CN104693789A - Flogopite and glass fiber compound filled PA6 reinforcing material and preparation method thereof - Google Patents
Flogopite and glass fiber compound filled PA6 reinforcing material and preparation method thereof Download PDFInfo
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- CN104693789A CN104693789A CN201510096850.0A CN201510096850A CN104693789A CN 104693789 A CN104693789 A CN 104693789A CN 201510096850 A CN201510096850 A CN 201510096850A CN 104693789 A CN104693789 A CN 104693789A
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- glass fibre
- phlogopite
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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
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- 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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention relates to the technical field of macromolecules and provides a flogopite and glass fiber compound filled PA6 reinforcing material and a preparation method thereof. The material is prepared from the following raw materials in percentage by weight: 60-70% of PA6, 18-22% of flogopite, 10-12% of glass fibers, 1-5% of a flexibilizer POE grafted maleic anhydride, 0.1-1% of an antioxidant, 0.1-1% of a lubricant and 0.4% of a coupling agent. The PA6 material is compound-filled by using flogopite and glass fibers. Flogopite powder is added based on the glass fiber reinforced PA6, so that the defects that single glass fiber reinforced PA6 is inconsistent in shrinking percentage, poor in dimensional stability, easy to warp, poor in weather resistance, poor in glossiness and the like are overcome. The material is good in mechanical property, low in cost, excellent in thermal stability, excellent in dimensional stability, good in surface glossiness, ultra-strong anti-ultraviolet property and the like, and the application range of the PA6 reinforcing material in indoor products is expanded.
Description
Technical field
The present invention relates to technical field of polymer materials, particularly relate to the preparation method of the composite filled PA6 strongthener material of a kind of phlogopite glass fibre.
Background technology
Nowadays glass fiber enhanced nylon matrix material is being widely used with its outstanding mechanical property, excellent its on structural part, but increasing outdoor outward appearance is held concurrently, structural part starts to be applied, so just need to develop some intensity, outward appearance, weathering resistance can deal with the market requirement by balanced material, usually we can adopt PA to add fibre or PP to add fibre and make, but it is unstable that PA adds fiber material size, surface floating fiber is seriously difficult to accomplish light, improve weathering resistance to need to add expensive weather resisting agent, thus cost remains high, PP adds fiber material under the prerequisite ensureing surface aesthetic, improve physical strength difficulty, and thermotolerance is poor.So market is low to cost all the time, appearance looks elegant, the material that mechanical property of holding concurrently is high has high demand.
Summary of the invention
In view of this, the object of the invention is to, PA6 strongthener material providing a kind of phlogopite glass fibre composite filled and preparation method thereof, this PA6 strongthener material over-all properties is outstanding.
For solving the problems of the technologies described above, the object of the invention is to be achieved through the following technical solutions:
The present invention relates to and provides the composite filled PA6 strongthener of a kind of phlogopite glass fibre, its raw material comprised and each raw materials quality per-cent as follows:
Wherein, described PA6 is the BL3280H of Hunan Ba Ling petrochemical industry, and viscosity is 2.75.
Wherein, described phlogopite is the HY-M1 of extra large powder spreading body, particle diameter 16-18um, whiteness 70.Described phlogopite through titanate coupling agent (ethanol: coupling agent=3:1 dilution), need carry out surface treatment in 5 ~ 10 minutes 75 DEG C of high-speed mixer and mixing.
Wherein, described glass fibre is the 988A glass fibre of Chinese megalith.
Wherein, described toughner is homemade POE grafted maleic anhydride, and percentage of grafting is 1.5% ~ 2.0%
Wherein, described oxidation inhibitor is N; N'-is two-(3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (1098) and phosphonous acid three (2,4 di-tert-butyl-phenyl ester) (168) composite by 1:1.
Wherein, described lubricant is the two fat fatty acid amide TAF of ethylene.
The present invention has following beneficial effect: the present invention is based on PA and add fine superelevation mechanical property, the phlogopite breeze adding low cost is filled, the outstanding weathering resistance of phlogopite powder is also made while significantly reducing costs, thermotolerance, surface luster, outward appearance is beautiful to be shown on material fully, thus obtains aly can making up part vacancy market requiring material to this kind.
Embodiment
The present invention relates to the PA6 strongthener that a kind of phlogopite glass fibre is composite filled, its raw material comprised and each raw materials quality % proportioning as follows: PA660-70%; Phlogopite 18-22%; Glass fibre 10-12%, toughner 1-5%; Oxidation inhibitor 0.1-1%; Lubricant 0.1-1%, coupling agent 0.4%.
