CN103805124B - A kind of preparation method of low temperature resistant polyamide thermosol - Google Patents
A kind of preparation method of low temperature resistant polyamide thermosol Download PDFInfo
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- CN103805124B CN103805124B CN201410017170.0A CN201410017170A CN103805124B CN 103805124 B CN103805124 B CN 103805124B CN 201410017170 A CN201410017170 A CN 201410017170A CN 103805124 B CN103805124 B CN 103805124B
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Abstract
A kind of low temperature resistant polyamide thermosol, it is made up of the following component counted by weight: dimer acid type polyamide and Grafted Derivatives 100 parts thereof, and rubber 10-50 part, cross-linking agent 1-3 part, assistant crosslinking agent 0-3 part, antioxidant 0.5-3 part are used in crosslinking; Described crosslinking rubber is the mixture of one or more in following material: ethylene propylene diene rubber, maleic anhydride graft ethylene propylene diene rubber, nitrile rubber; Described cross-linking agent is the mixture of one or more in following material: cumyl peroxide, ethylene thiourea, sulfur; Described assistant crosslinking agent is one or both the mixture in following material: triallyl cyanurate, iso-cyanuric acid triallyl ester. Low temperature resistant polyamide thermosol of the present invention can be used for electronics telecommunication, household electrical appliances, automobile and other industries, when being particularly suited in low temperature environment requiring higher to resistance to chemical reagents and oil resistivity, polar substances and apolar substance is bondd.
Description
Technical field
The invention belongs to PUR field, particularly relate to and adopt low temperature resistant polyamide thermosol of preparing of dynamic crosslinking method and preparation method thereof, improve resistance to low temperature and the adhesive property of polyamide hot.
Background technology
PA (Polyamide, polyamide) PUR, with polyamide for matrix, has softening point range narrow, and oil resistivity and drug resistance are good; To polar material cementability intensity advantages of higher, it it is the adhesive of a kind of function admirable. But polyamide hot has resistance to low temperature difference, it is susceptible to embrittlement at low temperatures, PUR performance is caused serious impact. Additionally polyamide hot polarity is strong, and the adhesive property for apolar substance (such as polyethylene) etc. is very poor, and its range of application is limited by very large.
Dynamic crosslinking is generally used in rubber plastic blend, carries out the preparation of thermoplastic elastomer (TPE), but has no the report for PUR field.
Summary of the invention
The technical problem to be solved in the present invention is in that: proposes a kind of low temperature resistant polyamide thermosol and preparation method thereof, improves resistance to low temperature and the adhesive property of polyamide hot.
In order to solve above-mentioned technical problem, the present invention proposes techniques below scheme: a kind of low temperature resistant polyamide thermosol, it is made up of the following component counted by weight: dimer acid type polyamide and Grafted Derivatives 100 parts thereof, rubber 10-50 part is used in crosslinking, cross-linking agent 1-3 part, assistant crosslinking agent 0-3 part, antioxidant 0.5-3 part;
Described crosslinking rubber is the mixture of one or more in following material: ethylene propylene diene rubber, maleic anhydride graft ethylene propylene diene rubber, nitrile rubber;
Described cross-linking agent is the mixture of one or more in following material: cumyl peroxide, ethylene thiourea, sulfur;
Described assistant crosslinking agent is one or both the mixture in following material: triallyl cyanurate, iso-cyanuric acid triallyl ester.
Limiting further of technique scheme is in that: described antioxidant is as the compound of one or more in following material: four [��-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester; 2,6 ditertiary butyl p cresol; 2-mercaptobenzimidazole; Zinc salt of 2 mercaptobenzimidazole; 2,2,4-trimethyl-1,2-dihyaroquinoline polymer; 4.4 a pair ofs (2.2-dimethyl benzyl) diphenylamines.
