CN105733495B - A kind of new type hot-melt adhesive and preparation method thereof - Google Patents
A kind of new type hot-melt adhesive and preparation method thereof Download PDFInfo
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- CN105733495B CN105733495B CN201610273411.7A CN201610273411A CN105733495B CN 105733495 B CN105733495 B CN 105733495B CN 201610273411 A CN201610273411 A CN 201610273411A CN 105733495 B CN105733495 B CN 105733495B
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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
- C09J177/00—Adhesives based on polyamides obtained by reactions forming a carboxylic amide link in the main chain; Adhesives based on derivatives of such polymers
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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
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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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
- 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
- C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
- C09J175/04—Polyurethanes
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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
- 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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Abstract
The present invention discloses a kind of new type hot-melt adhesive and preparation method thereof, especially a kind of suitable for metal compound new type hot-melt adhesive and preparation method thereof be bonded with ABS plastic.It is primarily characterized in that, raw material is constituted by mass percentage, comprising: nylon type copolyamide 40% ~ 45%, thermoplastic polyurethane 40% ~ 45%, compatilizer 4% ~ 10%, tackifier 5% ~ 15%, filler 1% ~ 5% and antioxidant 0.1% ~ 0.3%.It is to pick up specific proportion polymerizable raw material to react the nylon type copolyamide to be formed and have good adhesion to metal first, then by itself and thermoplastic polyurethane under the synergistic effect of specific compatilizer, with extrusion after other auxiliary materials in proportion blended melting to get the new type hot-melt adhesive for having good adhesion to metal and ABS plastic.So that products obtained therefrom through the invention, meet demand, simple process, and it is convenient for industrial production and application.
Description
Technical field
The present invention relates to a kind of new type hot-melt adhesives and preparation method thereof, especially a kind of to be suitable for the metal materials such as aluminium, stainless steel
Expect compound new type hot-melt adhesive and preparation method thereof be bonded with ABS plastic.
Background technique
Metal material and reinforced plastics are widely used engineering material, and performance has his own strong points: metal material is strong
Degree, toughness, heat-resisting, thermally conductive, wear-resisting, texture etc. are with the obvious advantage;ABS as most popular general engineering plastic it
One, have the characteristics that impact resistance, anti-corrosion, easy processing, dimensionally stable, lustrous surface are good, electroplating surface, weldering can also be carried out
It connects, the secondary operation such as hot pressing and bonding.Metal and the application that ABS plastic directly bonds are more and more wider, more and more apply
Instrument and meter industry, electronic enterprises, machinery industry, weaving and building trade etc..
But since the architectural difference between metal and plastics, the property of two kinds of materials differ greatly, lead to interfacial adhesion
Intensity is lower, is easy to appear degumming, and during the bonding process, the material easy damaged deformation bonded.Patent CN103770414A
A kind of emulsion-type polyacrylic acid adhesive for bonding ABS plastics and aluminium foil is disclosed, which has penetrating odor,
It is unfavorable for construction operation, and adhesion strength is lower, the scope of application is narrow；Patent CN101429413B discloses a kind of for gluing
Tie the double-layer composite hot melt adhesive film of the plastics such as aluminium, stainless steel and other metal materials and ABS, PVC, PET, although the glue film to metal and
Plastics have good bond effect, but the process of duplicature is more complicated, time-consuming, the furthermore storage and fortune of the glue film
The defeated protection for also needing release paper, leads to higher cost, is unfavorable for scale application.
In conclusion in terms of existing hot melt adhesive can't meet practical application to the adhesive property of metal and ABS plastic
Demand.A kind of new type hot-melt adhesive is developed, profession is used for bonded metal and ABS plastic, becomes urgent problem to be solved.
Summary of the invention
The purpose of the present invention is to provide a kind of new type hot-melt adhesives and preparation method thereof, so that resulting new through the invention
Type hot melt adhesive product meets bonding composite demand of the metal with ABS plastic.
