CN105602241A - Nano electroconducting heat-conducting composite material - Google Patents
Nano electroconducting heat-conducting composite material Download PDFInfo
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- CN105602241A CN105602241A CN201610080738.2A CN201610080738A CN105602241A CN 105602241 A CN105602241 A CN 105602241A CN 201610080738 A CN201610080738 A CN 201610080738A CN 105602241 A CN105602241 A CN 105602241A
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- composite material
- conductive
- nano heat
- material according
- conductive composite
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- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 12
- 229920002292 Nylon 6 Polymers 0.000 claims abstract description 9
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 8
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 8
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 239000000314 lubricant Substances 0.000 claims abstract description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 21
- 229910021389 graphene Inorganic materials 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000003054 catalyst Substances 0.000 claims description 7
- 239000000839 emulsion Substances 0.000 claims description 6
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 6
- 239000004677 Nylon Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229920001778 nylon Polymers 0.000 claims description 5
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 4
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 4
- 239000008116 calcium stearate Substances 0.000 claims description 4
- 235000013539 calcium stearate Nutrition 0.000 claims description 4
- 229920006225 ethylene-methyl acrylate Polymers 0.000 claims description 4
- 238000005453 pelletization Methods 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 229920001577 copolymer Polymers 0.000 claims description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 2
- 229920001296 polysiloxane Polymers 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 229920001897 terpolymer Polymers 0.000 claims description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 239000005043 ethylene-methyl acrylate Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 9
- 239000000383 hazardous chemical Substances 0.000 abstract 1
- 239000012745 toughening agent Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 239000004952 Polyamide Substances 0.000 description 2
- 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 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 description 2
- 229920002647 polyamide Polymers 0.000 description 2
- 229920002302 Nylon 6,6 Polymers 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 150000004645 aluminates Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000003951 lactams Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- MOMGDEWWZBKDDR-UHFFFAOYSA-M sodium;3,4,5,6-tetrahydro-2h-azepin-7-olate Chemical compound [Na+].O=C1CCCCC[N-]1 MOMGDEWWZBKDDR-UHFFFAOYSA-M 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/226—Compounding polymers with additives, e.g. colouring using masterbatch techniques using a polymer as a carrier
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- 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
- C08K2201/011—Nanostructured additives
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a nano electroconducting heat-conducting composite material and a preparation method thereof. The nano electroconducting heat-conducting composite material is characterized by comprising the following raw materials in parts by mass: 70-90 parts of nylon 6, 5-20 parts of nylon 6 master batch, 1-5 parts of toughener, 0.1-0.4 part of antioxidant and 0-5 parts of lubricant. The composite material has excellent properties. The composite material does not pollute the environment, and conforms to the instructions in European Union ROHs (Restriction of Hazardous Substances).
Description
Technical field
The present invention relates to a kind of conductive nano heat-conductive composite material and preparation method thereof.
Background technology
Plastics industry has been a Chaoyang industry since 20th century, is mainly applied range, is easily repeatedly used and quiltThe people accept.
Nylon is the general designation of polyamide, is that output maximum in five large general engineering plastic, kind are maximum, most widely used, comprehensiveExtrusion resin that can be the best. In polyamide, the output of nylon 6 and nylon 66 and consumption maximum, account for total polyamides90% left and right of amine, nylon mainly has outstanding feature at aspects such as mechanics, chemistry, thermal properties.
In recent years, heat-conductivity conducting composite is developed gradually, but price is high, processing is more difficult, so adopt newMaterial is extremely urgent, and along with the performance of Graphene manifests gradually, its heat-resisting electric conductivity is also by most material uses, stillDue to the easy reunion of nano material, in material, extrusion molding is difficult to demonstrate nano-meter characteristic.
Summary of the invention
For addressing the above problem, the invention provides a kind of conductive nano heat-conductive composite material, comprise the raw material of following mass fraction:
Preferably, nylon 6 master batches are Graphene master batch.
Preferably, Graphene master batch is composed of the following components: nylon 69 5-98 part, Graphene 2-3 part.
Preferably, Graphene master batch is prepared by following methods: (1), graphite is joined in the solution of strong silicyl oxide, and heating,Be stirred to even one-tenth liquid, mixing speed can be 400-600RPM; (2), by solution by accelerating to 50-100m/s, whereinCan accelerate by high pressure; (3) high-speed liquid, being obtained by step (2) enters the vaporific pelletizing head-on collision of high-speed ultrasonic equipment; (4),The emulsion being penetrated by step 3 enters into the emulsion of caprolactam, stirs, and adds catalyst, adds and is pressed into and get final product.
