CN106479036B - Polyolefin composite material for melt lamination rapid molding and preparation method thereof - Google Patents
Polyolefin composite material for melt lamination rapid molding and preparation method thereof Download PDFInfo
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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Abstract
The invention provides a polyolefin composite material for melt lamination rapid molding and a preparation method thereof, wherein the polyolefin composite material is prepared from 100 parts of a resin matrix, 5-45 parts of nano nitrile rubber, 1-5 parts of a compatilizer, 0.1-0.5 part of an antioxidant, 0.1-0.5 part of a heat stabilizer and 0.5-5 parts of a lubricant. The polyolefin composite material prepared by the invention has the characteristics of high mechanical strength, good wear resistance, high forming speed and the like, and simultaneously, the low temperature resistance of the composite material is greatly improved. In addition, the preparation process of the composite material is simple, and the application of the polyolefin material in the field of rapid molding can be directly promoted.
Description
Technical Field
The invention belongs to the technical field of rapid molding modification of polyolefin composite materials, and particularly relates to a polyolefin composite material applied to the field of melt lamination rapid molding and a preparation method thereof.
Background
The melt extrusion molding is also called melt spinning molding, and is a rapid molding process which takes filamentous materials as raw materials, utilizes heat energy as molding energy and realizes heating and melting of the raw materials. The working principle of the melting extrusion molding comprises the links of heating and melting raw materials by a heating wire controlled by a computer, cooling and molding the raw materials into a thin layer, three-dimensionally moving a workbench and the like, and finally molding the filamentous raw materials into a three-dimensional workpiece with a three-dimensional structure and certain functionality. The rapid forming process is relatively simple in technology, easy to operate, free of toxic substances or gas release in the forming process, and capable of being directly used in environments such as offices and the like.
Common raw materials for melt extrusion molding are engineering plastics, industrial oil wax, synthetic rubber and the like, wherein the engineering plastics are mostly pure resin raw materials, so that the defects exist in the aspects of mechanical strength, environmental tolerance, molding speed and the like, and in addition, a support structure and post-treatment work are needed when a large-scale part is prepared.
Disclosure of Invention
The invention aims to overcome the defects of common raw materials for melt extrusion molding in the aspects of mechanical strength, environmental tolerance, molding speed and the like, and provides a polyolefin composite material for melt lamination rapid molding and a preparation method thereof, wherein the polyolefin composite material has the characteristics of high mechanical strength, high low-temperature impact, good wear resistance, high molding speed and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
a polyolefin composite material for melt lamination rapid molding is prepared from the following components in parts by weight:
100 parts of resin matrix, namely 100 parts of,
5-45 parts of nano nitrile-butadiene rubber,
1-5 parts of a compatilizer,
0.1 to 0.5 part of antioxidant,
0.1 to 0.5 part of heat stabilizer,
0.5-5 parts of a lubricant.
In a further scheme, the resin matrix is homo-polypropylene or polyethylene.
The nanometer nitrile rubber is faint yellow powder with the diameter of 50-100 nm.
The compatilizer is maleic anhydride grafted polypropylene or maleic anhydride grafted polyethylene.
The antioxidant is two of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, tri [2, 4-di-tert-butylphenyl ] phosphite ester or dioctadecyl thiodipropionate.
The heat stabilizer is calcium stearate or barium stearate.
The lubricant is ethylene bis stearamide or pentaerythritol stearate.
It is another object of the present invention to provide a method for preparing the above polyolefin composite, which comprises the steps of:
(1) according to the proportion, 100 parts of resin matrix, 5-45 parts of nano nitrile rubber, 1-5 parts of compatilizer, 0.1-0.5 part of antioxidant, 0.1-0.5 part of heat stabilizer and 0.5-5 parts of lubricant are placed in a high-speed mixer to be dispersed for 10-30 minutes;
(2) and (3) the dispersed raw materials are melted, plasticized, extruded and pulled in an extruder to prepare the polyolefin composite material for melt lamination rapid molding.
And then the prepared polyolefin composite material is formed into a required part through a melt extrusion process.
The polyolefin composite material prepared by the invention has the characteristics of high mechanical strength, good wear resistance, high forming speed and the like, and simultaneously, the low temperature resistance of the composite material is greatly improved. In addition, the preparation process of the polyolefin composite material is simple, and the application of the polyolefin material in the field of rapid molding can be directly promoted.
The invention has the following beneficial effects:
1. the invention takes polypropylene or polyethylene as a matrix, and adopts nano nitrile rubber to modify the matrix, thus preparing the polyolefin composite material which can be used in the field of melt lamination rapid molding.