The technical scheme adopted by the invention is as follows: a kind of new type hot-melt adhesive, raw material are constituted, by mass percentage, packet
It includes: nylon type copolyamide 40% ~ 45%, thermoplastic polyurethane 40% ~ 45%, compatilizer 4% ~ 10%, tackifier 5% ~ 15%, filler 1%
~ 5% and antioxidant 0.1% ~ 0.3%.
Wherein, the fusing point of above-mentioned thermoplastic polyurethane is 80 DEG C ~ 100 DEG C, and melt index is 40 ~ 45g/10min/
2.16kg/190℃；
And above-mentioned nylon type copolyamide is then existed by three kinds of caprolactam, nylon salt and Nylon-1010 Salt primary raw materials
Be polymerized under suitable water and stearic acid effect, and the molar percentage of above-mentioned three kinds of primary raw materials be respectively 38% ~ 42%,
32% ~ 38% and 23% ~ 29%, the molar ratio of the sum of above-mentioned stearic acid and above-mentioned three kinds of primary raw materials is 0.9 ~ 1.2:100；
Above-mentioned compatilizer is the polyethylene-vinyl acetate that the maleic anhydride that grafting rate is 2.0 ~ 2.3% is grafted, either
The polyolefin that the maleic anhydride that grafting rate is 1.2 ~ 1.5% is grafted；
Above-mentioned tackifier are selected from one of newtrex, thermoplastic phenolic resin, terpene resin, hydrogenated petroleum resin；
Above-mentioned filler is one of talcum powder, white carbon black, calcium carbonate；
Above-mentioned antioxidant is selected from four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters or 2,6- bis-
One of t-butyl-p-methylphenol.
The preparation method of the above-mentioned new type hot-melt adhesive, then include the following steps:
(1) firstly, preparing nylon type copolyamide, with reference to the proportion of above-mentioned nylon type copolyamide, choose caprolactam,
Nylon salt, three kinds of primary raw materials of Nylon-1010 Salt and suitable water and stearic acid, add it in reaction kettle and are gathered
Reaction is closed, nylon type copolyamide is formed；
(2) secondly, with reference to above-mentioned new type hot-melt adhesive proportion, by mass percentage, by 40% ~ 45% above-mentioned nylon type
Copolyamide, 40% ~ 45% thermoplastic polyurethane and 4% ~ 10% compatilizer, 5% ~ 15% tackifier, 1% ~ 5% are filled out
Material, 0.1% ~ 0.3% antioxidant, be added in high-speed mixer and stir evenly；
(3) then, above-mentioned material after evenly mixing is added in double screw extruder, is squeezed out after melting to get this
New type hot-melt adhesive.
Powdery, granular, strip, glue film shape or retinitis etc. is made in the visual demand of the new type hot-melt adhesive, for convenience of metal with
ABS plastic is bonded composite industrial application, which is preferably made glue film shape or retinitis.
When needing to be made glue film shape, the above-mentioned new type hot-melt adhesive is coated i.e. by casting machine or heat seeling coating equipment
It can；
When needing that retinitis is made, the above-mentioned new type hot-melt adhesive is passed through into melt-out spinning web-forming equipment.
Innovation of the invention is, by design raw material and its proportion, copolymerization, which is formed, first has good glue to metal
The nylon type copolyamide for connecing performance, then by itself and thermoplastic polyurethane under the synergistic effect of specific compatilizer, with other
Auxiliary material is squeezed out after blended melting in proportion to get the new type hot-melt adhesive for having good adhesion to metal and ABS plastic.Together
When, it can be also directed to practical application request, metal be bonded with ABS plastic compound glue film or net can be directly suitable for by being made one layer
Film.Compared to existing adhesive, present invention process is relatively easy, is more suitable for large-scale industrial production；Meanwhile through the invention
The new type hot-melt adhesive of preparation is compound by hot pressing with ABS plastic to metal under the conditions of 30s at 100 DEG C, can be obtained preferable
Bond effect, hot pressing temperature is lower, and the time is short, not will lead to the deformation of ABS plastic plate.
Specific embodiment
The present invention is addressed further under below by embodiment, but is not limited thereto.
