CN111471295B - Impact-resistant composition and preparation method thereof - Google Patents
Impact-resistant composition and preparation method thereof Download PDFInfo
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- CN111471295B CN111471295B CN202010196162.2A CN202010196162A CN111471295B CN 111471295 B CN111471295 B CN 111471295B CN 202010196162 A CN202010196162 A CN 202010196162A CN 111471295 B CN111471295 B CN 111471295B
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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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/36—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino acids, polyamines and polycarboxylic acids
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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
- C08K2201/005—Additives being defined by their particle size in general
Abstract
The invention discloses an impact-resistant composition and a preparation method thereof, wherein the composition comprises the following components: 47.4-66.7 parts of polyamide, 17.7-27.1 parts of maleic anhydride grafted polypropylene, 13-23 parts of glass fiber powder, 0.8-1.1 parts of organic nucleating agent, 0.2-0.4 part of antioxidant, 0.2-0.4 part of light stabilizer and 0.2-0.5 part of cross-linking agent. The polyamide used in the invention is prepared by carrying out polycondensation reaction on adipic acid and hexamethylene diamine, azetidine-2-carboxylic acid is added to adjust the molecular weight distribution of the polyamide, the polyamide with more uniform molecular weight distribution is obtained, the polyamide can be modified by glass fiber powder and polypropylene to obtain a composition with excellent performance, and the mechanical property of the composition can still be kept good after water absorption treatment.
Description
Technical Field
The invention belongs to the field of high molecular polymers, and particularly relates to an impact-resistant composition and a preparation method thereof.
Background
Polyamide is commonly called Nylon (Nylon), and is called Polyamide, and Polyamide is a high molecular compound, and the Polyamide is various in variety, but the structure of the Polyamide is a linear high molecular compound containing amide groups. The polyamide can be prepared by ring-opening polymerization of lactam, or polycondensation of diamine and diacid. The Polyamide (PA) is a polymer having a polar amide group (-CO-NH-) in the main chain. Originally used as a raw material for manufacturing fibers, the PA is later used as an engineering plastic widely applied in the industry at present due to toughness, wear resistance, self-lubrication and wide use temperature range. The PA is often used for replacing copper and nonferrous metals to manufacture mechanical, chemical and electrical parts, such as a fuel pump gear of a diesel engine, a water pump, a high-pressure sealing ring, an oil delivery pipe and the like, due to the excellent performance of the PA.
However, polyamides have some disadvantages which limit their use in certain fields, such as their high moisture absorption and permeability, and their tendency to undergo dimensional shifts upon absorption of water. The polyamide has high water absorption and linear expansion coefficient, especially nylon-6 and nylon-66, and has balanced water absorption up to 3.5% in atmosphere and saturated water absorption up to 10.7% after being soaked in water at normal temperature for 24 hr. The water absorption resulted in volume expansion, and when the water absorption was 3.5%, the linear expansion coefficient was 0.65%, and when the water absorption was 2.3%, the dimensional stability was poor.
Disclosure of Invention
The invention aims to provide an impact-resistant composition which has good wear resistance and impact resistance, has good mechanical properties after water absorption, and is suitable for components such as water-stop sheets and the like which need to be in a humid environment for a long time.
Further, there is a need for a process for preparing an impact resistant composition as described above.
An impact resistant composition comprising the following ingredients:
a polyamide;
maleic anhydride grafted polypropylene;
glass fiber powder;
an organic nucleating agent;
an antioxidant;
a light stabilizer;
a crosslinking agent.
Preferably, the impact-resistant composition comprises the following components in parts by weight:
among them, the sum of the parts by weight of the above components is preferably 100 parts.
Still more preferably, the impact-resistant composition comprises the following components in parts by weight:
wherein, the polyamide is prepared by the following method:
mixing the following components in parts by weight: dissolving 1 mol ratio of adipic acid and hexamethylenediamine in an aqueous solution, adding azetidine-2-carboxylic acid, uniformly mixing, wherein the addition amount of the azetidine-2-carboxylic acid is 0.8-1wt% of the adipic acid, carrying out polycondensation reaction at 250-260 ℃ under the condition of 1.5MPa, simultaneously pumping away water in a reaction system, and reacting for 8 hours to obtain the polyamide.
