CN113667296A - Heat-resistant anti-aging high polymer material and preparation method thereof - Google Patents
Heat-resistant anti-aging high polymer material and preparation method thereof Download PDFInfo
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- CN113667296A CN113667296A CN202111002580.4A CN202111002580A CN113667296A CN 113667296 A CN113667296 A CN 113667296A CN 202111002580 A CN202111002580 A CN 202111002580A CN 113667296 A CN113667296 A CN 113667296A
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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
- 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
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
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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
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/24—Crystallisation aids
Abstract
The invention discloses a heat-resistant anti-aging high polymer material and a preparation method thereof, belonging to the field of vehicle high polymer materials, wherein the high polymer material comprises the following raw materials: the polyamide resin composite nuclear flow agent comprises linoleic acid, sodium benzoate, sodium carboxymethylcellulose and talcum powder, the prepared high polymer material polyamide has high fluidity, can be used for preparing products in a wider processing range, and meanwhile, the prepared products have high temperature resistance and ageing resistance.
Description
Technical Field
The invention relates to the technical field of vehicle high polymer materials, in particular to a heat-resistant anti-aging high polymer material and a preparation method thereof.
Background
Polyamide is a generic name for thermoplastic resins having a repeating amide group- [ NHCO ] -in the molecular main chain, and includes aliphatic polyamides, aliphatic-aromatic polyamides and aromatic polyamides. The aliphatic polyamide has many varieties, high yield and wide application. With the development of automobiles, new challenges are posed to materials for automobiles, and polyamide has become an alternative material for new automobiles due to its excellent properties.
In order to reduce the weight of high-voltage components and the required installation space, flame-retardant plastics are indispensable materials, so that the special polyamide material with aging resistance and high flame retardance can obviously improve the safety of automobiles, but on the basis of keeping the safety performance of automobiles, the light-weight production of the automobiles is an important direction. In automobile parts, many are made of plastic materials, but the plastic materials have poorer flame retardance and high temperature resistance compared with metal materials, so that the key point is how to effectively improve the flame retardance and the high temperature resistance of the plastic materials, for example, polyamide foam has the characteristics of light weight and noise reduction, and the cells of the polyamide foam are round and have higher rigidity, so that the polyamide foam is a substitute material for aluminum and metal in structural parts or materials used for insulators, pipes, gaskets, electric vehicle battery boxes and other light parts.
The invention patent with the application number of '201610441678.2', a flame-retardant high-temperature-resistant modified nylon material for automobile plastics, adopts the added inorganic filler A, inorganic filler B and polyurethane-graphene composite light foam filler, effectively reduces the density of the nylon material, has excellent noise reduction and heat insulation effects, and can improve the physical properties such as wear resistance, tensile strength and the like of the nylon material, but the nylon material for special parts is only obviously deficient in the physical properties, for example, the nylon material in an engine compartment needs to have high-temperature resistance and aging resistance and high-temperature stability, and needs to keep high fluidity in addition, thereby being beneficial to preparation in a wide processing range.
Disclosure of Invention
In view of the above, the present invention provides a heat-resistant and anti-aging polymer material and a preparation method thereof, wherein the polymer material polyamide has high fluidity, and can be used for preparing products in a wide processing range, and the prepared products have high temperature resistance and aging resistance.
The invention solves the technical problems by the following technical means:
a heat-resistant anti-aging high polymer material comprises the following raw materials: polyamide resin, mineral filler, fiber, a composite nuclear flow agent, peroxybenzoic acid, Fischer-Tropsch wax and an antioxidant, wherein the composite nuclear flow agent consists of linoleic acid, sodium benzoate, sodium carboxymethylcellulose and talcum powder.
The polyamide resin can be selected from one or more of PA6, PA66 and PA 11.
Further, the mineral filler is selected from one of kaolin, mica, wollastonite and calcium carbonate.
Further, the fiber is selected from one of carbon fiber and glass fiber.
Further, the raw materials comprise the following components in parts by weight: 100-200 parts of polyamide resin, 4-10 parts of mineral filler, 2-6 parts of fiber, 0.5-2 parts of composite nuclear flow agent, 5-8 parts of peroxybenzoic acid, 3-5 parts of Fischer-Tropsch wax and 0.2-1 part of antioxidant.
Further, the mass ratio of the linoleic acid to the sodium benzoate to the sodium carboxymethyl cellulose to the talcum powder is 0.8: 1: 1: 0.1.
furthermore, the particle size of the mineral filler is less than or equal to 5 micrometers, the purity is greater than or equal to 95%, and the length of the fiber is less than or equal to 0.5 cm.