Embodiment 1
Prepare nylon type copolyamide: by 113.16g caprolactam (1mol), 234.73g nylon salt
(0.895mol), 273.02g Nylon-1010 Salt (0.737mol), 6.74g stearic acid (0.0237mol) and 100g deionization
Water is added in the 2L autoclave with blender, thermometer and pressure gauge；After the completion of feeding intake, replaced with nitrogen
And vacuumize, eliminate the air in reaction kettle；It is then charged with the high pure nitrogen of 0.2MPa, heating is slowly ramped to 250 DEG C,
Under the pressure of 1.8MPa, insulation reaction 2 hours, it is slowly decompressed to normal pressure, and is continued after being decompressed to 0.05MPa dehydration 1 hour；It puts
Material pelletizing obtains granular nylon type copolyamide (PA-1).
The preparation of new type hot-melt adhesive: by 400g PA-1,400g thermoplastic polyurethane, (fusing point is 100 DEG C, and melt index is
40g/10min/2.16kg/190 DEG C), 5g maleic anhydride grafting polyethylene-vinyl acetate (grafting rate 2%), 150g polymerization
Rosin, 43g talcum powder, 2g antioxidant 1010 (four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters) are thrown
Enter in high-speed mixer and is uniformly mixed；Mixed material is put into double screw extruder, is squeezed out after melting novel to get this
Hot melt adhesive.
The new type hot-melt adhesive sample is labeled as A1.
Embodiment 2
Prepare nylon type copolyamide: by 116.14g caprolactam (1.026mol), 220.93g nylon salt
After the mixing of (0.842mol) and 282.77g Nylon-1010 Salt (0.763mol), one is added to blender, thermometer and pressure
In the 2L autoclave of power table；7.49g stearic acid (0.0263mol) and 100g deionized water are added, simultaneously with nitrogen displacement
It vacuumizes, eliminates the air in reaction kettle；It is then charged with the high pure nitrogen of 0.2MPa, heating is slowly ramped to 230 DEG C, in 1.0-
Under the pressure of 1.2MPa, insulation reaction 3 hours, it is slowly decompressed to normal pressure, and is continued after being decompressed to 0.05MPa dehydration 1 hour；It puts
Material pelletizing obtains granular nylon type copolyamide (PA-2).
Prepare new type hot-melt adhesive: by 435g PA-2,435g thermoplastic polyurethane, (fusing point is 80 DEG C, melt index 45g/
10min/2.16kg/190 DEG C), 7g maleic anhydride grafting polyethylene-vinyl acetate (grafting rate 2.3%), 112g thermoplasticity
Phenolic resin, 10g calcium carbonate, 1g antioxidant BHT (2,6-di-tert-butyl p-methylphenol), investment high-speed mixer mixing are equal
It is even；The material mixed is put into TE35 double screw extruder, is squeezed out after melting to get the new type hot-melt adhesive.
The new type hot-melt adhesive sample is labeled as A2.
Embodiment 3
Prepare nylon type copolyamide: by 116.14g caprolactam (1.026mol), 262.35g nylon salt (1mol),
After the mixing of 224.27 g Nylon-1010 Salts (0.605mol), it is added to the 2L high with blender, thermometer and pressure gauge
It presses in reaction kettle；8.23g stearic acid (0.0289mol) and 100g deionized water are added, is replaced and is vacuumized with nitrogen, eliminated
Air in reaction kettle；It is then charged with the high pure nitrogen of 0.2MPa, heating is slowly ramped to 230 DEG C, in the pressure of 1.0-1.2MPa
Under power, insulation reaction 3 hours, it is slowly decompressed to normal pressure, and is continued after being decompressed to 0.05MPa dehydration 1 hour；Blowing pelletizing obtains
Granular nylon type copolyamide (PA-3).