Preferably, the present invention also can comprise coupling agent, specifically can be Aluminate and/or titanate esters.
Preferably, described antioxidant is hindered phenol antioxygen or phosphite antioxidant.
Preferably, described antioxidant is one or more the mixture in B215, B225 and B900.
In the present invention, Graphene manufacture is in the following ways: 1, graphite is joined in the solution of strong silicyl oxide, and heating, at a high speedStir, to evenly becoming liquid; 2, solution is accelerated to 50-100m/s by high pressure; 3, the high-speed liquid being obtained by step 2 entersThe vaporific pelletizing head-on collision of high-speed ultrasonic equipment, produces gluey nano-solution.
In the present invention, Graphene master batch can be prepared by following mode: 1, in autoclave, add caprolactam, catalyst, above-mentionedGluey nano-solution; 2, heating, pressurization, stirring, long-chain polymer to be formed, extrudes formation particle.
Preferably, described flexibilizer is ethylene-methyl methacrylate butyl ester-glycidyl acrylate copolymer, ethene-metering systemThe mixture of one or more in acid methyl terpolymer and ethylene-methyl acrylate copolymer.
Described hindered phenol antioxygen can be one or more in 1076,168,264 and 1010.
Described lubricant is one or more in EBS, dolomol, calcium stearate, PE wax and silicone powder.
A preparation method for conductive nano heat-conductive composite material, comprises the steps: (1), mixes: by nylon 6, nylon 6Master batch, flexibilizer, antioxidant, lubricant are even in stirrer for mixing, put into main spout; (2), pass through twin-screw extrusionMoulding.
Preferably, described twin-screw is parallel double-screw.
Preferably, described twin-screw draw ratio is 48:1.
Preferably, described twin-screw processing temperature is 215-245 DEG C.
Preferably, nylon 6 master batches are Graphene master batch.
The present invention also provides a kind of preparation method of Graphene master batch, comprises the following steps: (1), graphite is joined to strong silicaIn the solution of alkane, heating, is stirred to even one-tenth liquid; (2), solution is accelerated to 50-100m/s by high pressure; (3), by stepSuddenly the high-speed liquid that (2) obtain enters the vaporific pelletizing head-on collision of high-speed ultrasonic equipment; (4) emulsion, being penetrated by step 3 enters into oneselfIn the emulsion of lactams, stir, add catalyst, add and be pressed into and get final product.
Preferably, described catalyst is base catalyst.
Preferably, described base catalyst is NaOH or sodium caprolactam.
The invention has the beneficial effects as follows: composite prepared by the present invention has excellent performance. Solve the reunion of Graphene,Provided a kind of industrial production process of nano-graphene simultaneously.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described further:
Embodiment 1:
A kind of conductive nano heat-conductive composite material and preparation thereof, its table composed as follows of filling a prescription:
Table 1: the formula composition of a kind of conductive nano heat-conductive composite material and preparation thereof
Embodiment 2:
Table 2: the formula composition of a kind of conductive nano heat-conductive composite material and preparation thereof
| Raw material | Mass parts |
| PA6 | 85 |
| Graphene master batch | 10 |
| Ethylene-methyl acrylate copolymer | 5 |
| Antioxidant 1010 | 0.1 |
| Antioxidant 1076 | 0.1 |
| Calcium stearate | 0.3 |
Comparative example 1:
Table 3: a kind of conductive nano heat-conductive composite material and preparation formula composition thereof
| Raw material | Mass parts |
| PA6 | 94 |
| Graphene | 1 |
| Ethylene-methyl acrylate copolymer | 5 |
| Antioxidant 1010 | 0.1 |
| Antioxidant 1076 | 0.1 |
| Calcium stearate | 0.3 |
Comparative example 2:
Table 4: a kind of conductive nano heat-conductive composite material and preparation formula composition thereof
The formula of embodiments of the invention can for example utilize double screw extruder to melt extrude moulding, melting by routine techniques mouldingThe temperature of extruding is 210-245 DEG C, screw speed: 380～420 turn/min, screw slenderness ratio is 48:1.
