CN112679819A - Modified APAO resin and preparation method thereof - Google Patents
Modified APAO resin and preparation method thereof Download PDFInfo
- Publication number
- CN112679819A CN112679819A CN202011552942.2A CN202011552942A CN112679819A CN 112679819 A CN112679819 A CN 112679819A CN 202011552942 A CN202011552942 A CN 202011552942A CN 112679819 A CN112679819 A CN 112679819A
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- China
- Prior art keywords
- polyolefin
- modified
- amorphous polyolefin
- antioxidant
- apao
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- XPVIQPQOGTVMSU-UHFFFAOYSA-N (4-acetamidophenyl)arsenic Chemical class CC(=O)NC1=CC=C([As])C=C1 XPVIQPQOGTVMSU-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000011347 resin Substances 0.000 title claims abstract description 19
- 229920005989 resin Polymers 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229920000098 polyolefin Polymers 0.000 claims abstract description 59
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 21
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 229920001384 propylene homopolymer Polymers 0.000 claims abstract description 13
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 238000007599 discharging Methods 0.000 claims description 5
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 3
- 229920013640 amorphous poly alpha olefin Polymers 0.000 abstract description 11
- 239000002994 raw material Substances 0.000 abstract description 4
- 238000010008 shearing Methods 0.000 abstract description 4
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000004831 Hot glue Substances 0.000 description 10
- 239000004743 Polypropylene Substances 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- 238000003763 carbonization Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Landscapes
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to an adhesive raw material and a preparation process thereof, in particular to a modified APAO resin and a preparation method thereof, so that the problem of weak heat shearing resistance of an APAO product is solved, the production process is simple, the APAO product can be prepared without improving a reaction kettle, the effect of low processing cost is further realized, and the APAO resin comprises 20-60% of amorphous polyolefin A by weight; 20-60% of amorphous polyolefin B; metallocene catalyzed polyolefin C5-30%; metallocene catalyzed polyolefin D5-30%; 5% -30% of modified propylene homopolymer E; 0.1 to 1 percent of antioxidant F; 0.1 to 1 percent of antioxidant G; the amorphous polyolefin A and the amorphous polyolefin B are two of 8300L, 8770L and 8825L; wherein 8300 is viscosity 3300 mPa.s at 190 deg.C, softening point 125 deg.C; wherein 8770 is viscosity 8500mPa · s at 190 ℃ and softening point 155 ℃; wherein 8825L has a viscosity of 30000 mPas at 190 deg.C and a softening point of 143 deg.C.
Description
Technical Field
The invention relates to an adhesive raw material and a preparation process thereof, in particular to a modified APAO resin and a preparation method thereof.
Background
APAO is a thermoplastic polymer that changes in physical state with temperature over a range of temperatures, while its chemical nature is unchanged. The material does not need solvent when in use, does not generate pungent smell when in melting, does not generate toxic and harmful volatile matters, and belongs to an environment-friendly material. APAO is solid at normal temperature, can be changed into liquid when being heated to a set temperature, and can be prepared into APAO hot melt adhesive by adding tackifying resin, plasticizer and the like; or can be partially added into the EVA hot melt adhesive to improve the heat resistance, solvent resistance, corrosion resistance and other properties of the EVA hot melt adhesive; can also be used as modified resin of rubber series pressure-sensitive adhesive to improve the thermal stability and the thermal shear resistance.
At present, the softening temperature of an APAO product is low, the heat retention is poor, and although the relay of the prepared APAO hot melt adhesive is enough, the heat shearing resistance performance still cannot reach the standard of automotive interior adhesive. The reactive hot melt adhesive can meet the performance requirements but has higher material cost and processing cost and needs a special reaction container, and the catalyst and reaction byproducts in the reactive hot melt adhesive can also be harmful to human bodies.
Disclosure of Invention
Aiming at the problems mentioned in the background technology, the invention aims to provide a modified APAO resin and a preparation method thereof, thereby improving the problem of weak heat shearing resistance of an APAO product, having simple production process, being prepared without improving a reaction kettle and further realizing the effect of low processing cost.