The aim of adding the azetidine-2-carboxylic acid is mainly to control the molecular weight and the uniformity of the molecular weight of the polyamide, and through a large number of researches, experiments and repeated certifications, a certain amount of azetidine-2-carboxylic acid is found to be added, the polyamide prepared by the invention can be used for preparing a composition with good comprehensive mechanical properties such as impact resistance, wear resistance and the like after being reinforced by glass fiber powder, and particularly, the mechanical property of the composition is still good after water absorption treatment.
Preferably, the specification of the glass fiber powder is 500-800 meshes, and when the mesh number of the glass fiber is too large or too small, the compatibility of each component in the composition is poor, and the comprehensive mechanical property of the composition is poor.
Preferably, the organic nucleating agent is selected from a benzene phosphonate or a fatty acid amide, and the organic nucleating agent is preferably sodium benzene phosphonate.
Wherein, the maleic anhydride grafted polypropylene is prepared by the following method:
mixing 100 parts by weight of polypropylene and 1-1.5 parts by weight of maleic anhydride, adding 0.4-1 part of di-tert-butyl peroxide and 0.5-1 part of styrene, uniformly mixing, adding into a screw extruder, and performing extrusion granulation to obtain the maleic anhydride grafted polypropylene.
Preferably, the maleic anhydride grafted polypropylene is prepared by the following method:
mixing 100 parts by weight of polypropylene and 1-1.5 parts by weight of maleic anhydride, adding 0.4-1 part by weight of di-tert-butyl peroxide and 0.5-1 part by weight of styrene, uniformly mixing, and adding into a screw extruder at the temperature of: the feeding section is 100-160 ℃, the melting section is 160-190 ℃, the homogenizing section is 190-210 ℃, and the head is 190-210 ℃; and (3) granulating at the main machine rotating speed of 300r/min by using a double-screw extruder to obtain the maleic anhydride grafted polypropylene.
Preferably, the polypropylene has a melt flow rate of less than 5g/10min, as measured according to ASTM D1238 at 230 ℃ under 2.16 kg. When the melt flow rate of the polypropylene is more than 5g/10min, the molecular weight distribution of the polypropylene is greatly different when the polypropylene is blended with the polyamide prepared by the invention, so that the internal arrangement of the molecular structure of the polypropylene is not tight enough, and the mechanical property of the composition is influenced.
Preferably, the antioxidant is selected from one or more of pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], dilauryl thiodipropionate, tris (4-nonylphenyl) phosphite and triphenyl phosphite.
Preferably, the antioxidant is selected from one or more of antioxidant 1010, antioxidant DLTP, antioxidant TNP or antioxidant TPP.
Preferably, the light stabilizer is a hindered amine light stabilizer or benzoate ultraviolet light absorber, preferably 2, 6-tetramethyl-4-piperidyl stearate.
Preferably, the cross-linking agent is methyl orthosilicate or trimethoxysilane.
A process for the preparation of an impact resistant composition as described above, comprising the steps of:
the polyamide, the maleic anhydride grafted polypropylene, the glass fiber powder, the organic nucleating agent, the antioxidant, the light stabilizer and the crosslinking agent are uniformly mixed according to the weight ratio, and are extruded by a double-screw extruder, the temperature of the double-screw extruder is set to be 180-200 ℃, and the composition is obtained by granulation.