2. Due to the introduction of the nanometer nitrile rubber, the bulk density of the polyolefin composite material in the melting and molding process is increased, the molding defect is reduced, and the mechanical property of the composite material can be obviously improved;
3. the nano nitrile rubber added into the matrix material can serve as an energy absorption unit when the material is damaged, so that the generation and development of silver streaks are reduced, and the impact performance, especially the low-temperature impact performance, of the composite material can be obviously improved;
4. because the nano-level rubber particles in the nano nitrile rubber are uniformly dispersed in the composite material system, the composite material can provide buffering and energy absorption effects in the friction process, thereby obviously improving the wear resistance of the composite material;
5. the nanometer nitrile rubber can be used as a crystallization point in the cooling and forming process of the polyolefin composite material, so that the solidification and forming of the composite material are accelerated, and the forming speed is greatly improved.
Detailed description of the invention
The present invention will be further described with reference to specific examples, which are not intended to be limiting of the spirit of the invention, and any simple modifications or equivalents thereof based on the spirit of the invention should fall within the scope of the invention as claimed.
After conditioning the samples prepared in the examples in an environment of 23 ℃ and 50% humidity, the flexural strength, low temperature impact strength and abrasion resistance of the composite material were measured using ASTM D790, ASTM D6110 and ASTM D1242, respectively, and the speed of melt extrusion molding thereof was recorded.
The specific embodiment of the invention is as follows:
example 1
(1) Preparing raw materials according to the following proportion:
100 parts of homopolymerized polypropylene resin matrix,
5 parts of nano nitrile-butadiene rubber,
1 part of compatilizer maleic anhydride grafted polypropylene,
0.04 part of antioxidant tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester,
0.06 part of antioxidant tris [ 2.4-di-tert-butylphenyl ] phosphite,
0.1 part of calcium stearate serving as a heat stabilizer,
0.5 part of lubricant ethylene bis stearamide.
Uniformly mixing the materials, and then placing the mixture into a high-speed mixer for dispersing for 10 minutes;
(2) and (3) the dispersed raw materials are melted, plasticized, extruded and pulled in an extruder to prepare the polyolefin composite material for melt lamination rapid molding.
(3) And (3) forming the prepared polyolefin composite material into a required workpiece through a melt extrusion process, and detecting the performance of the workpiece.
The properties of the prepared nano nitrile rubber modified polypropylene composite material are shown in the table I.
Example 2
(1) Preparing raw materials according to the following proportion:
100 parts of homopolymerized polypropylene resin matrix,
15 parts of nano nitrile-butadiene rubber,
2 parts of compatilizer maleic anhydride grafted polypropylene,
0.08 part of antioxidant tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester,
0.12 part of antioxidant tris [ 2.4-di-tert-butylphenyl ] phosphite,
0.2 part of calcium stearate serving as a heat stabilizer,
lubricant ethylene bis stearamide 1.5 parts.
Uniformly mixing the materials, and then placing the mixture in a high-speed mixer for dispersing for 15 minutes;
(2) and (3) the dispersed raw materials pass through an extruder, and the raw materials are subjected to melting, plasticizing, extruding and traction to prepare the polyolefin composite material for melt lamination rapid molding.
(3) And (3) forming the prepared polyolefin composite material into a required workpiece through a melt extrusion process, and detecting the performance.
The properties of the prepared nano nitrile rubber modified polypropylene composite material are shown in the table I.
Example 3
(1) Preparing raw materials according to the following proportion:
100 parts of homopolymerized polypropylene resin matrix,
25 parts of nano nitrile-butadiene rubber,
3 parts of compatilizer maleic anhydride grafted polypropylene,
0.12 part of antioxidant tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester,
0.18 part of antioxidant tris [ 2.4-di-tert-butylphenyl ] phosphite,
0.3 part of calcium stearate serving as a heat stabilizer,
2.5 parts of lubricant ethylene bis stearamide.
Uniformly mixing the materials, and then placing the mixture into a high-speed mixer for dispersing for 20 minutes;
(2) and (3) the dispersed raw materials pass through an extruder, and the raw materials are subjected to melting, plasticizing, extruding and traction to prepare the polyolefin composite material for melt lamination rapid molding.
(3) And (3) forming the prepared polyolefin composite material into a required workpiece through a melt extrusion process, and detecting the performance.
The properties of the prepared nano nitrile rubber modified polypropylene composite material are shown in the table I.
