CN115895237A - Supercritical foaming composite material and preparation method thereof - Google Patents

Supercritical foaming composite material and preparation method thereof Download PDF

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Publication number
CN115895237A
CN115895237A CN202310022790.2A CN202310022790A CN115895237A CN 115895237 A CN115895237 A CN 115895237A CN 202310022790 A CN202310022790 A CN 202310022790A CN 115895237 A CN115895237 A CN 115895237A
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parts
composite material
foaming
supercritical
composite
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邵亮
邬明杰
杨艳龙
马春燕
马建中
姬占有
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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Abstract

A supercritical foaming composite material and its preparation method, thermoplastic polyurethane elastomer 70-90; 5-15 parts of polytetrafluoroethylene powder; 5-15 parts of rice straw fiber; 0.5-1.5 parts; the preparation method comprises the following steps: melting and blending the thermoplastic polyurethane elastomer, the polytetrafluoroethylene powder, the rice straw fibers and the nucleating agent by using a double-screw extruder, and extruding and granulating to obtain a uniformly mixed composite material; injection molding the prepared composite material by using an injection molding machine; foaming the prepared composite material by using a supercritical foaming device to obtain a supercritical foaming composite material; the supercritical foaming composite material obtained by the invention has the characteristics of simple preparation process, light weight, high cell density, uniform cells, small average pore size, good foaming effect and excellent mechanical property.

Description

Supercritical foaming composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of preparation of microcellular foamed plastics, and particularly relates to a supercritical foamed composite material and a preparation method thereof.
Background
Thermoplastic polyurethane elastomer TPU foamed materials have good sound insulation, heat insulation and electrical insulation properties, excellent cushioning properties and good strength, and are therefore widely used in the fields of automobiles, biomedical materials, shoes, electrical packaging, sporting goods, structural materials, building applications and the like.
At present, the preparation of thermoplastic polyurethane elastomer TPU foaming materials is mainly divided into chemical foaming and physical foaming, wherein the chemical foaming takes azo substances as foaming agents, so that the foaming materials of independent foams are formed. But the defects are that the consumption of the foaming agent is large, the foaming agent cannot be recycled, harmful gas is generated in the foaming process, chemical residues exist, and the harm degree to the environment and human bodies is large; the processing is complex and the requirement on equipment is high. The physical foaming method is generally carried out by using a foaming agent such as butane or a hydrofluorocarbon.
As a novel physical foaming mode, supercritical fluid foaming is carried out, wherein foaming agents comprise carbon dioxide and nitrogen; because of cleanness, environmental protection, no pollution and low cost, the polyurethane foam is gradually and widely applied to material foaming.
However, the thermoplastic polyurethane elastomer TPU supercritical foaming material used at present has the following defects:
1) The material has poor foaming effect, uneven cell distribution and larger size;
2) The material has small foaming multiplying power and large shrinkage ratio;
3) After foaming, the strength of the material is greatly reduced, the mechanical property is poor, and the comprehensive use performance of the material is influenced.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide the supercritical foaming composite material and the preparation method thereof, and the supercritical foaming composite material has the characteristics of simple preparation process, light weight, high cell density, uniform cells, small average pore size, good foaming effect and excellent mechanical property.
In order to achieve the purpose, the invention adopts the technical scheme that:
a supercritical foaming composite material comprises the following components in parts by weight:
70-90 parts of a thermoplastic polyurethane elastomer;
5-15 parts of polytetrafluoroethylene powder;
5-15 parts of rice straw fiber;
0.5-1.5 parts of nucleating agent.
The nucleating agent is nano silicon dioxide.
The polytetrafluoroethylene powder has a size of 450-500 μm and a specific gravity of 2.12-2.16g/cm 3 Apparent density of 0.45-0.52g/cm 3 。
The rice straw fiber is fiber after alkali treatment, and the size of the rice straw fiber is 40-60 mu m.