In order to solve above-mentioned technical problem, the present invention proposes techniques below scheme: the preparation method of a kind of low temperature resistant polyamide thermosol, and it comprises the following steps:
Step 1: load weighted dimer acid type polyamide and Grafted Derivatives thereof, crosslinking rubber, antioxidant blender are stirred;
Step 2: through mixer mixing, pelletize;
Step 3: add cross-linking agent and assistant crosslinking agent in the blend that step 2 obtains, adopts double screw extruder to carry out dynamic crosslinking, pelletize, obtains the low temperature resistant polyamide thermosol that dynamic crosslinking is modified after stirring;
Step 4: obtain low temperature resistant polyamide thermosol grain and proceed to drying machine drying, packaging.
Limiting further of technique scheme is in that: first twin screw pelletize heating-up temperature adopts 100-120 degree Celsius, and twin-screw extrusion dynamic crosslinking heating-up temperature is 140 DEG C-160 DEG C.
Limiting further of technique scheme is in that: described antioxidant is as the compound of one or more in following material: four [��-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester; 2,6 ditertiary butyl p cresol; 2-mercaptobenzimidazole; Zinc salt of 2 mercaptobenzimidazole; 2,2,4-trimethyl-1,2-dihyaroquinoline polymer; 4.4 a pair ofs (2.2-dimethyl benzyl) diphenylamines.
Compared with prior art, the method have the advantages that
Its cryogenic property is not only had stronger improvement by the PUR prepared by the present invention, also the adhesion strength of polyamide hot and apolar substance (polyethylene) is obviously improved, and PE/PE peel strength significantly improves, and good fluidity.
Low temperature resistant polyamide thermosol prepared by described dynamic crosslinking method can be used for electronics telecommunication, household electrical appliances, automobile and other industries, when being particularly suited in low temperature environment requiring higher to resistance to chemical reagents and oil resistivity, polar substances and apolar substance is bondd.
Low temperature resistant polyamide thermosol prepared by this dynamic crosslinking method, the resistance to low temperature making PUR obtains good improvement,-40 DEG C (ASTMD3111) are reached, also make polyamide hot that the adhesion strength of non-polar material (polyethylene) is greatly improved, reach 200N/25mm (GB/T2971PE/PE).
Detailed description of the invention
The present invention proposes a kind of low temperature resistant polyamide thermosol, and it is made up of the following component counted by weight: dimer acid type polyamide and Grafted Derivatives 100 parts thereof, and rubber 10-50 part, cross-linking agent 1-3 part, assistant crosslinking agent 0-3 part, antioxidant 0.5-3 part are used in crosslinking.
Described crosslinking rubber is the mixture of one or more in following material: ethylene propylene diene rubber, maleic anhydride graft ethylene propylene diene rubber, nitrile rubber.
Described cross-linking agent is the mixture of one or more in following material: cumyl peroxide, ethylene thiourea, sulfur.
Described assistant crosslinking agent is one or both the mixture in following material: triallyl cyanurate, iso-cyanuric acid triallyl ester.
Described antioxidant is the compound of one or more in following material: four [��-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester; 2,6 ditertiary butyl p cresol; 2-mercaptobenzimidazole (MB); Zinc salt of 2 mercaptobenzimidazole (MBZ); 2,2,4-trimethyl-1,2-dihyaroquinoline polymer (RD); 4.4 a pair ofs (2.2-dimethyl benzyl) diphenylamines.
Above-mentioned low temperature resistant polyamide thermosol adopts dynamic crosslinking method to prepare, and comprises the following steps:
Step 1: load weighted dimer acid type polyamide and Grafted Derivatives thereof, crosslinking rubber, antioxidant blender are stirred;
Step 2: through mixer mixing, pelletize;
Step 3: add cross-linking agent and assistant crosslinking agent in the blend that step 2 obtains, adopts double screw extruder to carry out dynamic crosslinking, pelletize, obtains the low temperature resistant polyamide thermosol that dynamic crosslinking is modified after stirring;
Step 4: obtain low temperature resistant polyamide thermosol grain and proceed to drying machine drying, packaging.
First twin screw pelletize heating-up temperature adopts 100-120 degree Celsius, and twin-screw extrusion dynamic crosslinking heating-up temperature is 140 DEG C-160 DEG C.