Example 4
(1) Preparing raw materials according to the following proportion:
100 parts of homopolymerized polypropylene resin matrix,
35 parts of nano nitrile-butadiene rubber,
4 parts of compatilizer maleic anhydride grafted polypropylene,
0.16 part of antioxidant tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester,
0.24 part of antioxidant tris [ 2.4-di-tert-butylphenyl ] phosphite,
0.4 part of calcium stearate serving as a heat stabilizer,
3.5 parts of lubricant ethylene bis stearamide.
Uniformly mixing the materials, and then placing the mixture in a high-speed mixer for dispersing for 25 minutes;
(2) and (3) the dispersed raw materials pass through an extruder, and the raw materials are subjected to melting, plasticizing, extruding and traction to prepare the polyolefin composite material for melt lamination rapid molding.
(3) And (3) forming the prepared polyolefin composite material into a required workpiece through a melt extrusion process, and detecting the performance.
The properties of the prepared nano nitrile rubber modified polypropylene composite material are shown in the table I.
Example 5
(1) Preparing raw materials according to the following proportion:
100 parts of homopolymerized polypropylene resin matrix,
45 parts of nano nitrile-butadiene rubber,
5 parts of compatilizer maleic anhydride grafted polypropylene,
0.2 part of antioxidant tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester,
0.3 part of antioxidant tris [ 2.4-di-tert-butylphenyl ] phosphite,
0.5 part of calcium stearate serving as a heat stabilizer,
5 parts of lubricant ethylene bis stearamide.
Uniformly mixing the materials, and then placing the mixture into a high-speed mixer for dispersing for 30 minutes;
(2) and (3) the dispersed raw materials pass through an extruder, and the raw materials are subjected to melting, plasticizing, extruding and traction to prepare the polyolefin composite material for melt lamination rapid molding.
(3) And (3) forming the prepared polyolefin composite material into a required workpiece through a melt extrusion process, and detecting the performance.
The properties of the prepared nano nitrile rubber modified polypropylene composite material are shown in the table I.
Example 6
(1) Preparing raw materials according to the following proportion:
100 parts of polyethylene resin matrix, wherein the polyethylene resin matrix comprises 100 parts of polyethylene resin,
5 parts of nano nitrile-butadiene rubber,
1 part of compatilizer maleic anhydride grafted polyethylene,
0.04 part of antioxidant tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester,
0.06 part of antioxidant dioctadecyl thiodipropionate,
0.1 part of barium stearate serving as a heat stabilizer,
0.5 part of lubricant pentaerythritol stearate.
Uniformly mixing the materials, and then placing the mixture into a high-speed mixer for dispersing for 10 minutes;
(2) and (3) the dispersed raw materials pass through an extruder, and the raw materials are subjected to melting, plasticizing, extruding and traction to prepare the polyolefin composite material for melt lamination rapid molding.
(3) And (3) forming the prepared polyolefin composite material into a required workpiece through a melt extrusion process, and detecting the performance.
The properties of the prepared nanometer nitrile rubber modified polyethylene composite material are shown in the table I.
Example 7
(1) Preparing raw materials according to the following proportion:
100 parts of polyethylene resin matrix, wherein the polyethylene resin matrix comprises 100 parts of polyethylene resin,
15 parts of nano nitrile-butadiene rubber,
2 parts of compatilizer maleic anhydride grafted polyethylene,
0.08 part of antioxidant tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester,
0.12 part of antioxidant dioctadecyl thiodipropionate,
0.2 part of barium stearate serving as a heat stabilizer,
1.5 parts of lubricant pentaerythritol stearate.
Uniformly mixing the materials, and then placing the mixture in a high-speed mixer for dispersing for 15 minutes;
(2) and (3) the dispersed raw materials pass through an extruder, and the raw materials are subjected to melting, plasticizing, extruding and traction to prepare the polyolefin composite material for melt lamination rapid molding.
(3) And (3) forming the prepared polyolefin composite material into a required workpiece through a melt extrusion process, and detecting the performance.
The properties of the prepared nanometer nitrile rubber modified polyethylene composite material are shown in the table I.
Example 8
(1) Preparing raw materials according to the following proportion:
100 parts of polyethylene resin matrix, wherein the polyethylene resin matrix comprises 100 parts of polyethylene resin,
25 parts of nano nitrile-butadiene rubber,
3 parts of compatilizer maleic anhydride grafted polyethylene,
0.12 part of antioxidant tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester,
0.18 part of antioxidant dioctadecyl thiodipropionate,
0.3 part of barium stearate serving as a heat stabilizer,
2.5 parts of lubricant pentaerythritol stearate.