A preparation method of a supercritical foaming composite material comprises the following steps:
1) 70-90 parts of thermoplastic polyurethane elastomer; 5-15 parts of polytetrafluoroethylene powder; 5-15 parts of rice straw fiber; adding 0.5-1.5 parts of nucleating agent into a double-screw extruder, and carrying out melt blending, extrusion and granulation on the mixture to prepare composite beads;
2) Adding the composite beads into an injection molding machine, melting, injecting and molding the mixed material, and cutting the mixed material into composite sheets;
3) Placing the composite sheet prepared in the step 2) in an oven at 80 ℃ for 4 hours, removing water, placing the dried composite sheet in a supercritical foaming kettle, introducing carbon dioxide gas, stopping gas input when the carbon dioxide gas in the supercritical foaming kettle reaches a saturated pressure, and setting the pressure maintaining time and the foaming temperature; and (3) after carbon dioxide in the composite material is saturated, quickly releasing carbon dioxide gas in the kettle to foam the composite sheet, thus obtaining the supercritical foaming composite material.
In the step 1), the temperature of each section in the double-screw extruder is set as follows: the conveying section is 165 ℃, the melting section is 170 ℃, the mixing section is 170 ℃, the homogenizing section is 175 ℃ and the die orifice is 170 ℃.
In the step 2), the section temperatures in the injection molding machine are respectively set as follows: the conveying section is 165 ℃, the melting section is 170 ℃ and the glue injection opening is 175 ℃.
In the step 3), the pressure of carbon dioxide gas in the supercritical foaming kettle is 10-12MPa, the pressure maintaining time is 2-4h, and the foaming temperature is 90-110 ℃.
Compared with the prior art, the invention has the following advantages and beneficial effects:
the TPU/PTFE/RSF supercritical foaming composite material is prepared by adopting a mechanical blending method which is convenient for industrial production, and has the characteristics of light weight, high cell density, uniform cells, small average pore size, good foaming effect and excellent mechanical property. The preparation method adopted by the invention is simple and effective, has low cost and simple process, and can be suitable for large-scale industrial production.
Drawings
FIG. 1 is a SEM photograph of example 4 of the present invention.
FIG. 2 is a SEM photograph of inventive example 5.
FIG. 3 is an SEM photograph of inventive example 6.
Detailed Description
The present invention will be described in detail with reference to specific examples.
The invention relates to a supercritical foaming composite material which comprises the following components in parts by weight:
70-90 parts of thermoplastic polyurethane elastomer TPU,
5-15 parts of polytetrafluoroethylene powder PTFE,
5-15 parts of rice straw fiber RSF,
0.5-1.5 parts of nucleating agent.
The nucleating agent is nano silicon dioxide.
The polytetrafluoroethylene powder has a size of 450-500 μm and a specific gravity of 2.12-2.16g/cm 3 Apparent density of 0.45-0.52g/cm 3 。
The rice straw fiber is fiber after alkali treatment, and the size of the rice straw fiber is 40-60 mu m.
A preparation method of a supercritical foaming composite material comprises the following steps:
1) Adding thermoplastic polyurethane elastomer TPU beads, polytetrafluoroethylene powder PTFE powder, rice straw fiber RSF and a nucleating agent into a charging barrel of a double-screw extruder through a hopper, melting and blending the mixture, extruding and granulating, and compounding the beads;
2) Adding the composite beads into an injection molding machine, melting and injecting the mixed material for molding, and cutting the mixed material into sheets with certain specifications;
3) Placing the prepared composite sheet in an oven at 80 ℃ for 4 hours to remove water in the material, then placing the dried composite sheet in a supercritical foaming kettle, introducing carbon dioxide gas, stopping gas input when the carbon dioxide gas in the kettle reaches the saturated pressure, and setting the pressure maintaining time and the foaming temperature; and (3) after carbon dioxide in the composite material is saturated, quickly releasing carbon dioxide in the kettle to foam the composite sheet, and obtaining the TPU/PTFE/RSF supercritical foaming composite material.