The cryogenic property of the low temperature resistant polyamide thermosol obtained by above-mentioned preparation method is obviously improved than the polyamide hot of prior art, and PE/PE peel strength significantly improves, and good fluidity.
Preparation embodiment 1
Weigh according to parts by weight, dimer acid type polyamide and Grafted Derivatives 100 parts thereof, crosslinking rubber 10 parts, cross-linking agent 1 part, 0.5 part of antioxidant.
Described crosslinking rubber is made up of ethylene propylene diene rubber 8 parts, maleic anhydride graft ethylene propylene diene rubber 2 parts.
Described cross-linking agent is cumyl peroxide 1 part.
Described antioxidant is 2-mercaptobenzimidazole (MB) 0.5 part.
By load weighted dimer acid type polyamide and Grafted Derivatives, ethylene propylene diene rubber, maleic anhydride graft ethylene propylene diene rubber, antioxidant add and carry out batch mixing in banbury, mixing complete after through single screw rod pelletize.
Load weighted cumyl peroxide, 2-mercaptobenzimidazole (MB) are put into blender with first banburying gained material grain, stirs 3min; Double screw extruder is warming up to 150 DEG C, mixture proceeds to double screw extruder and carries out dynamic crosslinking, cooling and dicing, drying machine drying, obtain low temperature resistant polyamide thermosol product, the easy moisture absorption of polyamide, stores in dehumidifying room.
Being prepared by dynamic crosslinking method low temperature resistant polyamide thermosol test, test result is as shown in the table:
Preparation embodiment 2
Weigh according to parts by weight, dimer acid type polyamide and Grafted Derivatives 100 parts thereof, crosslinking rubber 20 parts, cross-linking agent 2 parts, assistant crosslinking agent 1 part, 1 part of antioxidant.
Described crosslinking rubber is made up of ethylene propylene diene rubber 15 parts, maleic anhydride graft ethylene propylene diene rubber 5 parts.
Described cross-linking agent is cumyl peroxide 2 parts.
Described assistant crosslinking agent is triallyl cyanurate 1 part.
Described antioxidant is 2-mercaptobenzimidazole (MB) 1 part.
By load weighted dimer acid type polyamide and Grafted Derivatives, ethylene propylene diene rubber, maleic anhydride graft ethylene propylene diene rubber, 2-mercaptobenzimidazole (MB) add and carry out batch mixing in banbury, mixing complete after through single screw rod pelletize.
Load weighted cumyl peroxide, triallyl cyanurate and first banburying gained material grain are put into blender, stirs 3min; Double screw extruder is warming up to 150 DEG C, mixture proceeds to double screw extruder and carries out dynamic crosslinking, cooling and dicing, drying machine drying, obtain low temperature resistant polyamide thermosol product, the easy moisture absorption of polyamide, stores in dehumidifying room.
Being prepared by dynamic crosslinking method low temperature resistant polyamide thermosol test, test result is as shown in the table:
| Inspection project | Touchstone | Measured value |
| Softening point (DEG C) | GB/T 2294 | 113 |
| Peel strength (PE/PE, N/25mm) | GB/T 2971 | 92 |
| Low temperature flexibility | ASTM D3111 | -55 DEG C do not rupture |
| Hot strength (MPa) | ASTM D638 | 5.31 |
| Elongation at break (%) | ASTM D638 | 492% |
Preparation embodiment 3
Weigh according to parts by weight, dimer acid type polyamide and Grafted Derivatives 100 parts thereof, crosslinking rubber 30 parts, cross-linking agent 3 parts, 3 parts of antioxidant.
Described crosslinking rubber is nitrile rubber 30 parts.
Described cross-linking agent is ethylene thiourea 3 parts.
Described antioxidant is 2,2,4-trimethyl-1,2-dihyaroquinoline polymer 3 parts.
By load weighted dimer acid type polyamide and Grafted Derivatives, nitrile rubber, 2,2,4-trimethyl-1,2-dihyaroquinoline polymer adds and carries out batch mixing in banbury, mixing complete after through single screw rod pelletize.