Wherein, the preparation method comprises the following steps:
1) Mixing 1: dissolving 1 mol ratio of adipic acid and hexamethylenediamine in an aqueous solution, adding azetidine-2-carboxylic acid, uniformly mixing, wherein the addition amount of the azetidine-2-carboxylic acid is 0.8-1wt% of the adipic acid, carrying out polycondensation reaction at 250-260 ℃ and 1.5MPa, and simultaneously pumping water in a reaction system for reaction for 8 hours to obtain polyamide;
2) Preparation of maleic anhydride grafted polypropylene:
mixing 100 parts by weight of polypropylene and 1-1.5 parts by weight of maleic anhydride, adding 0.4-1 part by weight of di-tert-butyl peroxide and 0.5-1 part by weight of styrene, uniformly mixing, and adding into a screw extruder at the temperature of: the feeding section is 100-160 ℃, the melting section is 160-190 ℃, the homogenizing section is 190-210 ℃, and the head is 190-210 ℃; the main machine rotating speed of the double-screw extruder is 300r/min, and the maleic anhydride grafted polypropylene is obtained by granulation;
3) Adding polyamide, maleic anhydride grafted polypropylene, glass fiber powder, an organic nucleating agent, an antioxidant, a light stabilizer and a crosslinking agent into a double-screw extruder according to the weight ratio, and extruding and granulating at 220-260 ℃ to obtain the composition.
Compared with the prior art, the composition provided by the invention is prepared by extruding polyamide, maleic anhydride grafted polypropylene, glass fiber powder, an organic nucleating agent, an antioxidant, a light stabilizer and a crosslinking agent through double screws. The polyamide used in the invention is prepared by carrying out polycondensation reaction on adipic acid and hexamethylene diamine, azetidine-2-carboxylic acid is added to adjust the molecular weight distribution of the polyamide, the polyamide with more uniform molecular weight distribution is obtained, the polyamide is modified by 500-800 meshes of glass fiber powder and polypropylene with the melt flow rate of less than 5g/10min, a composition with excellent performance can be obtained, the mechanical property of the polyamide is still good after water absorption treatment, particularly the wear resistance and the impact resistance are good, and the polyamide is suitable for being applied to components in a humid environment for a long time, and is particularly suitable for being applied to the production field of water baffles.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments in order to make the technical field better understand the scheme of the present invention.
Description of the raw materials used in the examples and comparative examples:
the glass fiber is glass fiber powder, and specifications of the Hangzhou high-tech composite material company are respectively 200 meshes, 500 meshes, 800 meshes and 1200 meshes;
polypropylene 1: ningbo Junyun plastification Co., ltd, designation H5300, melt flow Rate (MFR 2) of 3.4g/10min, according to ASTM D1238, at 230 ℃,2.16 kg;
polypropylene 2: ningbo Junyun plastification Co., ltd, no. EP3307, melt flow Rate (MFR 2) 15g/10min, according to ASTM D1238, at 230 ℃,2.16 kg;
chopped glass fiber with diameter of 13 μm and length of 3mm, hangzhou high-tech composite Co., ltd.
Azetidine-2-carboxylic acid, also known as 2-azetidinecarboxylic acid, CAS No.20063-89-2,
the structural formula is
Organic nucleating agent: sodium phenylphosphonate;
antioxidant: an antioxidant 1010;
light stabilizer: 2, 6-tetramethyl-4-piperidine stearate;
a crosslinking agent: trimethoxysilane;
the remaining material sources are commercially available.
Example 1
1) Preparation of the polyamide:
mixing the following components in parts by weight: dissolving 1 mol ratio of adipic acid and hexamethylenediamine in an aqueous solution, adding azetidine-2-carboxylic acid, uniformly mixing, wherein the addition amount of the azetidine-2-carboxylic acid is 0.8wt% of the adipic acid, performing polycondensation reaction at 250-260 ℃ under the condition of 1.5MPa, simultaneously pumping away water in a reaction system, and reacting for 8 hours to obtain polyamide;
2) Preparation of maleic anhydride grafted polypropylene:
mixing 100 parts by weight of polypropylene 1 and 1.2 parts by weight of maleic anhydride, adding 0.8 part of di-tert-butyl peroxide and 0.6 part of styrene, uniformly mixing, and adding into a screw extruder at the temperature of: the feeding section is 100-160 ℃, the melting section is 160-190 ℃, the homogenizing section is 190-210 ℃, and the head is 190-210 ℃; the main machine rotating speed of the double-screw extruder is 300r/min, and the maleic anhydride grafted polypropylene is obtained by granulation;
3) According to the weight parts shown in Table 1, polyamide, maleic anhydride grafted polypropylene, glass fiber powder (500 meshes), organic nucleating agent, antioxidant, light stabilizer and crosslinking agent are added into a double-screw extruder and extruded and granulated at 220-260 ℃ to obtain the composition.