The technical purpose of the invention is realized by the following technical scheme: a modified APAO resin comprises 20-60 wt% of amorphous polyolefin A; 20-60% of amorphous polyolefin B;
metallocene catalyzed polyolefin C5-30%; metallocene catalyzed polyolefin D5-30%;
5% -30% of modified propylene homopolymer E; 0.1 to 1 percent of antioxidant F; 0.1 to 1 percent of antioxidant G.
Preferably, the amorphous polyolefin a and the amorphous polyolefin B are two of 8300, 8770 and 8825L;
wherein 8300 is viscosity 3300 mPa.s at 190 deg.C, softening point 125 deg.C;
wherein 8770 is viscosity 8500mPa · s at 190 ℃ and softening point 155 ℃;
wherein 8825L has a viscosity of 30000 mPas at 190 deg.C and a softening point of 143 deg.C.
Preferably, the metallocene-catalyzed polyolefin C is two of 6202, 6502, 8380, 8780 and 8880, having a softening point of 100-.
Preferably, the modified propylene homopolymer E has a viscosity of 6003 at 190 ℃ and a softening point of 165 ℃.
Preferably, the antioxidant F is antioxidant 1010.
The technical purpose of the invention is realized by the following technical scheme: a method for preparing a modified APAO resin comprising the steps of: step one, heating a reaction kettle to 180 ℃, adding amorphous polyolefin A, amorphous polyolefin B and antioxidant F into the reaction kettle, melting, stirring and vacuumizing;
step two, controlling the stable rotating speed, adding metallocene catalyzed polyolefin C, metallocene catalyzed polyolefin D and modified propylene homopolymer E after the amorphous polyolefin A, the amorphous polyolefin B and the antioxidant F are completely melted, heating, stirring and vacuumizing;
step three, maintaining the temperature of the reaction kettle at 180 ℃ until all the materials are mixed into uniform and transparent liquid;
and step four, stopping vacuumizing and stirring, and discharging to obtain the modified APAO.
In summary, the invention mainly has the following beneficial effects: amorphous polyolefin in the modified APAO resin and the preparation method thereof can provide excellent adhesion, and the high-softening-point part can also provide excellent heat resistance, and metallocene-catalyzed polyolefin has lower crystallinity and high strength, so that the shear displacement of amorphous polyolefin at high temperature is reduced; the propylene homopolymer with high melting point is adopted, has higher crystallinity, ensures the fluidity of the amorphous polyolefin, and simultaneously improves the softening temperature of the amorphous polyolefin due to the high crystallinity, thereby further improving the thermal shear resistance and the aging resistance.
The invention distinguishes hot EVA and common APAO hot melt adhesive, not only has excellent tackifying effect, but also greatly improves the heat shearing resistance and aging resistance of amorphous polyolefin, has low VOCS, meets the requirement of APAO automobile interior hot melt adhesive customers on the heat resistance of raw materials, and can be used as the raw material of boiling-resistant hot melt adhesive.
The invention adopts simple and effective blending process preparation, avoids reactive preparation methods such as reactive polyurethane hot melt adhesives and the like, has simple and effective process, can save a large amount of energy consumption, does not generate hazardous waste, and has good environmental protection, economic benefit and industrial production prospect.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A modified APAO resin comprises 20-60 wt% of amorphous polyolefin A; 20-60% of amorphous polyolefin B;
metallocene catalyzed polyolefin C5-30%; metallocene catalyzed polyolefin D5-30%;
5% -30% of modified propylene homopolymer E; 0.1 to 1 percent of antioxidant F; 0.1 to 1 percent of antioxidant G.
The amorphous polyolefin A and the amorphous polyolefin B are two of 8300L, 8770L and 8825L;
wherein 8300 is viscosity 3300 mPa.s at 190 deg.C, softening point 125 deg.C;
wherein 8770 is viscosity 8500mPa · s at 190 ℃ and softening point 155 ℃;
wherein 8825L has a viscosity of 30000 mPas at 190 deg.C and a softening point of 143 deg.C.
The metallocene-catalyzed polyolefin C is two of 6202, 6502, 8380, 8780 and 8880, having a softening point of 100-.
The modified propylene homopolymer E has the viscosity of 6003 at 190 ℃ and the softening point of 165 ℃.
The antioxidant F is an antioxidant 1010.
