CN103613922B - A kind of high-barrier nano PA6 nano composite material and preparation method thereof - Google Patents
A kind of high-barrier nano PA6 nano composite material and preparation method thereof Download PDFInfo
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- CN103613922B CN103613922B CN201310619265.5A CN201310619265A CN103613922B CN 103613922 B CN103613922 B CN 103613922B CN 201310619265 A CN201310619265 A CN 201310619265A CN 103613922 B CN103613922 B CN 103613922B
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- composite material
- hexanolactam
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- 239000000463 material Substances 0.000 title claims abstract description 36
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229960000892 attapulgite Drugs 0.000 claims abstract description 19
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 19
- 229910052625 palygorskite Inorganic materials 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000007599 discharging Methods 0.000 claims abstract description 7
- 239000003112 inhibitor Substances 0.000 claims abstract description 7
- 230000003647 oxidation Effects 0.000 claims abstract description 7
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000003963 antioxidant agent Substances 0.000 claims description 6
- 230000003078 antioxidant effect Effects 0.000 claims description 6
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- VKLYZBPBDRELST-UHFFFAOYSA-N ethene;methyl 2-methylprop-2-enoate Chemical compound C=C.COC(=O)C(C)=C VKLYZBPBDRELST-UHFFFAOYSA-N 0.000 claims description 5
- 229920006225 ethylene-methyl acrylate Polymers 0.000 claims description 3
- 150000002989 phenols Chemical class 0.000 claims description 3
- 150000008301 phosphite esters Chemical class 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 abstract description 6
- 230000004888 barrier function Effects 0.000 abstract description 3
- 229920002292 Nylon 6 Polymers 0.000 description 20
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 239000004677 Nylon Substances 0.000 description 4
- 229920001778 nylon Polymers 0.000 description 4
- 150000001408 amides Chemical class 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
- 230000035699 permeability Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229920002302 Nylon 6,6 Polymers 0.000 description 1
- 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 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/14—Gas barrier composition
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of high-barrier nano PA6 nano composite material, it is made up of the raw material of following mass parts: the oxidation inhibitor of the obstruct material of PA6,5-20 part of 75-95 part, the toughner of 2-4 part, 0.1-0.3 part; Described obstruct material is preparation like this: 1) hexanolactam is put into reactor, add nano imvite, nano-attapulgite, nano silicon; 2) add sodium hydroxide again, vacuumize, heating, then add TDI, reaction 2-4h; 3) be cooled to room temperature in 30min-2h, open while starting cooling and stir, stop stirring when being cooled to room temperature, discharging.Matrix material of the present invention has good barrier property, and meanwhile, the matrix material of gained also has good mechanical property.
Description
Technical field
The present invention relates to a kind of high-barrier nano PA6 nano composite material and preparation method thereof.
Background technology
Nylon is the general designation of polymeric amide, is the extrusion resin that in five large general engineering plastic, output is maximum, kind is maximum, most widely used, over-all properties is the most excellent.In polyamide resin, output and the consumption of nylon 6 and nylon66 fiber are maximum, account for about 90% of total polymeric amide, and nylon mainly has outstanding feature in mechanics, chemistry, thermal property etc.
At present the modification of nylon is mainly concentrated on to the water-intake rate modification or mechanical property modification that reduce nylon, but, be but average in performance in obstruct modification, especially, well do not take into account mechanical property and barrier property to during PA modification.
Summary of the invention
The object of the present invention is to provide a kind of high-barrier nano PA6 nano composite material and preparation method thereof.
The technical solution used in the present invention is:
A kind of high-barrier nano PA6 nano composite material, it is made up of the raw material of following mass parts: the oxidation inhibitor of the obstruct material of PA6,5-20 part of 75-95 part, the toughner of 2-4 part, 0.1-0.3 part; Described obstruct material is preparation like this:
1) hexanolactam is put into reactor, add nano imvite, nano-attapulgite, nano silicon;
2) add sodium hydroxide again, vacuumize, heating, then add TDI, reaction 2-4h;
3) be cooled to room temperature in 30min-2h, open while starting cooling and stir, stop stirring when being cooled to room temperature, discharging.
In step 1), the mass ratio of nano imvite, nano-attapulgite, nano silicon is (20-25): (4-6): 1.
