CN103613922A - High-barrier nano PA6 composite material and preparation method thereof - Google Patents
High-barrier nano PA6 composite material and preparation method thereof Download PDFInfo
- Publication number
- CN103613922A CN103613922A CN201310619265.5A CN201310619265A CN103613922A CN 103613922 A CN103613922 A CN 103613922A CN 201310619265 A CN201310619265 A CN 201310619265A CN 103613922 A CN103613922 A CN 103613922A
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- nano
- barrier
- composite material
- hexanolactam
- material according
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- 238000002360 preparation method Methods 0.000 title claims description 16
- 239000002131 composite material Substances 0.000 title abstract 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- 239000000463 material Substances 0.000 claims abstract description 36
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 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 12
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 7
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000007599 discharging Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 239000002114 nanocomposite Substances 0.000 claims description 22
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- 239000003112 inhibitor Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 230000003647 oxidation Effects 0.000 claims description 6
- 238000007254 oxidation reaction Methods 0.000 claims description 6
- 229920001897 terpolymer Polymers 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
- 230000004888 barrier function Effects 0.000 abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 abstract 1
- 229910052901 montmorillonite Inorganic materials 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229920002292 Nylon 6 Polymers 0.000 description 22
- 230000004048 modification Effects 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 239000004677 Nylon Substances 0.000 description 4
- 239000011159 matrix material 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
- 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
-
- 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
Abstract
The invention discloses a high-barrier nano PA6 composite material which is prepared from the following raw materials in parts by mass: 75-95 parts of PA6, 5-20 parts of barrier material, 2-4 parts of flexibilizer, and 0.1-0.3 part of an antioxidant, wherein the barrier material is prepared through the following steps: 1) placing caprolactam in a reaction kettle, and adding nano montmorillonite, nano attapulgite and nano silicon dioxide into the reaction kettle; 2) adding sodium hydroxide into the reaction kettle, vacuumizing the reaction kettle, heating the reaction kettle, adding TDI into the reaction kettle, and reacting the obtained object 2-4 h; 3) cooling the reacted product to room temperature within 30 min-2 h, simultaneously beginning to cool and stir, stopping stirring while the reacted product is cooled to room temperature, and discharging the obtained product. The composite material disclosed by the invention has good barrier properties and good mechanical properties.
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 best.In polyamide resin, the output of nylon 6 and nylon 66 and consumption are maximum, account for 90% left and right of total polymeric amide, and nylon mainly has outstanding feature at aspects such as mechanics, chemistry, thermal properties.
At present the modification of nylon is mainly concentrated on to water-intake rate modification or the mechanical property modification that reduces nylon, yet, being but average in performance aspect obstruct modification, especially, during to PA modification, well do not take into account mechanical property and barrier property.
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 high-barrier nano PA6 nano composite material, its raw material by following mass parts forms: the oxidation inhibitor of the obstruct material of the PA6 of 75-95 part, 5-20 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 again sodium hydroxide, vacuumize, heating, then add TDI, reaction 2-4h;
3) in 30min-2h, be cooled to room temperature, when starting cooling, open and stir, while being cooled to room temperature, stop stirring 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 ℃.
Described toughner comprises ethylene-methyl methacrylate butyl ester-glycidyl acrylate multipolymer, ethylene-methyl methacrylate methyl terpolymer, 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 mixing is placed in to 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 high-barrier nano PA6 nano composite material, its raw material by following mass parts forms: the oxidation inhibitor of the obstruct material of the PA6 of 75-95 part, 5-20 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 methyl terpolymer, 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 again sodium hydroxide, vacuumize, heating, then add TDI(Toluene-2,4-diisocyanate, 4-vulcabond), reaction 2-4h;
3) in 30min-2h, be cooled to room temperature, when starting cooling, open and stir, while being cooled to room temperature, stop stirring 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 ℃.
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 mixing is placed in to forcing machine melt extrudes, granulation.
Below in conjunction with specific embodiment, the present invention is described further:
embodiment 1:
A high-barrier nano PA6 nano composite material, its raw material by following mass parts forms: the PA6 of 80 parts, the obstruct material of 10 parts, 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 again sodium hydroxide, vacuumize, be heated to 140 ℃, then add TDI, reaction 2-4h;
3) be cooled to room temperature (temperature fall time: 1h), open and stir when starting cooling, stop stirring discharging while being cooled to room temperature.
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 mixing is placed in to forcing machine melt extrudes, granulation.
embodiment 2:
A high-barrier nano PA6 nano composite material, its raw material by following mass parts forms: the PA6 of 75 parts, the obstruct material of 10 parts, the ethylene-methyl methacrylate methyl terpolymer 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 again sodium hydroxide, vacuumize, be heated to 170 ℃, then add TDI, reaction 2-4h;
3) be cooled to room temperature (temperature fall time: 1.5h), open and stir when starting cooling, stop stirring discharging while being cooled to room temperature.
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 mixing is placed in to forcing machine melt extrudes, granulation.
embodiment 3:
A high-barrier nano PA6 nano composite material, its raw material by following mass parts forms: the PA6 of 95 parts, the obstruct material of 20 parts, the ethylene-methyl methacrylate methyl terpolymer 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 again sodium hydroxide, vacuumize, be heated to 170 ℃, then add TDI, reaction 2-4h;
3) be cooled to room temperature (temperature fall time: 2h), open and stir when starting cooling, stop stirring discharging while being cooled to room temperature.
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 mixing is placed in to forcing machine melt extrudes, granulation.
Matrix material prepared by embodiment 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 to the film that thickness is 25.4 μ m; Water vapour permeability unit: g/m224h38 ℃ 100%RH.
Claims (9)
1. a high-barrier nano PA6 nano composite material, is characterized in that: its raw material by following mass parts forms: the oxidation inhibitor of the obstruct material of the PA6 of 75-95 part, 5-20 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 again sodium hydroxide, vacuumize, heating, then add TDI, reaction 2-4h;
3) in 30min-2h, be cooled to room temperature, when starting cooling, open and stir, while being cooled to room temperature, stop stirring discharging.
2. a kind of high-barrier nano PA6 nano composite material according to claim 1, is characterized in that: in step 1), the mass ratio of nano imvite, nano-attapulgite, nano silicon is (20-25): (4-6): 1.
3. a kind of high-barrier nano PA6 nano composite material according to claim 1, is characterized in that: 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.
4. 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.
5. 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.
6. 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 ℃.
7. 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 methyl terpolymer, ethylene-methyl acrylate copolymer.
8. 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.
9. the preparation method of a kind of high-barrier nano PA6 nano composite material claimed in claim 1, is characterized in that: comprise the following steps:
1) each raw material is mixed;
2) raw material mixing is placed in to forcing machine melt extrudes, granulation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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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| Publication Number | Publication Date |
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| CN103613922A true CN103613922A (en) | 2014-03-05 |
| CN103613922B CN103613922B (en) | 2016-04-20 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106009640A (en) * | 2016-06-16 | 2016-10-12 | 青岛万林橡塑科技有限公司 | Preparation method of graphene oxide and polyamide nanocomposite material with high barrier property |
| 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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| 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 | Publication date |
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| CN103613922B (en) | 2016-04-20 |
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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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