Example 2
1) Preparation of the polyamide:
mixing 1: dissolving 1 mol ratio of adipic acid and hexamethylenediamine in an aqueous solution, adding azetidine-2-carboxylic acid, uniformly mixing, wherein the addition amount of the azetidine-2-carboxylic acid is 0.9wt% of the adipic acid, carrying out polycondensation reaction at 250-260 ℃ and 1.5MPa, and simultaneously pumping water in a reaction system for reaction for 8 hours to obtain polyamide;
2) Preparation of maleic anhydride grafted polypropylene:
mixing 100 parts by weight of polypropylene 1 and 1 part by weight of maleic anhydride, then adding 0.4 part of di-tert-butyl peroxide and 0.5 part of styrene, uniformly mixing, and then adding into a screw extruder, wherein the temperature is as follows: the feeding section is 100-160 ℃, the melting section is 160-190 ℃, the homogenizing section is 190-210 ℃, and the head is 190-210 ℃; the main machine rotating speed of the double-screw extruder is 300r/min, and the maleic anhydride grafted polypropylene is obtained by granulation;
3) The polyamide, the maleic anhydride grafted polypropylene, the glass fiber powder (800 meshes), the organic nucleating agent, the antioxidant, the light stabilizer and the crosslinking agent are added into a double-screw extruder according to the weight parts shown in the table 1, and the mixture is extruded and granulated at 220-260 ℃ to obtain the composition.
Example 3
1) Preparation of the polyamide:
mixing 1: dissolving 1 mol ratio of adipic acid and hexamethylenediamine in an aqueous solution, adding azetidine-2-carboxylic acid, uniformly mixing, wherein the addition amount of the azetidine-2-carboxylic acid is 1wt% of the adipic acid, carrying out polycondensation reaction at 250-260 ℃ and 1.5MPa, and simultaneously pumping water in a reaction system for reaction for 8 hours to obtain polyamide;
2) Preparation of maleic anhydride grafted polypropylene:
mixing 100 parts by weight of polypropylene 1 and 1.5 parts by weight of maleic anhydride, adding 1 part of di-tert-butyl peroxide and 1 part of styrene, uniformly mixing, and adding into a screw extruder at the temperature of: the feeding section is 100-160 ℃, the melting section is 160-190 ℃, the homogenizing section is 190-210 ℃, and the head is 190-210 ℃; the main machine rotating speed of the double-screw extruder is 300r/min, and the maleic anhydride grafted polypropylene is obtained by granulation;
3) According to the weight parts shown in Table 1, polyamide, maleic anhydride grafted polypropylene, glass fiber powder (800 meshes), an organic nucleating agent, an antioxidant, a light stabilizer and a crosslinking agent are added into a double-screw extruder and extruded and granulated at 220-260 ℃ to obtain the composition.
Example 4
1) Preparation of the polyamide:
mixing 1: dissolving 1 mol ratio of adipic acid and hexamethylenediamine in an aqueous solution, adding azetidine-2-carboxylic acid, uniformly mixing, wherein the addition amount of the azetidine-2-carboxylic acid is 0.8wt% of the adipic acid, carrying out polycondensation reaction at 250-260 ℃ and 1.5MPa, and simultaneously pumping water in a reaction system for reaction for 8 hours to obtain polyamide;
2) Preparation of maleic anhydride grafted polypropylene:
mixing 100 parts by weight of polypropylene 1 and 1.2 parts by weight of maleic anhydride, adding 0.8 part of di-tert-butyl peroxide and 0.6 part of styrene, uniformly mixing, and adding into a screw extruder at the temperature of: the feeding section is 100-160 ℃, the melting section is 160-190 ℃, the homogenizing section is 190-210 ℃, and the head is 190-210 ℃; the main machine rotating speed of the double-screw extruder is 300r/min, and the maleic anhydride grafted polypropylene is obtained by granulation;
3) The polyamide, the maleic anhydride grafted polypropylene, the glass fiber powder (500 meshes), the organic nucleating agent, the antioxidant, the light stabilizer and the crosslinking agent are added into a double-screw extruder according to the weight parts shown in the table 1, and the mixture is extruded and granulated at 220-260 ℃ to obtain the composition.