In step 1), the quality of hexanolactam is 1:15-20 with the ratio of the total mass of nano imvite, nano-attapulgite, nano silicon.
The amount ratio of sodium hydroxide and hexanolactam is: 0.7-0.9mol:100ml.
The amount ratio of TDI and hexanolactam is: 0.2-0.4mol:100ml.
Step 2) in, be heated to 140-185 DEG C.
Described toughner comprises ethylene-methyl methacrylate butyl ester-glycidyl acrylate multipolymer, ethylene methyl methacrylate multipolymer, ethylene-methyl acrylate copolymer.
Described oxidation inhibitor comprises phosphite ester kind antioxidant and Hinered phenols antioxidant.
A preparation method for high-barrier nano PA6 nano composite material, comprises the following steps:
1) each raw material is mixed;
2) raw material mixed is placed in forcing machine melt extrudes, granulation.
The invention has the beneficial effects as follows: matrix material of the present invention has good barrier property, meanwhile, the matrix material of gained also has good mechanical property.
Embodiment
A kind of high-barrier nano PA6 nano composite material, it is made up of the raw material of following mass parts: the oxidation inhibitor of the obstruct material of PA6,5-20 part of 75-95 part, the toughner of 2-4 part, 0.1-0.3 part;
Described toughner comprises ethylene-methyl methacrylate butyl ester-glycidyl acrylate multipolymer, ethylene methyl methacrylate multipolymer, ethylene-methyl acrylate copolymer.
Described oxidation inhibitor comprises phosphite ester kind antioxidant and Hinered phenols antioxidant.
Described obstruct material is preparation like this:
1) hexanolactam is put into reactor, add nano imvite, nano-attapulgite, nano silicon;
2) add sodium hydroxide again, vacuumize, heating, then add TDI(Toluene-2,4-diisocyanate, 4-vulcabond), reaction 2-4h;
3) be cooled to room temperature in 30min-2h, open while starting cooling and stir, stop stirring when being cooled to room temperature, discharging.
In step 1), the mass ratio of nano imvite, nano-attapulgite, nano silicon is (20-25): (4-6): 1.
In step 1), the quality of hexanolactam is 1:15-20 with the ratio of the total mass of nano imvite, nano-attapulgite, nano silicon.
The amount ratio of sodium hydroxide and hexanolactam is: 0.7-0.9mol:100ml.
The amount ratio of TDI and hexanolactam is: 0.2-0.4mol:100ml.
Step 2) in, be heated to 140-185 DEG C.
Corresponding, a kind of preparation method of high-barrier nano PA6 nano composite material, comprises the following steps:
1) each raw material is mixed;
2) raw material mixed is placed in forcing machine melt extrudes, granulation.
Below in conjunction with specific embodiment, the present invention is described further:
embodiment 1:
A kind of high-barrier nano PA6 nano composite material, it is made up of the raw material of following mass parts: the PA6 of 80 parts, the obstruct material of 10 parts, the ethylene-methyl methacrylate butyl ester-glycidyl acrylate multipolymer of 3 parts, the antioxidant 1010 of 0.2 part;
Described obstruct material is preparation like this:
1) hexanolactam is put into reactor, add nano imvite, nano-attapulgite, nano silicon;
2) add sodium hydroxide again, vacuumize, be heated to 140 DEG C, then add TDI, reaction 2-4h;
3) be cooled to room temperature (temperature fall time: 1h), open while starting cooling and stir, stop stirring when being cooled to room temperature, discharging.
In step 1), the mass ratio of nano imvite, nano-attapulgite, nano silicon is 20:4:1.
In step 1), the quality of hexanolactam is 1:15 with the ratio of the total mass of nano imvite, nano-attapulgite, nano silicon.
The amount ratio of sodium hydroxide and hexanolactam is: 0.7mol:100ml.
The amount ratio of TDI and hexanolactam is: 0.2mol:100ml.
Corresponding, a kind of preparation method of high-barrier nano PA6 nano composite material, comprises the following steps:
1) each raw material is mixed;
2) raw material mixed is placed in forcing machine melt extrudes, granulation.
embodiment 2:
A kind of high-barrier nano PA6 nano composite material, it is made up of the raw material of following mass parts: the PA6 of 75 parts, the obstruct material of 10 parts, the ethylene methyl methacrylate multipolymer of 2 parts, the antioxidant 1076 of 0.1 part;
Described obstruct material is preparation like this:
1) hexanolactam is put into reactor, add nano imvite, nano-attapulgite, nano silicon;
2) add sodium hydroxide again, vacuumize, be heated to 170 DEG C, then add TDI, reaction 2-4h;
3) be cooled to room temperature (temperature fall time: 1.5h), open while starting cooling and stir, stop stirring when being cooled to room temperature, discharging.