Load weighted ethylene thiourea is put into blender with first banburying gained material grain, stirs 3min; Double screw extruder is warming up to 150 DEG C, mixture proceeds to double screw extruder and carries out dynamic crosslinking, cooling and dicing, drying machine drying, obtain low temperature resistant polyamide thermosol product, the easy moisture absorption of polyamide, stores in dehumidifying room.
Being prepared by dynamic crosslinking method low temperature resistant polyamide thermosol test, test result is as shown in the table:
Preparation embodiment 4
Weigh according to parts by weight, dimer acid type polyamide and Grafted Derivatives 100 parts thereof, crosslinking rubber 40 parts, cross-linking agent 2 parts, assistant crosslinking agent 1 part, 1 part of antioxidant.
Described crosslinking rubber is made up of ethylene propylene diene rubber 10 parts, maleic anhydride graft ethylene propylene diene rubber 30 parts.
Described cross-linking agent is cumyl peroxide 2 parts.
Described assistant crosslinking agent is triallyl cyanurate 1 part.
Described antioxidant is 2-mercaptobenzimidazole (MB) 1 part.
By load weighted dimer acid type polyamide and Grafted Derivatives, ethylene propylene diene rubber, maleic anhydride graft ethylene propylene diene rubber, 2-mercaptobenzimidazole (MB) add and carry out batch mixing in banbury, mixing complete after through single screw rod pelletize.
Load weighted cumyl peroxide, triallyl cyanurate and first banburying gained material grain are put into blender, stirs 3min; Double screw extruder is warming up to 150 DEG C, mixture proceeds to double screw extruder and carries out dynamic crosslinking, cooling and dicing, drying machine drying, obtain low temperature resistant polyamide thermosol product, the easy moisture absorption of polyamide, stores in dehumidifying room.
Being prepared by dynamic crosslinking method low temperature resistant polyamide thermosol test, test result is as shown in the table:
| Inspection project | Touchstone | Measured value |
| Softening point (DEG C) | GB/T 2294 | 129 |
| Peel strength (PE/PE, N/25mm) | GB/T 2971 | 143 |
| Low temperature flexibility | ASTM D3111 | -55 DEG C do not rupture |
| Hot strength (MPa) | ASTM D638 | 6.74 |
| Elongation at break (%) | ASTM D638 | 471% |
Preparation embodiment 5
Weigh according to parts by weight, dimer acid type polyamide and Grafted Derivatives 100 parts thereof, crosslinking rubber 50 parts, cross-linking agent 3 parts, assistant crosslinking agent 3 parts, 2 parts of antioxidant.
Described crosslinking rubber is made up of ethylene propylene diene rubber 30 parts, maleic anhydride graft ethylene propylene diene rubber 20 parts.
Described cross-linking agent is cumyl peroxide 3 parts.
Described assistant crosslinking agent is triallyl cyanurate 1 part.
Described antioxidant is 2-mercaptobenzimidazole (MB) 2 parts.
By load weighted dimer acid type polyamide and Grafted Derivatives, ethylene propylene diene rubber, maleic anhydride graft ethylene propylene diene rubber, 2-mercaptobenzimidazole (MB) add and carry out batch mixing in banbury, mixing complete after through single screw rod pelletize.
Load weighted cumyl peroxide, triallyl cyanurate and first banburying gained material grain are put into blender, stirs 3min; Double screw extruder is warming up to 150 DEG C, mixture proceeds to double screw extruder and carries out dynamic crosslinking, cooling and dicing, drying machine drying, obtain low temperature resistant polyamide thermosol product, the easy moisture absorption of polyamide, stores in dehumidifying room.
Being prepared by dynamic crosslinking method low temperature resistant polyamide thermosol test, test result is as shown in the table:
| Inspection project | Touchstone | Measured value |
| Softening point (DEG C) | GB/T 2294 | 145 |
| Peel strength (PE/PE, N/25mm) | GB/T 2971 | 179 |
| Low temperature flexibility | ASTM D3111 | -55 DEG C do not rupture |
| Hot strength (MPa) | ASTM D638 | 6.52 |
| Elongation at break (%) | ASTM D638 | 397% |
Above content is in conjunction with concrete preferred implementation, the present invention to be illustrated; not as the restriction assert the specific embodiment of the present invention; for those skilled in the art; on the basis of thinking of the present invention; made simple conversion, all should be considered as belonging to the present invention and be determined scope of patent protection by submitted claims.