Example 5
1) Preparation of the polyamide:
mixing 1: dissolving 1 mol ratio of adipic acid and hexamethylenediamine in an aqueous solution, adding azetidine-2-carboxylic acid, uniformly mixing, wherein the addition amount of the azetidine-2-carboxylic acid is 0.8wt% of the adipic acid, carrying out polycondensation reaction at 250-260 ℃ and 1.5MPa, and simultaneously pumping water in a reaction system for reaction for 8 hours to obtain polyamide;
2) Preparation of maleic anhydride grafted polypropylene:
mixing 100 parts by weight of polypropylene 1 and 1.2 parts by weight of maleic anhydride, adding 0.8 part of di-tert-butyl peroxide and 0.6 part of styrene, uniformly mixing, and adding into a screw extruder at the temperature of: the feeding section is 100-160 ℃, the melting section is 160-190 ℃, the homogenizing section is 190-210 ℃, and the head is 190-210 ℃; the main machine rotating speed of the double-screw extruder is 300r/min, and the maleic anhydride grafted polypropylene is obtained by granulation;
3) According to the weight parts shown in Table 1, polyamide, maleic anhydride grafted polypropylene, glass fiber powder (500 meshes), organic nucleating agent, antioxidant, light stabilizer and crosslinking agent are added into a double-screw extruder and extruded and granulated at 220-260 ℃ to obtain the composition.
Example 6
1) Preparation of the polyamide:
mixing the following components in parts by weight: dissolving adipic acid and hexamethylenediamine in a molar ratio of 1 in an aqueous solution, adding acetic acid, uniformly mixing, wherein the addition amount of the acetic acid is 0.8wt% of the adipic acid, carrying out polycondensation reaction at 250-260 ℃ and under the condition of 1.5MPa, simultaneously pumping water in a reaction system, and reacting for 8 hours to obtain polyamide;
2) Preparation of maleic anhydride grafted polypropylene:
mixing 100 parts by weight of polypropylene 1 and 1.2 parts by weight of maleic anhydride, adding 0.8 part of di-tert-butyl peroxide and 0.6 part of styrene, uniformly mixing, and adding into a screw extruder at the temperature of: the feeding section is 100-160 ℃, the melting section is 160-190 ℃, the homogenizing section is 190-210 ℃, and the head is 190-210 ℃; the main machine rotating speed of the double-screw extruder is 300r/min, and the maleic anhydride grafted polypropylene is obtained by granulation;
3) According to the weight parts shown in Table 1, polyamide, maleic anhydride grafted polypropylene, glass fiber powder (500 meshes), organic nucleating agent, antioxidant, light stabilizer and crosslinking agent are added into a double-screw extruder and extruded and granulated at 220-260 ℃ to obtain the composition.