Example 1
A supercritical foaming composite material comprises the following components in parts by weight:
80 parts of a thermoplastic polyurethane elastomer;
15 parts of polytetrafluoroethylene powder; the polytetrafluoroethylene powder has a size of 500 μm and a specific gravity of 2.16g/cm 3 Apparent density of 0.52g/cm 3 ；
5 parts of rice straw fiber; the rice straw fiber is alkali-treated fiber, and the size of the rice straw fiber is 60 mu m;
0.5 part of nucleating agent; the nucleating agent is nano silicon dioxide.
The composite foaming material has the characteristics of low density, large cell density, small average pore size, uniform cells, moderate hardness, good buffering performance and excellent mechanical property. The preparation method adopted by the invention is simple and effective, has low cost and simple process and can be suitable for large-scale industrial production.
Example 2
A supercritical foaming composite material comprises the following components in parts by weight:
90 parts of thermoplastic polyurethane elastomer;
15 parts of polytetrafluoroethylene powder; the polytetrafluoroethylene powder has a size of 500 μm and a specific gravity of 2.16g/cm 3 Apparent density of 0.52g/cm 3 ；
15 parts of rice straw fiber; the rice straw fiber is the fiber after alkali treatment, and the size of the rice straw fiber is 50 mu m;
1.5 parts of nucleating agent, wherein the nucleating agent is nano silicon dioxide.
The composite foaming material has the characteristics of low density, uniform cell size, small average pore size, high tensile strength and excellent mechanical property. The preparation method adopted by the invention is simple and effective, has low cost and simple process and can be suitable for large-scale industrial production.
Example 3
A supercritical foaming composite material comprises the following components in parts by weight:
70 parts of thermoplastic polyurethane elastomer;
5 parts of polytetrafluoroethylene powder; the polytetrafluoroethylene powder has a size of 450 μm and a specific gravity of 2.14g/cm 3 Apparent density of 0.49g/cm 3 ；
5 parts of rice straw fiber; the rice straw fiber is alkali-treated fiber, and the size of the rice straw fiber is 60 mu m;
1.0 part of nucleating agent; the nucleating agent is nano silicon dioxide.
The composite foaming material has the characteristics of large cell density, uniform cells, small average pore size, good rebound resilience, good buffering effect and the like. The preparation method adopted by the invention is simple and effective, has low cost and simple process and can be suitable for large-scale industrial production.
Example 4
A supercritical foamed composite comprising the steps of:
1) Adding 80 parts of thermoplastic polyurethane elastomer (TPU), 15 parts of polytetrafluoroethylene Powder (PTFE), 5 parts of Rice Straw Fiber (RSF) and 0.5 part of nano silicon dioxide into a charging barrel of a double-screw extruder through a hopper, and carrying out melt blending, extrusion and granulation on the mixture to prepare composite beads;
2) Adding the composite beads into a charging barrel of an injection molding machine through a hopper, melting and injecting the mixed material for molding, and cutting the mixed material into sheets with the size of 5 multiplied by 1 multiplied by 0.2 cm;
3) Placing the prepared composite sheet in an oven at 80 ℃ for 4 hours, removing water in the material, then placing the dried composite sheet in a supercritical foaming kettle, introducing carbon dioxide gas, stopping gas input when the carbon dioxide gas in the kettle reaches the saturated pressure, and setting the pressure maintaining time and the foaming temperature; and (3) after carbon dioxide in the composite material is saturated, quickly releasing carbon dioxide gas in the kettle to foam the composite sheet, thus obtaining the supercritical foaming composite material.
Wherein: in the step 1), the temperature of each section in the twin-screw extruder is set as follows: the conveying section is 165 ℃, the melting section is 170 ℃, the mixing section is 170 ℃, the homogenizing section is 175 ℃ and the die orifice is 170 ℃;
in the step 2), the section temperatures in the injection molding machine are respectively set as follows: the conveying section is 165 ℃, the melting section is 170 ℃ and the glue injection opening is 175 ℃;
in the step 3), the saturation pressure of carbon dioxide in the high-pressure kettle is 10MPa, the saturation time is 3h, and the foaming temperature is 100 ℃.