Prepare new type hot-melt adhesive: by 440g PA-3,440g thermoplastic polyurethane, (fusing point is 88 DEG C, melt index 42g/
10min/2.16kg/190 DEG C), 9g maleic anhydride grafting polyolefin (grafting rate 1.2%), 58g terpene resin, 50g hard charcoal
Black, 3g antioxidant 1010 (four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters) puts into high-speed mixer
It is uniformly mixed；Then the material mixed is put into TE35 double screw extruder, is squeezed out after melting to get the new-type heat-melting
Glue.
The new type hot-melt adhesive sample is labeled as A3.
Embodiment 4
Prepare nylon type copolyamide: by 125.07g caprolactam (1.105mol), 234.73g nylon salt
After the mixing of (0.895mol), 234.02g Nylon-1010 Salt (0.632mol), one is added to blender, thermometer and pressure
In the 2L autoclave of power table；8.98g stearic acid (0.0316mol) and 100g deionized water are added, simultaneously with nitrogen displacement
It vacuumizes, eliminates the air in reaction kettle；It is then charged with the high pure nitrogen of 0.2MPa, heating is slowly ramped to 230 DEG C, in 1.0-
Under the pressure of 1.2MPa, insulation reaction 3 hours, it is slowly decompressed to normal pressure, and is continued after being decompressed to 0.05MPa dehydration 1 hour；It puts
Material pelletizing obtains granular nylon type copolyamide (PA-4).
Prepare new type hot-melt adhesive: by 450g PA-4,450g thermoplastic polyurethane, (fusing point is 95 DEG C, melt index 44g/
10min/2.16kg/190 DEG C), polyolefin (grafting rate 1.5%), 50g hydrogenated petroleum resin, the 38g of the grafting of 10g maleic anhydride it is sliding
Mountain flour, 2g antioxidant 1010 (four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters) put into mixed at high speed
Machine is uniformly mixed；Then the material mixed is put into TE35 double screw extruder, is squeezed out after melting to get the novel heat
Melten gel.
The new type hot-melt adhesive sample is labeled as A4.
Performance test
For convenience of metal Application of composite Nian Jie with ABS plastic or test, by each new type hot-melt adhesive sample of above-mentioned A1-A4,
The new-type heat-melting glue film with a thickness of 0.10mm is respectively prepared, with reference to No. 2790 standards of GB/T, tests each new-type heat-melting film sample
90 ° of peel strength of ABS/ aluminium and ABS/ stainless steel is bonded at 100 DEG C, 0.2MPa, hot pressing 30s.
Test result is as follows table 1:
Table 1: adhesion strength of each new-type heat-melting film sample to ABS/ metal.
It can be seen that from upper table 1, through the invention adhesive strength of the prepared new type hot-melt adhesive to metal and ABS plastic
It is bigger, and bond damage mode is largely cohesional failure, glue film has residual, explanation on metal and ABS plastic surface
The new type hot-melt adhesive has very strong cementitiousness to metal and ABS plastic.And in practical application, pressing temperature is lower, it is
100 DEG C, ABS material will not be damaged；The pressing time is also shorter, is 30s, is convenient for constructing operation.
Claims (8)
1. a kind of hot melt adhesive, which is characterized in that its raw material is constituted, by mass percentage, comprising:
Nylon type copolyamide 40%~45%；
Thermoplastic polyurethane 40%~45%；
Compatilizer 4%~10%；
Tackifier 5%~15%；
Filler 1%~5%；
Antioxidant 0.1%~0.3%；
Wherein, the fusing point of the thermoplastic polyurethane is 80 DEG C~100 DEG C, and melt index is 40~45g/10min/
2.16kg/190℃；The nylon type copolyamide is existed by three kinds of caprolactam, nylon salt and Nylon-1010 Salt primary raw materials
Be polymerized under suitable water and stearic acid effect, and the molar percentage of three kinds of primary raw materials be respectively 38%~
42%, 32%~38% and 23%~29%；The molar ratio of the sum of the stearic acid and three kinds of primary raw materials is 0.9~
1.2:100；The compatilizer is in the polyethylene-vinyl acetate of maleic anhydride grafting or the polyolefin of maleic anhydride grafting
One kind.