The invention also discloses a preparation method of the heat-resistant anti-aging high polymer material, which comprises the following steps:
(1) adding polyamide resin, mineral filler, composite nuclear flow agent, peroxybenzoic acid, Fischer-Tropsch wax and antioxidant into a high-speed mixer, and uniformly mixing to obtain a mixture;
(2) placing the obtained mixture in a double screw machine at the rotation speed of 200-300rpm, heating to 230 ℃ at 220-275 ℃, adding fibers, heating again to 260-275 ℃, and then cooling to 250 ℃ at 220-250 ℃ for extrusion granulation to obtain the polymer material.
Further, the high polymer material is prepared into the vehicle product by injection or injection molding, and when the vehicle product is used, the injection temperature is 220-.
Further, the preparation method of the composite nuclear flow agent comprises the following steps:
(1) mixing talcum powder and water according to the weight ratio of 1: 50 to prepare a suspension system;
(2) sodium benzoate and sodium carboxymethyl cellulose were mixed according to a ratio of 1: 1, then heating to 60-70 ℃, adding linoleic acid, stirring at 300-400rpm for 3-4h, and performing ultrasonic separation for 10min to obtain the composite nuclear flow agent. The emulsified composite nucleating agent and the polyamide resin are easier to be mixed evenly in high-speed stirring, and the polyamide resin is easier to be modified in a high-temperature double-screw machine.
Has the advantages that:
the invention adopts the composite nuclear flow agent modified polyamide to prepare the high polymer material, has the characteristics of heat resistance, ageing resistance and high strength, and can be used as the material of the engine compartment or other products needing high temperature ageing resistance. Meanwhile, the high polymer material has high fluidity, is easier to fill a cavity, is not easy to generate defects such as material shortage or dissolution marks and the like, has higher yield, can ensure that the high polymer material can produce products in a wider processing range of 220-.
Drawings
FIG. 1: the polymer material prepared in example 3 was injection molded.
Detailed Description
The present invention will be described in detail with reference to specific examples below:
example 1:
weighing the following raw materials by mass: 100g of polyamide resin, 4g of kaolin, 2g of carbon fiber, 0.5g of composite nuclear flow agent, 5g of peroxybenzoic acid, 3g of Fischer-Tropsch wax and 0.2g of antioxidant. The prepared composite nuclear flow agent comprises linoleic acid, sodium benzoate, sodium carboxymethyl cellulose and talcum powder, and the mass ratio of the prepared composite nuclear flow agent to the sodium carboxymethyl cellulose is 0.8: 1: 1: 0.1. the mineral filler is powder kaolin with the particle size of less than or equal to 5 microns and the purity of more than or equal to 95 percent, and the length of the carbon fiber is less than or equal to 0.5 cm.
Firstly, preparing a composite nuclear flow agent:
(1) mixing talcum powder and water according to the weight ratio of 1: 50, and uniformly stirring to prepare a suspension system;
(2) sodium benzoate and sodium carboxymethyl cellulose were mixed according to a ratio of 1: 1, stirring to dissolve, heating to 65 ℃, adding linoleic acid, stirring for 3.5 hours at the speed of 350rpm, and then ultrasonically dispersing for 10 minutes by using 25KHz ultrasonic waves to obtain the composite nuclear flow agent.
The compound nuclear flow agent is used immediately after the preparation is finished, and is preferably stored in a dark place and in a room. After standing for a long time, the powder needs to be dispersed again before use.
Preparing a composite high polymer material:
(1) adding PA6 polyamide resin, kaolin, a composite nuclear flow agent, peroxybenzoic acid, Fischer-Tropsch wax and an antioxidant into a high-speed mixer, and uniformly mixing to obtain a mixture;
(2) placing the obtained mixture in a double screw machine, wherein the rotating speed is 250rpm, heating the heating zone to 220-.
Example 2:
weighing the following raw materials by mass: 150g of polyamide resin, 6g of kaolin, 4g of glass fiber, 1g of composite nuclear flow agent, 6g of peroxybenzoic acid, 4g of Fischer-Tropsch wax and 0.1g of antioxidant. Wherein the composite core-forming flow agent is prepared by selecting the one prepared in example 1. The mineral filler is powdered calcium carbonate with particle size not greater than 5 micron and purity not less than 95% and glass fiber length not greater than 0.5 cm.