The TPU/PTFE/RSF supercritical foaming composite material prepared by the equipment and the process parameters provided by the invention has the density of 0.274g/cm 3 The cells had an average diameter of 7.31 μm and a cell density of 1.68X 10 12 cell/cm 3 Hardness (Shore A) was 84, tensile strength was 24.91MPa, and FIG. 1 is a view showing the structure of cells thereof.
Example 5
A preparation method of a supercritical foaming composite material comprises the following steps:
1) Adding 80 parts of thermoplastic polyurethane elastomer (TPU), 10 parts of polytetrafluoroethylene Powder (PTFE), 10 parts of Rice Straw Fiber (RSF) and 1 part of nano silicon dioxide into a charging barrel of a double-screw extruder through a hopper, and carrying out melt blending, extrusion and granulation on the mixture to prepare composite beads;
2) Adding the composite beads into a charging barrel of an injection molding machine through a hopper, melting and injecting the mixed material for molding, and cutting the mixed material into sheets with the size of 5 multiplied by 1 multiplied by 0.2 cm;
3) Placing the prepared composite sheet in an oven at 80 ℃ for 4 hours to remove water in the material, then placing the dried composite sheet in a supercritical foaming kettle, introducing carbon dioxide gas, stopping gas input when the carbon dioxide gas in the kettle reaches the saturated pressure, and setting the pressure maintaining time and the foaming temperature; and (3) after carbon dioxide in the composite material is saturated, quickly releasing carbon dioxide in the kettle to foam the composite sheet, and obtaining the TPU/PTFE/RSF supercritical foaming composite material.
Wherein:
in the step 1), the temperature of each section in the twin-screw extruder is set as follows: the conveying section is 165 ℃, the melting section is 170 ℃, the mixing section is 170 ℃, the homogenizing section is 175 ℃ and the die orifice is 170 ℃.
In the step 2), the section temperatures in the injection molding machine are respectively set as: the conveying section is 165 ℃, the melting section is 170 ℃ and the glue injection opening is 175 ℃.
In the step 3), the saturation pressure of carbon dioxide in the high-pressure kettle is 11 MPa, the saturation time is 3h, and the foaming temperature is 100 ℃.
The TPU/PTFE/RSF supercritical foaming composite material prepared by the equipment and the process parameters provided by the invention has the density of 0.222g/cm 3 The cells had an average diameter of 6.18 μm and a cell density of 2.16X 10 12 cell/cm 3 Hardness (Shore A) was 86 and tensile strength was 28.14MPa, and FIG. 2 is a view showing a structure of cells thereof.
Example 6
A preparation method of a supercritical foaming composite material comprises the following steps:
1) Adding 70 parts of thermoplastic polyurethane elastomer (TPU), 15 parts of polytetrafluoroethylene Powder (PTFE), 15 parts of Rice Straw Fiber (RSF) and 1 part of nano silicon dioxide into a charging barrel of a double-screw extruder through a hopper, and carrying out melt blending, extrusion and granulation on the mixture to prepare composite beads;
2) Adding the composite beads into a charging barrel of an injection molding machine through a hopper, melting and injecting the mixed material for molding, and cutting the mixed material into sheets with the size of 5 multiplied by 1 multiplied by 0.2 cm;
3) Placing the prepared composite sheet in an oven at 80 ℃ for 4 hours to remove water in the material, then placing the dried composite sheet in a supercritical foaming kettle, introducing carbon dioxide gas, stopping gas input when the carbon dioxide gas in the kettle reaches the saturated pressure, and setting the pressure maintaining time and the foaming temperature; and (3) after carbon dioxide in the composite material is saturated, quickly releasing carbon dioxide in the kettle to foam the composite sheet, and obtaining the TPU/PTFE/RSF supercritical foaming composite material.
