
Afterwards, it is added, polyethylene wax and naphthenic oil, after mixing discharge, amino-acid modified graft polypropylene, hybrid composite material resists
Oxidant, terpene phenolic resin, polyethylene wax, the mass ratio of naphthenic oil are 140:35:2:22:24:9, and packaging obtains heat resistant type
Polyolefin hot-melt.
Embodiment 5
A kind of preparation method of heat resistant type PP hot melt adhesive, comprising the following steps:
S1. by polypropylene, glycidyl methacrylate, styrene and cumyl peroxide 130:1:4 in mass ratio:
0.2 adds twin-screw extrude after mixing, reactive extrursion, pelletizing, drying, purification, and extrusion reaction temperature is 180 DEG C,
Screw speed takes 280r/min, finds time as 100s, obtains graft polypropylene；
S2. by 1,6-aminocaprolc acid and graft polypropylene are added twin-screw extrude in the ratio of 1:100, and reactive extrursion is cut
Grain, each barrel temperature of double screw extruder is respectively 160,180,200,200,190,180 DEG C, is dried to obtain amino-acid modified connect
Branch polypropylene；
S3. by ethyl orthosilicate and methacrylic acid-β-hydroxypropyl acrylate, 100min is reacted at 60 DEG C, deionized water is then added,
Hydrochloric acid and ethyl alcohol are hydrolyzed, and the pH for controlling solution is 3, and benzoyl peroxide, methyl methacrylate then is added by nitrogen
Ester and ethyl acetate, condensing reflux reaction, ethyl orthosilicate, methacrylic acid-β-hydroxypropyl acrylate and methyl methacrylate rub
You obtain hybrid collosol, are being aged, dry, obtain hybrid composite material than being 1:1:1；
S4. it after mixing the obtained amino-acid modified graft polypropylene of step S2 and antioxidant, is added in mixer and mixes, so
The hybrid composite material of terpene phenolic resin and step S3 preparation is added afterwards, is heated to terpene phenolic resin resin and melts completely
Afterwards, it is added, polyethylene wax and naphthenic oil, after mixing discharge, amino-acid modified graft polypropylene, hybrid composite material resists
Oxidant, terpene phenolic resin, polyethylene wax, the mass ratio of naphthenic oil are 130:32:3:25:3:8, and packaging obtains heat resistant type
Polyolefin hot-melt.
Comparative example 1
It is compared with embodiment 1, polypropylene is unmodified, remaining is identical.
Comparative example 2
It is compared with embodiment 1, directly addition SiO2, remaining is identical.
Peel strength: it according to GB/T 2790-1995 standard, is measured using universal testing machine；MFR value: melt is used
Flow rate analyzer is measured (100 DEG C of test temperature, load 21N).
Claims (6)
1. a kind of preparation method of heat resistant type PP hot melt adhesive, which comprises the following steps:
S1. by polypropylene, glycidyl methacrylate, styrene and cumyl peroxide 100-150:1- in mass ratio
2:3-6:0.15-0.25 adding twin-screw extrude after mixing, reactive extrursion, pelletizing, drying, purification are grafted
Polypropylene；
S2. by 1,6-aminocaprolc acid and graft polypropylene are added twin-screw extrude in the ratio of 1:100, and reactive extrursion is cut
Grain, is dried to obtain amino-acid modified graft polypropylene；
S3. by ethyl orthosilicate and methacrylic acid-β-hydroxypropyl acrylate, then deionized water, hydrochloric acid and ethyl alcohol is added in fully reacting
It is hydrolyzed, the pH for controlling solution is 3-4, and benzoyl peroxide, methyl methacrylate and acetic acid then is added by nitrogen
Ethyl ester is condensed back reaction, obtains hybrid collosol, be aged, and dries, obtains hybrid composite material；
S4. it after mixing the obtained amino-acid modified graft polypropylene of step S2 and antioxidant, is added in mixer and mixes, so
The hybrid composite material of terpene phenolic resin and step S3 preparation is added afterwards, is heated to terpene phenolic resin resin and melts completely
Afterwards, it is added, polyethylene wax and naphthenic oil, after mixing discharge, packaging obtains heat resistant type polyolefin hot-melt.
2. a kind of preparation method of heat resistant type PP hot melt adhesive according to claim 1, it is characterised in that: in the step S1
Extrusion reaction temperature is 180-190 DEG C, and screw speed takes 200-350r/min, finds time as 60-180s；
3. a kind of preparation method of heat resistant type PP hot melt adhesive according to claim 1, it is characterised in that: in the step S2
Wherein each barrel temperature of double screw extruder is respectively 160,180,200,200,190,180 DEG C.
4. a kind of preparation method of heat resistant type PP hot melt adhesive according to claim 1, it is characterised in that: in the step S3
Ethyl orthosilicate and methacrylic acid-β-hydroxypropyl acrylate react 60-150min at 50-60 DEG C.
5. a kind of preparation method of heat resistant type PP hot melt adhesive according to claim 1, it is characterised in that: in the step S3
The molar ratio of ethyl orthosilicate, methacrylic acid-β-hydroxypropyl acrylate and methyl methacrylate is 1:1:1.
6. a kind of preparation method of heat resistant type PP hot melt adhesive according to claim 1, it is characterised in that: in the step S3
Amino-acid modified graft polypropylene, hybrid composite material, antioxidant, terpene phenolic resin, polyethylene wax, the quality of naphthenic oil
Than for 100-150:25-40:2-4:20-30:1-5:5-10.
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| CN201811370216.1A CN109439240A (en) | 2018-11-17 | 2018-11-17 | A kind of preparation method of heat resistant type PP hot melt adhesive |
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| CN201811370216.1A CN109439240A (en) | 2018-11-17 | 2018-11-17 | A kind of preparation method of heat resistant type PP hot melt adhesive |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115216243A (en) * | 2022-07-14 | 2022-10-21 | 广东汇齐新材料有限公司 | Environment-friendly high-viscosity hot melt adhesive film and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86107790A (en) * | 1986-11-11 | 1988-04-06 | 山东省新材料研究所 | A kind of hot melt adhesive |
| EP0911148A2 (en) * | 1997-10-20 | 1999-04-28 | Hoechst Celanese Corporation | Adhesives for making multilayer films comprising liquid crystalline polymers and polyethylene |
| CN101717474A (en) * | 2009-11-20 | 2010-06-02 | 广州市合诚化学有限公司 | Adhesive master batch used for preparing polypropylene hot melt adhesive and preparation method thereof |
-
2018
- 2018-11-17 CN CN201811370216.1A patent/CN109439240A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86107790A (en) * | 1986-11-11 | 1988-04-06 | 山东省新材料研究所 | A kind of hot melt adhesive |
| EP0911148A2 (en) * | 1997-10-20 | 1999-04-28 | Hoechst Celanese Corporation | Adhesives for making multilayer films comprising liquid crystalline polymers and polyethylene |
| CN101717474A (en) * | 2009-11-20 | 2010-06-02 | 广州市合诚化学有限公司 | Adhesive master batch used for preparing polypropylene hot melt adhesive and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 史铁钧等: "PP/SiO2杂化复合材料的制备与性能研究", 《高分子通报》 * |
| 米长虹等: "硅杂化丙烯酸酯的制备及粘结性能研究", 《有机硅材料》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115216243A (en) * | 2022-07-14 | 2022-10-21 | 广东汇齐新材料有限公司 | Environment-friendly high-viscosity hot melt adhesive film and preparation method thereof |
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