A method for preparing a modified APAO resin comprising the steps of: step one, heating a reaction kettle to 180 ℃, adding amorphous polyolefin A, amorphous polyolefin B and antioxidant F into the reaction kettle, melting, stirring and vacuumizing;
step two, controlling the stable rotating speed, adding metallocene catalyzed polyolefin C, metallocene catalyzed polyolefin D and modified propylene homopolymer E after the amorphous polyolefin A, the amorphous polyolefin B and the antioxidant F are completely melted, heating, stirring and vacuumizing;
step three, maintaining the temperature of the reaction kettle at 180 ℃ until all the materials are mixed into uniform and transparent liquid;
and step four, stopping vacuumizing and stirring, and discharging to obtain the modified APAO.
Example 1: heating a reaction kettle to 180 ℃, adding 8770400 g and 8300390 g of amorphous polyolefin into the reaction kettle for melting, stirring and vacuumizing, adding 10105 g of antioxidant, 1685 g of antioxidant, 6202150 g of metallocene catalyzed polyolefin and 600350 g of modified propylene homopolymer after the amorphous polyolefin is completely melted, heating, stirring and vacuumizing, and maintaining the temperature of the reaction kettle at 180 ℃ until all materials are mixed into uniform and transparent liquid; stopping vacuumizing and stirring, and discharging to obtain 1kg of modified APAO.
50g of the prepared modified APAO is placed in a beaker and placed in an oven at the temperature of 200 ℃, and after 24h/48h/72h, the appearance, the viscosity and the carbonization degree are observed. Another 50g of the modified APAO was placed in a glue gun, and the perforated PP panels were glued and subjected to SAFT testing in a SAFT tester.
The experimental data are as follows in table 1:
TABLE 1
Example 2: heating a reaction kettle to 180 ℃, adding 8825L 450g of amorphous polyolefin and 8770400 g of amorphous polyolefin into the reaction kettle for melting, stirring and vacuumizing, adding 10105 g of antioxidant, 1685 g of antioxidant, 878050 g of metallocene-catalyzed polyolefin and 600390 g of modified propylene homopolymer after the amorphous polyolefin is completely melted, heating, stirring and vacuumizing, and maintaining the temperature of the reaction kettle at 180 ℃ until all materials are mixed into uniform and transparent liquid. Stopping vacuumizing and stirring, and discharging to obtain 1kg of modified APAO. 50g of the prepared modified APAO is placed in a beaker and is placed in an oven at the temperature of 200 ℃, and the appearance, the viscosity and the carbonization degree are observed after 24h/48h/72 h. Taking another 50g of modified APAO in a glue gun, bonding the perforated PP plate, and carrying out SAFT test in a SAFT tester; increasing the ratio of amorphous polyolefin to modified polypropylene increases SAFT while maintaining heat aging.
The experimental data are as follows in table 2:
TABLE 2
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. A modified APAO resin characterized by: according to weight percentage, comprises 20 to 60 percent of amorphous polyolefin A; 20-60% of amorphous polyolefin B;
metallocene catalyzed polyolefin C5-30%; metallocene catalyzed polyolefin D5-30%;
5% -30% of modified propylene homopolymer E; 0.1 to 1 percent of antioxidant F; 0.1 to 1 percent of antioxidant G.
2. The modified APAO resin of claim 1, characterized in that: the amorphous polyolefin A and the amorphous polyolefin B are two of 8300L, 8770L and 8825L;
wherein 8300 is viscosity 3300 mPa.s at 190 deg.C, softening point 125 deg.C;
wherein 8770 is viscosity 8500mPa · s at 190 ℃ and softening point 155 ℃;
wherein 8825L has a viscosity of 30000 mPas at 190 deg.C and a softening point of 143 deg.C.
3. The modified APAO resin of claim 1, characterized in that: the metallocene-catalyzed polyolefin C is two of 6202, 6502, 8380, 8780 and 8880, having a softening point of 100-.
4. The modified APAO resin of claim 1, characterized in that: the modified propylene homopolymer E has the viscosity of 6003 at 190 ℃ and the softening point of 165 ℃.