2. hot melt adhesive as described in claim 1, it is characterised in that: the polyethylene-vinyl acetate of the maleic anhydride grafting
Grafting rate is 2.0~2.3%, and the grafting rate of the polyolefin of the maleic anhydride grafting is 1.2~1.5%.
3. hot melt adhesive as described in claim 1, it is characterised in that: the tackifier are selected from newtrex, thermoplastic phenolic resin
One of rouge, terpene resin, hydrogenated petroleum resin；The filler is one of talcum powder, white carbon black, calcium carbonate；It is described
Antioxidant be selected from four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters or 2,6- di-t-butyl is to methyl
Phenol.
4. a kind of preparation method of hot melt adhesive, which comprises the steps of:
(1) prepare nylon type copolyamide, by mole meter, choose respectively 38%~42% caprolactam, 32%~
38% nylon salt and 23%~29% three kinds of primary raw materials of Nylon-1010 Salt and suitable water and stearic acid, be added
Polymerization reaction is carried out into reaction kettle to form；
(2) by mass percentage, by 40%~45% above-mentioned nylon type copolyamide, 40%~45% fusing point is 80 DEG C
~100 DEG C, melt index be 40~45g/10min/2.16kg/190 DEG C of thermoplastic polyurethane and 4%~10% phase
Hold agent, 5%~15% tackifier, 1%~5% filler, 0.1%~0.3% antioxidant, be added in high-speed mixer
It stirs evenly；
(3) above-mentioned material after evenly mixing is added in double screw extruder, is squeezed in 100~120 DEG C of at a temperature of melting
Out to get the hot melt adhesive；
In the step (1), the stearic acid is 0.9~1.2:100 with the molar ratio with the sum of three kinds of primary raw materials；Institute
State one of the polyolefin of polyethylene-vinyl acetate or maleic anhydride grafting that compatilizer is maleic anhydride grafting.
5. the preparation method of hot melt adhesive as claimed in claim 4, which is characterized in that the polyethylene-of the maleic anhydride grafting
The grafting rate of vinylacetate is 2.0~2.3%, and the grafting rate of the polyolefin of the maleic anhydride grafting is 1.2~1.5%.
6. the preparation method of hot melt adhesive as claimed in claim 4, it is characterised in that: in the step (2), the tackifier choosing
One of auto polymerization rosin, thermoplastic phenolic resin, terpene resin, hydrogenated petroleum resin；The filler is talcum powder, hard charcoal
One of black, calcium carbonate；The antioxidant is selected from four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythrites
Ester or 2,6- di-tert-butyl methyl phenol.
7. the preparation method of hot melt adhesive as claimed in claim 4, which is characterized in that further include following steps:
(4) above-mentioned hot melt adhesive is coated by casting machine or heat seeling coating equipment, hot melt adhesive film is made.
8. the preparation method of hot melt adhesive as claimed in claim 4, which is characterized in that further include following steps:
(4) hot-melt adhesive film is made by melt-out spinning web-forming equipment in above-mentioned hot melt adhesive.
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| CN108841355A (en) * | 2018-07-19 | 2018-11-20 | 佛山陵朝新材料有限公司 | A kind of preparation method of composite polyamide hot melt adhesive |
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| CN111696715B (en) * | 2020-06-22 | 2021-06-29 | 中天科技装备电缆有限公司 | Flexible cable with sheath and preparation method thereof |
| CN113290977B (en) * | 2021-05-06 | 2022-02-15 | 安徽森泰木塑集团股份有限公司 | Wood-plastic coated metal composite profile and production process thereof |
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| CN114539965A (en) * | 2022-03-03 | 2022-05-27 | 东莞市华盛新材料有限公司 | Hot-melt adhesive capable of hot-pressing and water-splashing-preventing treatment and made of nylon material and preparation process of hot-melt adhesive |
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| CN102766413A (en) * | 2012-08-20 | 2012-11-07 | 天津博苑高新材料有限公司 | Integrated circuit (IC) card packaging special hot melting adhesive tape and preparation method thereof |
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