Preparing a composite high polymer material:
(1) adding PA66 polyamide resin, calcium carbonate, composite nuclear flow agent, peroxybenzoic acid, Fischer-Tropsch wax and antioxidant into a high-speed mixer, and uniformly mixing to obtain a mixture;
(2) and (3) placing the obtained mixture in a double screw machine, wherein the rotating speed is 250rpm, heating the mixture to the temperature of 220-.
Example 3:
weighing the following raw materials by mass: 200g of polyamide resin, 10g of kaolin, 6g of glass fiber, 2g of composite nuclear flow agent, 8g of peroxybenzoic acid, 5g of Fischer-Tropsch wax and 1g of antioxidant. Wherein the composite core-forming flow agent is prepared by selecting the one prepared in example 1. The mineral filler is powder wollastonite with particle size not greater than 5 microns and purity not less than 95%, and the glass fiber has length not greater than 0.5 cm.
Preparing a composite high polymer material:
(1) adding PA66 polyamide resin, wollastonite, a composite nuclear flow agent, peroxybenzoic acid, Fischer-Tropsch wax and an antioxidant into a high-speed mixer, and uniformly mixing to obtain a mixture;
(2) and (3) placing the obtained mixture in a double screw machine, wherein the rotating speed is 250rpm, heating the mixture to the temperature of 220-.
The polymer material prepared in the embodiments 1-3 of the invention can be used for preparing the vehicle product by injection or injection molding, wherein the injection or injection temperature is 220-260 ℃, and the injection pressure is 80-180 MPa.
For injection molding of a small product as shown in FIG. 1, the injection molding temperature is 240 ℃ and the injection molding pressure is 120 MPa.
Comparative example 1:
comparative example 1 and example 3 are compared, and the difference from example 3 is only in the selection of raw materials, the addition amount of the composite nucleation flow agent is zero, and the preparation method is the same as that of example 3, so that comparative material 1 is obtained.
Comparative example 2:
comparative example 2 is compared with example 3, and differs from example 3 only in the selection of raw materials, replacement of the composite nuclear flow agent with the conventional modifier for polyamide, hypophosphite, addition amount and preparation method are the same as those of example 3, and comparative material 2 is obtained.
Comparative example 3:
comparative example 3 contrasts with example 3, and only differs from example 3 in the selection of the raw materials of the composite nuclear flow agent, and the raw materials in the composite nuclear flow agent are as follows: sodium benzoate, sodium carboxymethylcellulose and talcum powder in a mass ratio of 1: 1: 0.1, the preparation method of the composite nuclear flow agent comprises the following steps: (1) mixing talcum powder and water according to the weight ratio of 1: 50, and uniformly stirring to prepare a suspension system; (2) sodium benzoate and sodium carboxymethyl cellulose were mixed according to a ratio of 1: 1, stirring until the mixture is dissolved, and stirring for 3.5 hours at the speed of 350rpm to obtain the composite nuclear flow agent.
Polymer Material preparation-same as in example 3, comparative material 3 was obtained.
Comparative example 4:
comparative example 4 is compared with example 3, and differs from example 3 only in the selection of raw materials of the composite nuclear flow agent, wherein the raw materials of the composite nuclear flow agent are as follows: linoleic acid and talcum powder, the mass ratio is 0.8: 0.1, the preparation method of the composite nuclear flow agent comprises the following steps: mixing talcum powder and water according to the weight ratio of 1: 50, stirring uniformly, heating to 65 ℃, adding linoleic acid, stirring at 350rpm for 3.5h, and then ultrasonically dispersing for 10min by using 25KHz ultrasonic waves to obtain the composite nucleating flowing agent.
The polymer material was prepared in the same manner as in example 3 to obtain comparative material 4.
Comparative example 5:
comparative example 5 is compared with example 3, and differs from example 3 only in that the raw material ratio of the composite core flow agent is different, and the mass ratio of the linoleic acid to the sodium benzoate, the sodium carboxymethyl cellulose and the talcum powder is 0.2: 1: 1: 0.1. the polymer material was prepared in the same manner as in example 3 to obtain comparative material 5.