In step 1), the mass ratio of nano imvite, nano-attapulgite, nano silicon is 22:5:1.
In step 1), the quality of hexanolactam is 1:18 with the ratio of the total mass of nano imvite, nano-attapulgite, nano silicon.
The amount ratio of sodium hydroxide and hexanolactam is: 0.8mol:100ml.
The amount ratio of TDI and hexanolactam is: 0.35mol:100ml.
Corresponding, a kind of preparation method of high-barrier nano PA6 nano composite material, comprises the following steps:
1) each raw material is mixed;
2) raw material mixed is placed in forcing machine melt extrudes, granulation.
embodiment 3:
A kind of high-barrier nano PA6 nano composite material, it is made up of the raw material of following mass parts: the PA6 of 95 parts, the obstruct material of 20 parts, the ethylene methyl methacrylate multipolymer of 4 parts, the antioxidant 1076 of 0.3 part;
Described obstruct material is preparation like this:
1) hexanolactam is put into reactor, add nano imvite, nano-attapulgite, nano silicon;
2) add sodium hydroxide again, vacuumize, be heated to 170 DEG C, then add TDI, reaction 2-4h;
3) be cooled to room temperature (temperature fall time: 2h), open while starting cooling and stir, stop stirring when being cooled to room temperature, discharging.
In step 1), the mass ratio of nano imvite, nano-attapulgite, nano silicon is 25:6:1.
In step 1), the quality of hexanolactam is 1:20 with the ratio of the total mass of nano imvite, nano-attapulgite, nano silicon.
The amount ratio of sodium hydroxide and hexanolactam is: 0.9mol:100ml.
The amount ratio of TDI and hexanolactam is: 0.4mol:100ml.
Corresponding, a kind of preparation method of high-barrier nano PA6 nano composite material, comprises the following steps:
1) each raw material is mixed;
2) raw material mixed is placed in forcing machine melt extrudes, granulation.
Matrix material embodiment prepared and blank PA6 contrast, and its result is as following table:
table 1: the performance of matrix material and blank PA6
Note: water vapour permeability is that formula or PA6 are made the film that thickness is 25.4 μm; Water vapour permeability unit: g/m224h38 DEG C 100%RH.
Claims (7)
1. a high-barrier nano PA6 nano composite material, is characterized in that: it is made up of the raw material of following mass parts: the oxidation inhibitor of the obstruct material of PA6,5-20 part of 75-95 part, the toughner of 2-4 part, 0.1-0.3 part; Described obstruct material is preparation like this:
1) hexanolactam is put into reactor, add nano imvite, nano-attapulgite, nano silicon;
2) add sodium hydroxide again, vacuumize, heating, then add TDI, reaction 2-4h;
3) be cooled to room temperature in 30min-2h, open while starting cooling and stir, stop stirring when being cooled to room temperature, discharging; In step 1), the mass ratio of nano imvite, nano-attapulgite, nano silicon is (20-25): (4-6): 1; The quality of hexanolactam is 1:15-20 with the ratio of the total mass of nano imvite, nano-attapulgite, nano silicon.
2. a kind of high-barrier nano PA6 nano composite material according to claim 1, is characterized in that: the amount ratio of sodium hydroxide and hexanolactam is: 0.7-0.9mol:100mL.
3. a kind of high-barrier nano PA6 nano composite material according to claim 1, is characterized in that: the amount ratio of TDI and hexanolactam is: 0.2-0.4mol:100mL.
4. a kind of high-barrier nano PA6 nano composite material according to claim 1, is characterized in that: step 2) in, be heated to 140-185 DEG C.
5. a kind of high-barrier nano PA6 nano composite material according to claim 1, is characterized in that: described toughner comprises ethylene-methyl methacrylate butyl ester-glycidyl acrylate multipolymer, ethylene methyl methacrylate multipolymer, ethylene-methyl acrylate copolymer.