Comparative example 1
1) Preparation of the polyamide:
mixing the following components in parts by weight: dissolving 1 mol ratio of adipic acid and hexamethylenediamine in an aqueous solution, adding azetidine-2-carboxylic acid, uniformly mixing, wherein the addition amount of the azetidine-2-carboxylic acid is 0.8wt% of the adipic acid, carrying out polycondensation reaction at 250-260 ℃ and 1.5MPa, and simultaneously pumping water in a reaction system for reaction for 8 hours to obtain polyamide;
2) Preparation of maleic anhydride grafted polypropylene:
mixing 100 parts by weight of polypropylene 1 and 1.2 parts by weight of maleic anhydride, adding 0.8 part of di-tert-butyl peroxide and 0.6 part of styrene, uniformly mixing, and adding into a screw extruder at the temperature of: the feeding section is 100-160 ℃, the melting section is 160-190 ℃, the homogenizing section is 190-210 ℃, and the head is 190-210 ℃; the main machine rotating speed of the double-screw extruder is 300r/min, and the maleic anhydride grafted polypropylene is obtained by granulation;
3) According to the weight parts shown in Table 1, polyamide, maleic anhydride grafted polypropylene, chopped glass fiber (diameter 13 μm, length 3mm, hangzhou high-tech composite Co., ltd.), organic nucleating agent, antioxidant, light stabilizer and crosslinking agent are added into a double-screw extruder, and extrusion granulation is carried out at 220-260 ℃ to obtain the composition.
Example 7
1) Preparation of the polyamide:
mixing the following components in parts by weight: dissolving 1 mol ratio of adipic acid and hexamethylenediamine in an aqueous solution, adding azetidine-2-carboxylic acid, uniformly mixing, wherein the addition amount of the azetidine-2-carboxylic acid is 0.8wt% of the adipic acid, performing polycondensation reaction at 250-260 ℃ under the condition of 1.5MPa, simultaneously pumping away water in a reaction system, and reacting for 8 hours to obtain polyamide;
2) Preparation of maleic anhydride grafted polypropylene:
mixing 100 parts by weight of polypropylene 2 and 1.2 parts by weight of maleic anhydride, adding 0.8 part of di-tert-butyl peroxide and 0.6 part of styrene, uniformly mixing, and adding into a screw extruder at the temperature of: the feeding section is 100-160 ℃, the melting section is 160-190 ℃, the homogenizing section is 190-210 ℃, and the head is 190-210 ℃; the main machine rotating speed of the double-screw extruder is 300r/min, and the maleic anhydride grafted polypropylene is obtained by granulation;
3) According to the weight parts shown in Table 1, polyamide, maleic anhydride grafted polypropylene, glass fiber powder (500 meshes), organic nucleating agent, antioxidant, light stabilizer and crosslinking agent are added into a double-screw extruder and extruded and granulated at 220-260 ℃ to obtain the composition.
Example 8
1) Preparation of the polyamide:
mixing the following components in parts by weight: dissolving 1 mol ratio of adipic acid and hexamethylenediamine in an aqueous solution, adding azetidine-2-carboxylic acid, uniformly mixing, wherein the addition amount of the azetidine-2-carboxylic acid is 0.8wt% of the adipic acid, carrying out polycondensation reaction at 250-260 ℃ and 1.5MPa, and simultaneously pumping water in a reaction system for reaction for 8 hours to obtain polyamide;
2) Preparation of maleic anhydride grafted polypropylene:
mixing 100 parts by weight of polypropylene 1 and 1.2 parts by weight of maleic anhydride, adding 0.8 part of di-tert-butyl peroxide and 0.6 part of styrene, uniformly mixing, and adding into a screw extruder at the temperature of: the feeding section is 100-160 ℃, the melting section is 160-190 ℃, the homogenizing section is 190-210 ℃, and the head is 190-210 ℃; the main machine rotating speed of the double-screw extruder is 300r/min, and the maleic anhydride grafted polypropylene is obtained by granulation;
3) The polyamide, the maleic anhydride grafted polypropylene, the glass fiber powder (1200 meshes), the organic nucleating agent, the antioxidant, the light stabilizer and the crosslinking agent are added into a double-screw extruder according to the weight parts shown in the table 1, and the mixture is extruded and granulated at 220-260 ℃ to obtain the composition.