The prepared material was tested for melt index using astm d1238 to determine the flowability of the plastic, and the data obtained are shown in table 1:
the prepared material is prepared into a vehicle test sample piece by adopting an injection molding mode, and the obtained data is shown in table 2, wherein the test sample piece is used for testing the tensile strength (GB/T1040.2), the bending strength (GB/T9341), the notch impact strength (GB/T1043.1) of the tube beam, the notch impact strength (GB/T1043.1) of the tube beam at low temperature (-30 ℃), the thermal deformation temperature (1.8Mpa) (GB/T1634.2) and the long-term thermal aging (the test temperature is 140 +/-2 ℃, and the aging time is 1000 +/-5 h):
TABLE 2
From the data analysis of table 1 and table 2, it can be seen that:
1. the polymer materials prepared in examples 1-3 had high flowability, and the melt index was 32g/10min or more, which was improved by about 10 times or more as compared with PA 66. Example 3 is about 3 times higher in fluidity than comparative examples 1 and 2, which shows that the composite nucleating agent can significantly improve the fluidity. Compared with comparative example 3 and comparative example 4, the core forming flow agent prepared from the raw materials of the linoleic acid, the sodium benzoate and the like is improved by about 15g/10min, which shows that the composite core forming flow agent prepared from the raw materials of the linoleic acid, the sodium benzoate and the like has larger influence on the polyamide material.
2. As is clear from Table 2, the polymer materials prepared in examples 1 to 3 have high strength, good heat resistance and good aging resistance, and are particularly suitable for use in high-temperature environments such as engine compartments. Compared with comparative examples 1 and 2, the composite nuclear flow agent added in example 3 has obviously improved various performances, which shows that the composite nuclear flow agent has a promoting effect on improving the performances of the high polymer material. Compared with comparative examples 3, 4 and 5, the composite nuclear flow agent prepared from the raw materials such as the linoleic acid, the sodium benzoate and the like or the proportion of the raw materials for the composite nuclear flow has larger influence on the performance of the polyamide material.
Although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention as defined in the appended claims. The techniques, shapes, and configurations not described in detail in the present invention are all known techniques.
Claims (9)
1. The heat-resistant anti-aging high polymer material is characterized by comprising the following raw materials: polyamide resin, mineral filler, fiber, a composite nuclear flow agent, peroxybenzoic acid, Fischer-Tropsch wax and an antioxidant, wherein the composite nuclear flow agent consists of linoleic acid, sodium benzoate, sodium carboxymethylcellulose and talcum powder.
2. A heat and aging resistant polymer material as claimed in claim 1, wherein the mineral filler is selected from one of kaolin, mica, wollastonite, and calcium carbonate.
3. A heat-resistant anti-aging polymer material according to claim 2, wherein the fiber is selected from one of carbon fiber and glass fiber.
4. A heat-resistant anti-aging polymer material as claimed in claim 3, wherein the raw materials comprise the following components in parts by weight: 100-200 parts of polyamide resin, 4-10 parts of mineral filler, 2-6 parts of fiber, 0.5-2 parts of composite nuclear flow agent, 5-8 parts of peroxybenzoic acid, 3-5 parts of Fischer-Tropsch wax and 0.2-1 part of antioxidant.
5. The heat-resistant anti-aging high polymer material as claimed in claim 4, wherein the mass ratio of the linoleic acid to the sodium benzoate, the sodium carboxymethyl cellulose and the talcum powder is 0.8: 1: 1: 0.1.
6. a heat-resistant anti-aging polymer material as claimed in claim 5, wherein the particle size of the mineral filler is not more than 5 μm, the purity is not less than 95%, and the length of the fiber is not more than 0.5 cm.
7. A method for preparing a heat-resistant anti-aging polymer material according to any one of claims 1 to 6, wherein the method comprises the following steps:
(1) adding polyamide resin, mineral filler, composite nuclear flow agent, peroxybenzoic acid, Fischer-Tropsch wax and antioxidant into a high-speed mixer, and uniformly mixing to obtain a mixture;
(2) placing the obtained mixture in a double screw machine at the rotation speed of 200-300rpm, heating to 230 ℃ at 220-275 ℃, adding fibers, heating again to 260-275 ℃, and then cooling to 250 ℃ at 220-250 ℃ for extrusion granulation to obtain the polymer material.
8. The method as claimed in claim 7, wherein the injection temperature of the polymer material is 220-260 ℃ and the injection pressure is 80-180 MPa.
9. The method for preparing a heat-resistant anti-aging polymer material according to claim 8, wherein the method for preparing the composite nuclear flow agent comprises the following steps:
(1) mixing talcum powder and water according to the weight ratio of 1: 50 to prepare a suspension system;
(2) sodium benzoate and sodium carboxymethyl cellulose were mixed according to a ratio of 1: 1, then heating to 60-70 ℃, adding linoleic acid, stirring at 300-400rpm for 3-4h, and then performing ultrasonic dispersion for 10min to obtain the composite nuclear flow agent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115746556A (en) * | 2022-11-29 | 2023-03-07 | 金发科技股份有限公司 | Low-mold-fouling halogen-free flame-retardant reinforced nylon material and preparation method and application thereof |
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