Wherein: in the step 1), the temperature of each section in the twin-screw extruder is set as follows: the conveying section is 165 ℃, the melting section is 170 ℃, the mixing section is 170 ℃, the homogenizing section is 175 ℃ and the die orifice is 170 ℃;
in the step 2), the section temperatures in the injection molding machine are respectively set as: the conveying section is 165 ℃, the melting section is 170 ℃ and the glue injection port is 175 ℃.
In the step 3), the saturation pressure of carbon dioxide in the high-pressure kettle is 12MPa, the saturation time is 4h, and the foaming temperature is 100 ℃.
The TPU/PTFE/RSF supercritical foaming composite material prepared by the equipment and the process parameters provided by the invention has the density of 0.344g/cm 3 The cells had an average diameter of 7.02 μm and a cell density of 3.47X 10 12 cell/cm 3 The hardness (Shore A) was 87, the tensile strength was 31.87 MPa, and FIG. 3 is a view showing the structure of cells thereof.
Example 7
A preparation method of a supercritical foaming composite material comprises the following steps:
1) Adding 90 parts of thermoplastic polyurethane elastomer (TPU), 15 parts of polytetrafluoroethylene Powder (PTFE), 15 parts of Rice Straw Fiber (RSF) and 1.5 parts of nano silicon dioxide into a charging barrel of a double-screw extruder through a hopper, and carrying out melt blending, extrusion and granulation on the mixture to prepare composite beads;
2) Adding the composite beads into a charging barrel of an injection molding machine through a hopper, melting and injecting the mixed material for molding, and cutting the mixed material into sheets with the size of 5 multiplied by 1 multiplied by 0.2 cm;
3) Placing the prepared composite sheet in an oven at 80 ℃ for 4 hours to remove water in the material, then placing the dried composite sheet in a supercritical foaming kettle, introducing carbon dioxide gas, stopping gas input when the carbon dioxide gas in the kettle reaches the saturated pressure, and setting the pressure maintaining time and the foaming temperature; and (3) after carbon dioxide in the composite material is saturated, quickly releasing carbon dioxide in the kettle to foam the composite sheet, and obtaining the TPU/PTFE/RSF supercritical foaming composite material.
Wherein: in the step 1), the temperature of each section in the twin-screw extruder is set as follows: the conveying section is 165 ℃, the melting section is 170 ℃, the mixing section is 170 ℃, the homogenizing section is 175 ℃ and the die orifice is 170 ℃;
in the step 2), the section temperatures in the injection molding machine are respectively set as: the conveying section is 165 ℃, the melting section is 170 ℃ and the glue injection opening is 175 ℃.
In the step 3), the saturation pressure of carbon dioxide gas in the autoclave is 11 MPa, the saturation time is 2h, and the foaming temperature is 90 ℃.
The composite foaming material has the characteristics of small density, large cell density, small average pore size, moderate hardness and excellent tensile strength. The preparation method adopted by the invention is simple and effective, has low cost and simple process, and can be suitable for large-scale industrial production.
Example 8
A preparation method of a supercritical foaming composite material comprises the following steps:
1) Adding 70 parts of thermoplastic polyurethane elastomer TPU, 5 parts of polytetrafluoroethylene powder PTFE, 5 parts of rice straw fiber RSF and 1.0 part of nano silicon dioxide into a double-screw extruder charging barrel through a hopper, and carrying out melt blending, extrusion and granulation on the mixture to prepare composite beads;
2) Adding the composite beads into a charging barrel of an injection molding machine through a hopper, melting and injecting the mixed material, and cutting the mixed material into sheets with the size of 5 multiplied by 1 multiplied by 0.2 cm;
3) Placing the prepared composite sheet in an oven at 80 ℃ for 4 hours to remove water in the material, then placing the dried composite sheet in a supercritical foaming kettle, introducing carbon dioxide gas, stopping gas input when the carbon dioxide gas in the kettle reaches the saturated pressure, and setting the pressure maintaining time and the foaming temperature; and (3) after carbon dioxide in the composite material is saturated, quickly releasing carbon dioxide in the kettle to foam the composite sheet, and obtaining the TPU/PTFE/RSF supercritical foaming composite material.