5. The modified APAO resin of claim 1, characterized in that: the antioxidant F is an antioxidant 1010.
6. A process for the preparation of a modified APAO resin according to claim 1, characterized in that: the method comprises the following steps: step one, heating a reaction kettle to 180 ℃, adding amorphous polyolefin A, amorphous polyolefin B and antioxidant F into the reaction kettle, melting, stirring and vacuumizing;
step two, controlling the stable rotating speed, adding metallocene catalyzed polyolefin C, metallocene catalyzed polyolefin D and modified propylene homopolymer E after the amorphous polyolefin A, the amorphous polyolefin B and the antioxidant F are completely melted, heating, stirring and vacuumizing;
step three, maintaining the temperature of the reaction kettle at 180 ℃ until all the materials are mixed into uniform and transparent liquid;
and step four, stopping vacuumizing and stirring, and discharging to obtain the modified APAO.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011552942.2A CN112679819A (en) | 2020-12-24 | 2020-12-24 | Modified APAO resin and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011552942.2A CN112679819A (en) | 2020-12-24 | 2020-12-24 | Modified APAO resin and preparation method thereof |
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| CN112679819A true CN112679819A (en) | 2021-04-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202011552942.2A Pending CN112679819A (en) | 2020-12-24 | 2020-12-24 | Modified APAO resin and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1571825A (en) * | 2001-10-18 | 2005-01-26 | 博斯蒂克芬德利公司 | Hot melt adhesive composition based on a blend of amorphous poly-alpha-olefin and syndiotactic polypropylene |
| CN102786895A (en) * | 2012-09-11 | 2012-11-21 | 无锡市万力粘合材料有限公司 | Hot-melt adhesive for transparent PP (polypropylene) boxes and preparation method of hot-melt adhesive |
| CN104449465A (en) * | 2013-09-22 | 2015-03-25 | 杭州邦林热熔胶有限公司 | Hot melt adhesive for mattresses and sofas and preparation method thereof |
| CN106349975A (en) * | 2016-08-30 | 2017-01-25 | 华威粘结材料（上海）股份有限公司 | APAO cladding hot melt glue composition and preparation method thereof |
| CN107257833A (en) * | 2015-01-23 | 2017-10-17 | 波士胶公司 | Metallocene-polyolefin base low activation temperature seals hot-melt adhesive |
| CN107523235A (en) * | 2017-08-16 | 2017-12-29 | 华威粘结材料（上海）股份有限公司 | A kind of PUR and preparation method and application |
| CN108587536A (en) * | 2018-04-02 | 2018-09-28 | 无锡海特新材料研究院有限公司 | A kind of APAO hot melt adhesives and preparation method thereof |
| CN110540818A (en) * | 2019-09-18 | 2019-12-06 | 杭州之江新材料有限公司 | Non-reactive polyolefin hot melt adhesive, preparation method and application thereof |
-
2020
- 2020-12-24 CN CN202011552942.2A patent/CN112679819A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1571825A (en) * | 2001-10-18 | 2005-01-26 | 博斯蒂克芬德利公司 | Hot melt adhesive composition based on a blend of amorphous poly-alpha-olefin and syndiotactic polypropylene |
| CN102786895A (en) * | 2012-09-11 | 2012-11-21 | 无锡市万力粘合材料有限公司 | Hot-melt adhesive for transparent PP (polypropylene) boxes and preparation method of hot-melt adhesive |
| CN104449465A (en) * | 2013-09-22 | 2015-03-25 | 杭州邦林热熔胶有限公司 | Hot melt adhesive for mattresses and sofas and preparation method thereof |
| CN107257833A (en) * | 2015-01-23 | 2017-10-17 | 波士胶公司 | Metallocene-polyolefin base low activation temperature seals hot-melt adhesive |
| CN106349975A (en) * | 2016-08-30 | 2017-01-25 | 华威粘结材料（上海）股份有限公司 | APAO cladding hot melt glue composition and preparation method thereof |
| CN107523235A (en) * | 2017-08-16 | 2017-12-29 | 华威粘结材料（上海）股份有限公司 | A kind of PUR and preparation method and application |
| CN108587536A (en) * | 2018-04-02 | 2018-09-28 | 无锡海特新材料研究院有限公司 | A kind of APAO hot melt adhesives and preparation method thereof |
| CN110540818A (en) * | 2019-09-18 | 2019-12-06 | 杭州之江新材料有限公司 | Non-reactive polyolefin hot melt adhesive, preparation method and application thereof |
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Application publication date: 20210420 |