In above-mentioned formula, PA6 is the BL3280H of Hunan Ba Ling petrochemical industry, and viscosity is 2.75.Phlogopite is the HY-M1 of extra large powder spreading body, particle diameter 16-18um, whiteness 70.Described phlogopite through titanate coupling agent (ethanol: coupling agent=3:1 dilution), need carry out surface treatment in 5 ~ 10 minutes 75 DEG C of high-speed mixer and mixing.Described glass fibre is the 988A glass fibre of Chinese megalith.Described toughner is self-control POE grafted maleic anhydride, and percentage of grafting is 1.5% ~ 2.0%.Described oxidation inhibitor be N, N'-two-(168) 1:1 is composite for (3-(3,5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine (1098) and phosphonous acid three (2,4 di-tert-butyl-phenyl ester).Lubricant is the two fat fatty acid amide TAF of ethylene.
In the present embodiment technical scheme, select PA6 (i.e. nylon 6) as starting material, it is after micro-fiberglass reinforced, and mechanical property and thermotolerance can significantly improve, thus improves thermotolerance and the mechanical property of material; In addition, owing to employing treated phlogopite in material, compare other and fill class breeze, cost is low, and improve obviously the weathering resistance of material and thermotolerance, surface gloss is high, also has good enhancement to the intensity of material; 3rd, the toughner POE grafted maleic anhydride due to materials'use, well improves the toughness of material; 4th, the long glass fibres due to materials'use, the effective intensity promoting PA6 resin, because add-on is few, so do not affect the outward appearance of material.
In addition, the embodiment of the present invention additionally provides the preparation method of the composite filled PA6 strongthener of above-mentioned phlogopite glass fibre, comprises the steps:
(1) each raw material is taken according to the quality % proportioning of the composite filled PA6 strongthener raw material of phlogopite glass fibre as described in any one of claim 1-7;
(2) by the PA6 taken, the phlogopite processed, and toughner, oxidation inhibitor, lubricant, in moderate-speed mixers, 5-10 minute is mixed;
(3) mixed raw material and described glass fibre are placed in twin screw extruder blending, through melt extruding, granulation.The processing parameter of described twin screw extruder is: twin screw extruder one district temperature is 220-250 DEG C, two district's temperature are 220-250 DEG C, three district's temperature are 220-250 DEG C, four district's temperature are 220-250 DEG C, five district's temperature 230 DEG C, six district's temperature 230 DEG C, seven district's temperature 230 DEG C, eight district's temperature 260 DEG C compounds time of delivery in screw rod is 1-2 minute.
Below in conjunction with specific embodiment, the present invention is explained in detail:
Embodiment 1
Get the raw materials ready by following component proportion: PA674%; Phlogopite 10%; Glass fibre 10%, toughner POE grafted maleic anhydride 5%; Oxidation inhibitor 0.4%; Lubricant 0.2%, coupling agent 0.4%.Wherein glass fibre adds fine mouth by position, side and adds, and is then that 220-250 DEG C of twin screw extruder is extruded through melt temperature, granulation.
Wherein each zone temperatures is: 220 DEG C, a district, two 230 DEG C, districts, three 250 DEG C, districts, four 250 DEG C, districts, five 230 DEG C, districts, six 230 DEG C, districts, seven 230 DEG C, districts, and eight 260 DEG C, districts, the residence time was 90 seconds.
Embodiment 2
Get the raw materials ready by following component proportion: PA669%; Phlogopite 15%; Glass fibre 10%, toughner POE grafted maleic anhydride 5%; Oxidation inhibitor 0.4%; Lubricant 0.2%, coupling agent 0.4%.Wherein glass fibre adds fine mouth by position, side and adds, and is then that 220-250 DEG C of twin screw extruder is extruded through melt temperature, granulation.
Wherein each zone temperatures is: 220 DEG C, a district, two 230 DEG C, districts, three 250 DEG C, districts, four 250 DEG C, districts, five 230 DEG C, districts, six 230 DEG C, districts, seven 230 DEG C, districts, and eight 260 DEG C, districts, the residence time was 90 seconds.
Embodiment 3
Get the raw materials ready by following component proportion: PA664%; Phlogopite 20%; Glass fibre 10%, toughner POE grafted maleic anhydride 5%; Oxidation inhibitor 0.4%; Lubricant 0.2%, coupling agent 0.4%.Wherein glass fibre adds fine mouth by position, side and adds, and is then that 220-250 DEG C of twin screw extruder is extruded through melt temperature, granulation.
Wherein each zone temperatures is: 220 DEG C, a district, two 230 DEG C, districts, three 250 DEG C, districts, four 250 DEG C, districts, five 230 DEG C, districts, six 230 DEG C, districts, seven 230 DEG C, districts, and eight 260 DEG C, districts, the residence time was 90 seconds.