Wherein: in the step 1), the temperature of each section in the twin-screw extruder is set as follows: the conveying section is 165 ℃, the melting section is 170 ℃, the mixing section is 170 ℃, the homogenizing section is 175 ℃ and the die orifice is 170 ℃;
in step 2), the section temperatures in the injection molding machine are respectively set as: the conveying section is 165 ℃, the melting section is 170 ℃ and the glue injection port is 175 ℃.
In the step 3), the saturation pressure of carbon dioxide in the high-pressure kettle is 12MPa, the saturation time is 4h, and the foaming temperature is 110 ℃.
The composite foaming material has the characteristics of light weight, uniform foam pores, small average pore size, good foaming effect and excellent performances in various aspects. The preparation method adopted by the invention is simple and effective, has low cost and simple process, and can be suitable for large-scale industrial production.

Claims (8)

1. The supercritical foaming composite material is characterized by comprising the following components in parts by weight:
70-90 parts of a thermoplastic polyurethane elastomer;
5-15 parts of polytetrafluoroethylene powder;
5-15 parts of rice straw fiber;
0.5-1.5 parts of nucleating agent.
2. The supercritical foamed composite of claim 1 wherein the nucleating agent is nanosilica.
3. The supercritical foamed composite according to claim 1, wherein the polytetrafluoroethylene powder has a size of 450 to 500 μm and a specific gravity of 2.12 to 2.16g/cm 3 Apparent density of 0.45-0.52g/cm 3 。
4. The supercritical foamed composite material according to claim 1, wherein the rice straw fiber is an alkali-treated fiber with a size of 40-60 μm.
5. The preparation method of the supercritical foaming composite material is characterized by comprising the following steps:
1) 70-90 parts of a thermoplastic polyurethane elastomer; 5-15 parts of polytetrafluoroethylene powder; 5-15 parts of rice straw fiber; adding 0.5-1.5 parts of nucleating agent into a double-screw extruder, and carrying out melt blending, extrusion and granulation on the mixture to prepare composite beads;
2) Adding the composite beads into an injection molding machine, melting and injecting the mixed material for molding, and cutting the mixed material into composite sheets;
3) Placing the composite sheet prepared in the step 2) in an oven at 80 ℃ for 4 hours, removing water, placing the dried composite sheet in a supercritical foaming kettle, introducing carbon dioxide gas, stopping gas input when the carbon dioxide gas in the supercritical foaming kettle reaches a saturated pressure, and setting the pressure maintaining time and the foaming temperature; and (3) after carbon dioxide in the composite material is saturated, quickly releasing carbon dioxide gas in the kettle to foam the composite sheet, thus obtaining the supercritical foaming composite material.
6. The method for preparing a supercritical foaming composite material according to the claim 3, wherein in the step 1), the temperature of each section in the twin-screw extruder is set as follows: the conveying section is 165 ℃, the melting section is 170 ℃, the mixing section is 170 ℃, the homogenizing section is 175 ℃ and the die orifice is 170 ℃.
7. The method for preparing a supercritical foaming composite material according to claim 3, wherein in the step 2), the section temperatures in the injection molding machine are respectively set as follows: the conveying section is 165 ℃, the melting section is 170 ℃ and the glue injection opening is 175 ℃.
8. The method for preparing a supercritical foaming composite material according to claim 3, wherein in the step 3), the pressure of the carbon dioxide gas in the supercritical foaming kettle is 10-12MPa, the dwell time is 2-4h, and the foaming temperature is 90-110 ℃.
CN202310022790.2A 2023-01-08 2023-01-08 Supercritical foaming composite material and preparation method thereof Pending CN115895237A (en)

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CN115895237A true CN115895237A (en) 2023-04-04

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