Uniformly mixing the materials, and then placing the mixture into a high-speed mixer for dispersing for 20 minutes;
(2) and (3) the dispersed raw materials pass through an extruder, and the raw materials are subjected to melting, plasticizing, extruding and traction to prepare the polyolefin composite material for melt lamination rapid molding.
(3) And (3) forming the prepared polyolefin composite material into a required workpiece through a melt extrusion process, and detecting the performance.
The properties of the prepared nanometer nitrile rubber modified polyethylene composite material are shown in the table I.
Example 9
(1) Preparing raw materials according to the following proportion:
100 parts of polyethylene resin matrix, wherein the polyethylene resin matrix comprises 100 parts of polyethylene resin,
35 parts of nano nitrile-butadiene rubber,
4 parts of compatilizer maleic anhydride grafted polyethylene,
0.16 part of antioxidant tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester,
0.24 part of antioxidant dioctadecyl thiodipropionate,
0.4 part of barium stearate serving as a heat stabilizer,
3.5 parts of lubricant pentaerythritol stearate.
Uniformly mixing the materials, and then placing the mixture in a high-speed mixer for dispersing for 25 minutes;
(2) and (3) the dispersed raw materials pass through an extruder, and the raw materials are subjected to melting, plasticizing, extruding and traction to prepare the polyolefin composite material for melt lamination rapid molding.
(3) And (3) forming the prepared polyolefin composite material into a required workpiece through a melt extrusion process, and detecting the performance.
The properties of the prepared nanometer nitrile rubber modified polyethylene composite material are shown in the table I.
Example 10
(1) Preparing raw materials according to the following proportion:
100 parts of polyethylene resin matrix, wherein the polyethylene resin matrix comprises 100 parts of polyethylene resin,
45 parts of nano nitrile-butadiene rubber,
5 parts of compatilizer maleic anhydride grafted polyethylene,
0.2 part of antioxidant tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester,
0.3 part of antioxidant dioctadecyl thiodipropionate,
0.5 part of barium stearate serving as a heat stabilizer,
5 parts of lubricant pentaerythritol stearate.
Uniformly mixing the materials, and then placing the mixture into a high-speed mixer for dispersing for 30 minutes;
(2) and (3) the dispersed raw materials pass through an extruder, and the raw materials are subjected to melting, plasticizing, extruding and traction to prepare the polyolefin composite material for melt lamination rapid molding.
(3) And (3) forming the prepared polyolefin composite material into a required workpiece through a melt extrusion process, and detecting the performance.
The properties of the prepared nanometer nitrile rubber modified polyethylene composite material are shown in the table I.
Comparative example 1
(1) Preparing raw materials according to the following proportion:
100 parts of homopolymerized polypropylene resin matrix,
0.04 part of antioxidant tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester,
0.06 part of antioxidant tris [ 2.4-di-tert-butylphenyl ] phosphite,
0.1 part of calcium stearate serving as a heat stabilizer,
0.5 part of lubricant ethylene bis stearamide.
Uniformly mixing the materials, and then placing the mixture into a high-speed mixer for dispersing for 10 minutes;
(2) and (3) the dispersed raw materials pass through an extruder, and the raw materials are subjected to melting, plasticizing, extruding and traction to prepare the polyolefin composite material for melt lamination rapid molding.
(3) And (3) forming the prepared polyolefin composite material into a required workpiece through a melt extrusion process, and detecting the performance.
The properties of the prepared polypropylene composite material are shown in the table I.
Comparative example 2
(1) Preparing raw materials according to the following proportion:
100 parts of polyethylene resin matrix, wherein the polyethylene resin matrix comprises 100 parts of polyethylene resin,
0.04 part of antioxidant tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester,
0.06 part of antioxidant dioctadecyl thiodipropionate,
0.1 part of barium stearate serving as a heat stabilizer,
0.5 part of lubricant pentaerythritol stearate.
Uniformly mixing the materials, and then placing the mixture into a high-speed mixer for dispersing for 10 minutes;
(2) and (3) the dispersed raw materials pass through an extruder, and the raw materials are subjected to melting, plasticizing, extruding and traction to prepare the polyolefin composite material for melt lamination rapid molding.
(3) And (3) forming the prepared polyolefin composite material into a required workpiece through a melt extrusion process, and detecting the performance of the workpiece.
The properties of the prepared polyethylene composite material are shown in the table I.