Embodiment 4
Get the raw materials ready by following component proportion: PA659%; Phlogopite 25%; Glass fibre 10%, toughner POE grafted maleic anhydride 5%; Oxidation inhibitor 0.4%; Lubricant 0.2%, coupling agent 0.4%.Wherein glass fibre adds fine mouth by position, side and adds, and is then that 220-250 DEG C of twin screw extruder is extruded through melt temperature, granulation.
Wherein each zone temperatures is: 220 DEG C, a district, two 230 DEG C, districts, three 250 DEG C, districts, four 250 DEG C, districts, five 230 DEG C, districts, six 230 DEG C, districts, seven 230 DEG C, districts, and eight 260 DEG C, districts, the residence time was 90 seconds.
Performance test and the standard of implementation:
Above-mentioned 4 embodiments are completed particle dry 4-6 hour in the convection oven of 80-100 DEG C of granulation, then by the injection moulding sample preparation on 80T injection moulding machine of the particle of drying, in sample making course, keep mould temperature between 70-100 DEG C.
Tensile strength is tested by GB/T 1040 standard, specimen types is I type, batten size (mm): 170 (length) × (20 ± 0.2) (end portion width) × (4 ± 0.2) (thickness), draw speed is 50mm/min;
Flexural strength and modulus in flexure are tested by GB 9341/T standard.Specimen types is specimen size (mm): (80 ± 2) × (10 ± 0.2) × (4 ± 0.2), and rate of bending is 20mm/min;
Notched Izod impact strength is tested by GB/T 1043 standard, and specimen types is I type, specimen size (mm): (80 ± 2) × (10 ± 0.2) × (4 ± 0.2); Breach type is category-A, and breach residual thickness is 3.2mm;
Embodiment 1 ~ 4 formula and performance are in table 1:
Table 1
| Embodiment | 1 | 2 | 3 | 4 |
| PA6 | 74 | 69 | 64 | 59 |
| Glass fibre | 10 | 10 | 10 | 10 |
| Phlogopite powder | 10 | 15 | 20 | 25 |
| Toughner | 5 | 5 | 5 | 5 |
| Coupling agent | 0.4 | 0.4 | 0.4 | 0.4 |
| Oxidation inhibitor | 0.4 | 0.4 | 0.4 | 0.4 |
| Lubricant | 0.2 | 0.2 | 0.2 | 0.2 |
| Notched Izod impact strength | 120 | 102 | 88 | 54 |
| Tensile strength | 90 | 96 | 101 | 103 |
| Elongation | 1.0 | 2.5 | 1.8 | 3.1 |
| Flexural strength | 123 | 131 | 140 | 143 |
| Modulus in flexure | 3520 | 3710 | 4030 | 4130 |
Can find out from above table, in the PA6 strongthener that described phlogopite glass fibre is composite filled, along with the content of phlogopite improves constantly, the mechanical property of material also improves thereupon, this substantially increases the tensile strength of material, flexural strength and surface hardness, and surface gloss change not quite and more and more light, but more add along with phlogopite, material also can become more and more crisp, after adding 25% phlogopite, material is very crisp, is no longer applicable to doing appearance component.So comprehensive, add 20% phlogopite and 10% the enhancing PA6 mechanics of materials effect of glass fibre be best.
Above composite filled PA6 strongthener of a kind of phlogopite glass fibre provided by the present invention and preparation method thereof is described in detail, apply specific case herein to set forth principle of the present invention and embodiment, the explanation of above embodiment just understands method of the present invention and core concept thereof for helping; Meanwhile, for one of ordinary skill in the art, according to thought of the present invention, all will change in specific embodiments and applications, in sum, this description should not be construed as limitation of the present invention.
Claims (9)
1. the PA6 strongthener that phlogopite glass fibre is composite filled, is characterized in that, its raw material comprised and each raw materials quality per-cent as follows:
2. the PA6 strongthener that phlogopite glass fibre as claimed in claim 1 is composite filled, it is characterized in that, described PA6 is the BL3280H of Hunan Ba Ling petrochemical industry, and viscosity is 2.75.
3. the PA6 strongthener that phlogopite glass fibre as claimed in claim 1 is composite filled, it is characterized in that, described phlogopite is the HY-M1 of extra large powder spreading body, particle diameter 16-18um, whiteness is 70, and described phlogopite carries out surface treatment in 5 ~ 10 minutes through titanate coupling agent 75 DEG C of high-speed mixer and mixing.
4. the PA6 strongthener that phlogopite glass fibre as claimed in claim 1 is composite filled, it is characterized in that, described glass fibre is the 988A glass fibre of Chinese megalith.
5. the PA6 strongthener that phlogopite glass fibre as claimed in claim 1 is composite filled, is characterized in that, described toughner is self-control POE grafted maleic anhydride, and percentage of grafting is 1.5 ~ 2.0%.