Composite prepared by routine 1-4 carries out performance test, and the test result of gained sees the following form:
Table 5: the performance of embodiment gained composite
| Embodiment 1 | Embodiment 2 | Comparative example 1 | Comparative example 2 | |
| Hot strength (Mpa) | 45 | 47 | 43 | 44 |
| Notched Izod impact strength (kJ/ ㎡) | 6.5 | 6 | 4.8 | 4.3 |
| Bending strength (Mpa) | 90 | 96 | 86 | 89 |
| Electrical conductivity (S.CM-1) | 56 | 73 | 4 | 11 |
| Thermal conductivity (W..M-1.K-1) | 4.1 | 5.6 | 1.2 | 1.6 |
Claims (9)
1. a conductive nano heat-conductive composite material, is characterized in that, is made up of the raw material of following mass fraction:
2. conductive nano heat-conductive composite material according to claim 1, is characterized in that: nylon 6 master batches are Graphene master batch.
3. conductive nano heat-conductive composite material according to claim 2, is characterized in that: Graphene master batch is composed of the following components:Nylon 69 5-98 part, Graphene 2-3 part.
4. conductive nano heat-conductive composite material according to claim 3, wherein Graphene master batch is prepared by following methods: (1), generalGraphite joins in the solution of strong silicyl oxide, and heating, is stirred to even one-tenth liquid; (2), solution is accelerated to 50-100m/s;(3), the high-speed liquid that obtained by step (2) enters the vaporific pelletizing of high-speed ultrasonic head-on collision equipment, makes Graphene; (4), willThe emulsion that step 3 penetrates adds in the emulsion of caprolactam, stirs, and adds catalyst, adds and is pressed into and obtains Graphene master batch.
5. conductive nano heat-conductive composite material according to claim 1, is characterized in that: described antioxidant is hindered phenol antioxygenOr phosphite antioxidant.
6. conductive nano heat-conductive composite material according to claim 6, is characterized in that: described antioxidant is B215, B225With one or more the mixture in B900.
7. conductive nano heat-conductive composite material according to claim 6, is characterized in that: described hindered phenol antioxygen is 1076,168, one or more in 264 and 1010.
8. conductive nano heat-conductive composite material according to claim 6, is characterized in that: described flexibilizer is ethene-methyl-propOlefin(e) acid butyl ester-glycidyl acrylate copolymer, ethylene-methyl methacrylate methyl terpolymer and ethylene-methyl acrylate copolymerIn one or more mixture.
9. conductive nano heat-conductive composite material according to claim 1, described lubricant be EBS, dolomol, calcium stearate,One or more in PE wax and silicone powder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610080738.2A CN105602241B (en) | 2016-02-04 | 2016-02-04 | A kind of conductive nano heat-conductive composite material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610080738.2A CN105602241B (en) | 2016-02-04 | 2016-02-04 | A kind of conductive nano heat-conductive composite material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105602241A true CN105602241A (en) | 2016-05-25 |
| CN105602241B CN105602241B (en) | 2018-04-17 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN201610080738.2A Active CN105602241B (en) | 2016-02-04 | 2016-02-04 | A kind of conductive nano heat-conductive composite material |
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| Country | Link |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107189428A (en) * | 2017-07-12 | 2017-09-22 | 长沙五犇新材料科技有限公司 | Graphene/carbon fiber reinforced nylon composite abrasion resistance material and preparation method and application |
| CN108193318A (en) * | 2017-12-28 | 2018-06-22 | 上海德福伦化纤有限公司 | A kind of graphene modified polylactic acid fiber and preparation method thereof |
| CN109181289A (en) * | 2018-09-30 | 2019-01-11 | 刘彦彦 | A kind of tenacity nylon material and preparation method thereof |
| CN109265986A (en) * | 2018-09-25 | 2019-01-25 | 杭州本松新材料技术股份有限公司 | A kind of high thermal conductivity nylon composite materials |
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Cited By (4)
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| CN107189428A (en) * | 2017-07-12 | 2017-09-22 | 长沙五犇新材料科技有限公司 | Graphene/carbon fiber reinforced nylon composite abrasion resistance material and preparation method and application |
| CN108193318A (en) * | 2017-12-28 | 2018-06-22 | 上海德福伦化纤有限公司 | A kind of graphene modified polylactic acid fiber and preparation method thereof |
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| CN109181289A (en) * | 2018-09-30 | 2019-01-11 | 刘彦彦 | A kind of tenacity nylon material and preparation method thereof |
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| Publication number | Publication date |
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| CN105602241B (en) | 2018-04-17 |
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