Claims (1)
1. the preparation method of a low temperature resistant polyamide thermosol, it is characterised in that
Above-mentioned low temperature resistant polyamide thermosol is made up of the following component counted by weight: dimer acid type polyamide and Grafted Derivatives 100 parts thereof, and rubber 10-50 part, cross-linking agent 1-3 part, assistant crosslinking agent 0-3 part, antioxidant 0.5-3 part are used in crosslinking;
Described crosslinking rubber is the mixture of one or more in following material: ethylene propylene diene rubber, maleic anhydride graft ethylene propylene diene rubber, nitrile rubber;
Described cross-linking agent is the mixture of one or more in following material: cumyl peroxide, ethylene thiourea, sulfur;
Described assistant crosslinking agent is one or both the mixture in following material: triallyl cyanurate, iso-cyanuric acid triallyl ester; Described antioxidant is the compound of one or more in following material: four [��-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester; 2,6 ditertiary butyl p cresol; 2-mercaptobenzimidazole; Zinc salt of 2 mercaptobenzimidazole; 2,2,4-trimethyl-1,2-dihyaroquinoline polymer; 4.4 a pair ofs (2.2-dimethyl benzyl) diphenylamines;
Described antioxidant is the compound of one or more in following material: four [��-(3,5-di-tert-butyl-hydroxy phenyl) propanoic acid] pentaerythritol ester; 2,6 ditertiary butyl p cresol; 2-mercaptobenzimidazole; Zinc salt of 2 mercaptobenzimidazole; 2,2,4-trimethyl-1,2-dihyaroquinoline polymer; 4.4 a pair ofs (2.2-dimethyl benzyl) diphenylamines;
Described preparation method comprises the following steps:
Step 1: load weighted dimer acid type polyamide and Grafted Derivatives thereof, crosslinking rubber, antioxidant blender are stirred;
Step 2: through mixer mixing, pelletize;
Step 3: add cross-linking agent and assistant crosslinking agent in the blend that step 2 obtains, adopts double screw extruder to carry out dynamic crosslinking, pelletize, obtains the low temperature resistant polyamide thermosol that dynamic crosslinking is modified after stirring;
Step 4: obtain low temperature resistant polyamide thermosol grain and proceed to drying machine drying, packaging;
First twin screw pelletize heating-up temperature adopts 100-120 degree Celsius, and twin-screw extrusion dynamic crosslinking heating-up temperature is 140 DEG C-160 DEG C.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4359556A (en) * | 1981-06-05 | 1982-11-16 | Gulf Oil Corporation | Thermoplastic polyamide hot melt adhesive composition |
| CN101633829A (en) * | 2008-07-23 | 2010-01-27 | 上海轻工业研究所有限公司 | Low temperature resistant daiamid hot melt adhesive with high air tightness and application thereof |
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2014
- 2014-01-15 CN CN201410017170.0A patent/CN103805124B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4359556A (en) * | 1981-06-05 | 1982-11-16 | Gulf Oil Corporation | Thermoplastic polyamide hot melt adhesive composition |
| CN101633829A (en) * | 2008-07-23 | 2010-01-27 | 上海轻工业研究所有限公司 | Low temperature resistant daiamid hot melt adhesive with high air tightness and application thereof |
Non-Patent Citations (3)
| Title |
|---|
| 《丁腈橡胶/ 聚酰胺热塑性硫化胶的制备》;赵素合等;《合成橡胶工业》;20040915;第27卷(第5期);第305-308页 * |
| 《聚酰胺共混改性研究进展》;陈民杰等;《合成树脂及塑料》;20031231;第20卷(第1期);第72-77页 * |
| 《聚酰胺类热塑性弹性体的研究进展》;邱贤亮等;《橡胶工业》;20121231(第3期);第187-191页 * |
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