6. the PA6 strongthener that phlogopite glass fibre as claimed in claim 1 is composite filled; it is characterized in that; described oxidation inhibitor is N; N'-pair-(3-(3; 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine and phosphonous acid three (2,4 di-tert-butyl-phenyl ester) composite by 1:1.
7. the PA6 strongthener that phlogopite glass fibre as claimed in claim 1 is composite filled, is characterized in that, described lubricant is the two fat fatty acid amide TAF of ethylene.
8. a preparation method for the PA6 strongthener that phlogopite glass fibre is composite filled, is characterized in that, comprise the steps:
(1) each raw material is taken according to the quality % proportioning of the composite filled PA6 strongthener raw material of phlogopite glass fibre as described in any one of claim 1-7;
(2) by the PA6 taken, the phlogopite processed, and toughner, oxidation inhibitor, lubricant, in moderate-speed mixers, 5-10 minute is mixed;
(3) mixed raw material and described glass fibre are placed in twin screw extruder blending, through melt extruding, granulation.
9. the preparation method of the PA6 strongthener that phlogopite glass fibre is composite filled as claimed in claim 8, it is characterized in that, the processing parameter of described twin screw extruder is: twin screw extruder one district temperature is 220-250 DEG C, two district's temperature are 220-250 DEG C, and three district's temperature are 220-250 DEG C, and four district's temperature are 220-250 DEG C, five district's temperature 230 DEG C, six district's temperature 230 DEG C, seven district's temperature 230 DEG C, eight district's temperature 260 DEG C compounds time of delivery in screw rod is 1-2 minute.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510096850.0A CN104693789A (en) | 2015-03-04 | 2015-03-04 | Flogopite and glass fiber compound filled PA6 reinforcing material and preparation method thereof |
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| CN201510096850.0A CN104693789A (en) | 2015-03-04 | 2015-03-04 | Flogopite and glass fiber compound filled PA6 reinforcing material and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109722015A (en) * | 2019-01-14 | 2019-05-07 | 江西集银科技有限公司 | Suspended casting suspended basket lightweight material and load-bearing backing plate based on lightweight material |
| CN110079079A (en) * | 2019-05-17 | 2019-08-02 | 天津长芦海晶集团有限公司 | Mine fibre composite reinforced modified nylon material and preparation method thereof for automobile central appliance terminal box |
| WO2021128964A1 (en) * | 2019-12-24 | 2021-07-01 | 上海中镭新材料科技有限公司 | Electroplated nylon material and preparation method thereof |
| CN113248908A (en) * | 2021-04-26 | 2021-08-13 | 宁波普立隆高分子材料有限公司 | Modified nylon material for wind generating set and preparation method thereof |
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| CN1970629A (en) * | 2005-11-26 | 2007-05-30 | 东丽纤维研究所（中国）有限公司 | High-performance resin/ mica composite material and its production method |
| CN101875781A (en) * | 2010-03-31 | 2010-11-03 | 深圳市科聚新材料有限公司 | High-toughness low-shrink polyamide material and preparation method thereof |
| CN103333488A (en) * | 2013-06-26 | 2013-10-02 | 江苏启蓝新材料有限公司 | Toughened nylon alloy and preparation method thereof |
| CN104151578A (en) * | 2014-08-19 | 2014-11-19 | 南通瑞隆新材料有限公司 | Preparation method of enhanced flame-retardant nylon PA6 modified engineering plastic |
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2015
- 2015-03-04 CN CN201510096850.0A patent/CN104693789A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1970629A (en) * | 2005-11-26 | 2007-05-30 | 东丽纤维研究所（中国）有限公司 | High-performance resin/ mica composite material and its production method |
| CN101875781A (en) * | 2010-03-31 | 2010-11-03 | 深圳市科聚新材料有限公司 | High-toughness low-shrink polyamide material and preparation method thereof |
| CN103333488A (en) * | 2013-06-26 | 2013-10-02 | 江苏启蓝新材料有限公司 | Toughened nylon alloy and preparation method thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109722015A (en) * | 2019-01-14 | 2019-05-07 | 江西集银科技有限公司 | Suspended casting suspended basket lightweight material and load-bearing backing plate based on lightweight material |
| CN110079079A (en) * | 2019-05-17 | 2019-08-02 | 天津长芦海晶集团有限公司 | Mine fibre composite reinforced modified nylon material and preparation method thereof for automobile central appliance terminal box |
| WO2021128964A1 (en) * | 2019-12-24 | 2021-07-01 | 上海中镭新材料科技有限公司 | Electroplated nylon material and preparation method thereof |
| CN113248908A (en) * | 2021-04-26 | 2021-08-13 | 宁波普立隆高分子材料有限公司 | Modified nylon material for wind generating set and preparation method thereof |
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Application publication date: 20150610 |