6. a kind of high-barrier nano PA6 nano composite material according to claim 1, is characterized in that: described oxidation inhibitor comprises phosphite ester kind antioxidant and Hinered phenols antioxidant.
7. the preparation method of a kind of high-barrier nano PA6 nano composite material according to claim 1, is characterized in that: comprise the following steps:
1) each raw material is mixed;
2) raw material mixed is placed in forcing machine melt extrudes, granulation.
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| CN201310619265.5A CN103613922B (en) | 2013-11-29 | 2013-11-29 | A kind of high-barrier nano PA6 nano composite material and preparation method thereof |
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| CN201310619265.5A CN103613922B (en) | 2013-11-29 | 2013-11-29 | A kind of high-barrier nano PA6 nano composite material and preparation method thereof |
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| CN103613922B true CN103613922B (en) | 2016-04-20 |
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| CN106009640B (en) * | 2016-06-16 | 2017-12-29 | 青岛万林橡塑科技有限公司 | The preparation method of graphene oxide with high barrier/Nylon Nanocomposite |
| CN113621231A (en) * | 2021-07-01 | 2021-11-09 | 广东奇德新材料股份有限公司 | Barrier polyamide composite material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH0747644B2 (en) * | 1989-05-19 | 1995-05-24 | 宇部興産株式会社 | Polyamide composite material and method for producing the same |
| CN1081207C (en) * | 1997-07-17 | 2002-03-20 | 中国科学院化学研究所 | Nanometer composite polyamide-clay material and its preparation |
| US6136908A (en) * | 1999-06-17 | 2000-10-24 | Industrial Technology Research Institute | Preparation of thermoplastic nanocomposite |
| US6906127B2 (en) * | 2002-08-08 | 2005-06-14 | Amcol International Corporation | Intercalates, exfoliates and concentrates thereof formed with low molecular weight; nylon intercalants polymerized in-situ via ring-opening polymerization |
| CN1212347C (en) * | 2003-06-09 | 2005-07-27 | 杭州鸿雁电器公司 | Parent material containing high organic montmorillonite, and its prepn. method |
| CN1796458A (en) * | 2004-12-28 | 2006-07-05 | 上海杰事杰新材料股份有限公司 | Method for toughening and reinforcing nylon by using new type organic montmorillonite |
| CN100532456C (en) * | 2004-12-29 | 2009-08-26 | 上海杰事杰新材料股份有限公司 | Method for preparing Nano composite material of nylon / clay of laminar silicate |
| CN101362858B (en) * | 2008-09-28 | 2010-09-01 | 华东理工大学 | Magnetic silicate clay/polyamide compound resin |
| CN101768302B (en) * | 2008-12-29 | 2013-03-27 | 上海杰事杰新材料(集团)股份有限公司 | Preparation method of high barrier property polyethylene/nylon 6 in-situ nanocomposite material |
| CN102618024A (en) * | 2012-03-30 | 2012-08-01 | 深圳市科聚新材料有限公司 | Nylon-based nano composite material and preparation method thereof |
| CN103073714B (en) * | 2013-01-17 | 2015-08-12 | 株洲时代新材料科技股份有限公司 | A kind of preparation method of nylon monomer-cast nylon/Nano composite material of montmorillonite |
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Address after: 529000 No. 135 Dongsheng Road, Jianghai District, Guangdong, Jiangmen Applicant after: GUANGDONG QIDE ENGINEERING PLASTIC TECHNOLOGY CO., LTD. Address before: 529000 No. 135 Dongsheng Road, Jianghai hi tech Industrial Zone, Jianghai District, Guangdong, Jiangmen Applicant before: Qide Engineering Plastics Technology Co., Ltd. |
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Denomination of invention: High-barrier nano PA6 composite material and preparation method thereof Effective date of registration: 20170713 Granted publication date: 20160420 Pledgee: Bank of China Limited by Share Ltd Jiangmen branch Pledgor: GUANGDONG QIDE ENGINEERING PLASTIC TECHNOLOGY CO., LTD. Registration number: 2017990000629 |
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Date of cancellation: 20200608 Granted publication date: 20160420 Pledgee: Bank of China Limited by Share Ltd. Jiangmen branch Pledgor: GUANGDONG QIDE ENGINEERING PLASTIC TECHNOLOGY Co.,Ltd. Registration number: 2017990000629 |