Table one:
| performance of | Flexural Strength (MPa) | Impact Strength (KJ/m)2 -20℃） | Taber abrasion (mg/1000 times) | Speed of formation (cm)3/h) |
| Example 1 | 42 | 7.9 | 62 | 39 |
| Example 2 | 44 | 8.1 | 61 | 41 |
| Example 3 | 56 | 8.2 | 60 | 42 |
| Example 4 | 48 | 8.5 | 58 | 44 |
| Example 5 | 47 | 8.3 | 59 | 43 |
| Example 6 | 29 | 4.8 | 69 | 33 |
| Example 7 | 30 | 5.1 | 67 | 34 |
| Example 8 | 33 | 5.4 | 64 | 38 |
| Example 9 | 32 | 5.3 | 65 | 37 |
| Example 10 | 31 | 5.1 | 66 | 35 |
| Comparative example 1 | 35 | 5.1 | 95 | 28 |
| Comparative example 2 | 24 | 3.2 | 100 | 26 |
From the data in Table one, it can be seen that comparative examples 1-5 and comparative example 1: after the polyolefin composite material prepared by the invention is molded into a product by a melt extrusion process, the bending strength is up to 48MPa, and is improved by 37.1 percent compared with that before modification (comparative example 1); maximum low temperature impact strength8.5Kj/m2The yield is improved by 66.7 percent compared with that before modification; the Taber abrasion is 58mg/100 times at least, and is reduced by 38.9 percent compared with that before modification; the forming speed is 44cm at the maximum3The improvement is 57.1 percent compared with the improvement before modification.
As can be seen from comparative examples 6-10 and comparative example 2: after the polyolefin composite material prepared by the invention is molded into a product by a melt extrusion process, the bending strength is at most 33MPa, and is improved by 37.5 percent compared with that before modification (comparative example 2); the maximum low-temperature impact strength is 5.4Kj/m2The improvement is 68.8 percent compared with the improvement before modification; the minimum Taber abrasion is 64mg/100 times, which is reduced by 36.0 percent compared with that before modification; the forming speed is 38cm at the highest3The improvement is 46.2 percent compared with the improvement before modification.
In addition, the preparation process is simple, and can directly promote the application of the polyolefin material in the field of rapid molding.
The embodiments described above are intended to facilitate one of ordinary skill in the art in understanding and using the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (5)
1. A polyolefin composite for melt lamination rapid prototyping characterized in that: the composition is prepared from the following components in parts by weight:
100 parts of resin matrix, namely 100 parts of,
5-45 parts of nano nitrile-butadiene rubber,
1-5 parts of a compatilizer,
0.1 to 0.5 part of antioxidant,
0.1 to 0.5 part of heat stabilizer,
1.5-5 parts of a lubricant;
the resin matrix is homopolymerized polypropylene or polyethylene;
the nanometer nitrile rubber is light yellow powdery particles with the diameter of 50-100 nm;
the lubricant is ethylene bis stearamide or pentaerythritol stearate.
2. Polyolefin composite according to claim 1, characterized in that: the compatilizer is maleic anhydride grafted polypropylene or maleic anhydride grafted polyethylene.
3. Polyolefin composite according to claim 1, characterized in that: the antioxidant is two of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, tri [2, 4-di-tert-butylphenyl ] phosphite ester or dioctadecyl thiodipropionate.
4. Polyolefin composite according to claim 1, characterized in that: the heat stabilizer is calcium stearate or barium stearate.
5. A method of preparing the polyolefin composite of claim 1, wherein: comprises the following steps:
(1) according to the proportion, 100 parts of resin matrix, 5-45 parts of nano nitrile rubber, 1-5 parts of compatilizer, 0.1-0.5 part of antioxidant, 0.1-0.5 part of heat stabilizer and 1.5-5 parts of lubricant are placed in a high-speed mixer to be dispersed for 10-30 minutes;
(2) and (3) the dispersed raw materials are melted, plasticized, extruded and pulled in an extruder to prepare the polyolefin composite material for melt lamination rapid molding.
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| CN109134993A (en) * | 2017-06-16 | 2019-01-04 | 合肥杰事杰新材料股份有限公司 | A kind of wear-resistant polyolefin composite material and preparation method for rapid shaping |
| CN107857936A (en) * | 2017-11-19 | 2018-03-30 | 王秋林 | PP, PE, BR tertiary blending formula |
| CN110066439A (en) * | 2018-01-23 | 2019-07-30 | 合肥杰事杰新材料股份有限公司 | A kind of antiwear heat resisting composite polyolefine material and preparation method thereof |
| CN116041832A (en) * | 2023-02-28 | 2023-05-02 | 江苏惠升管业集团有限公司 | POE grafted GMA and application method thereof in polyethylene gas pipe |
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