Example 9
1) Preparation of the polyamide:
mixing the following components in parts by weight: dissolving 1 mol ratio of adipic acid and hexamethylenediamine in an aqueous solution, adding azetidine-2-carboxylic acid, uniformly mixing, wherein the addition amount of the azetidine-2-carboxylic acid is 0.8wt% of the adipic acid, carrying out polycondensation reaction at 250-260 ℃ and 1.5MPa, and simultaneously pumping water in a reaction system for reaction for 8 hours to obtain polyamide;
2) Preparation of maleic anhydride grafted polypropylene:
mixing 100 parts by weight of polypropylene 1 and 1.2 parts by weight of maleic anhydride, adding 0.8 part of di-tert-butyl peroxide and 0.6 part of styrene, uniformly mixing, and adding into a screw extruder at the temperature of: the feeding section is 100-160 ℃, the melting section is 160-190 ℃, the homogenizing section is 190-210 ℃, and the head is 190-210 ℃; the main machine rotating speed of the double-screw extruder is 300r/min, and the maleic anhydride grafted polypropylene is obtained by granulation;
3) According to the weight parts shown in Table 1, polyamide, maleic anhydride grafted polypropylene, glass fiber powder (200 meshes), an organic nucleating agent, an antioxidant, a light stabilizer and a crosslinking agent are added into a double-screw extruder and extruded and granulated at 220-260 ℃ to obtain the composition.
Comparative example 2
1) Preparation of the polyamide:
mixing 1: dissolving 1 mol ratio of adipic acid and hexamethylenediamine in an aqueous solution, adding azetidine-2-carboxylic acid, uniformly mixing, wherein the addition amount of the azetidine-2-carboxylic acid is 0.9wt% of the adipic acid, performing polycondensation reaction at 250-260 ℃ under the condition of 1.5MPa, simultaneously pumping away water in a reaction system, and reacting for 8 hours to obtain polyamide;
2) Preparation of maleic anhydride grafted polypropylene:
mixing 100 parts by weight of polypropylene 1 and 1.2 parts by weight of maleic anhydride, adding 0.8 part of di-tert-butyl peroxide and 0.6 part of styrene, uniformly mixing, and adding into a screw extruder at the temperature of: the feeding section is 100-160 ℃, the melting section is 160-190 ℃, the homogenizing section is 190-210 ℃, and the head is 190-210 ℃; the main machine rotating speed of the double-screw extruder is 300r/min, and the maleic anhydride grafted polypropylene is obtained by granulation;
3) According to the weight parts shown in Table 1, polyamide, maleic anhydride grafted polypropylene, glass fiber powder (500 meshes), an antioxidant, a light stabilizer and a crosslinking agent are added into a double-screw extruder and extruded and granulated at 220-260 ℃ to obtain the composition.
Table 1 examples formulations table (units are parts by weight)
The compositions prepared in the examples and comparative examples were subjected to the following performance tests, and the test results are shown in table 2:
description of Performance test methods
The tensile strength was examined according to GB/T1040-2006, at a tensile rate of 5mm/s.
The bending strength is tested according to the GB/T9341-2008 standard; sample size (mm): (80. + -.2) × (10. + -. 0.2) × (4. + -. 0.2), and the bending speed was 20mm/min.
The notch impact strength is tested according to the GB/T1843-2008 standard; sample size (mm): (80. + -.2) × (10. + -. 0.2) × (4. + -. 0.2), the radius of the bottom of the notch (mm) is 0.25. + -. 0.05, and the notch retention thickness (mm) is 8.0. + -. 0.2.
Mechanical property test after water absorption
Tensile strength after water absorption:
preparing a sample according to GB/T1040-2006 standard, soaking the sample in water, placing the sample in a high-low temperature alternating test box for processing for 48h, setting the temperature to be cyclically changed between 10 ℃ and 50 ℃ within 24 hours before, setting the temperature to be cyclically changed between-10 ℃ and 30 ℃ within 20 ℃/10min within 24 hours after, and setting the temperature to be cyclically changed between-10 ℃ and 30 ℃, wherein the temperature change speed is 20 ℃/10min. The treated sample was dried and cooled to room temperature, and the tensile strength after water absorption was measured at a tensile rate of 5mm/s in accordance with GB/T1040-2006.
Bending strength after water absorption
Performing inspection according to GB/T9341-2008 standard; the prepared sample size was (mm): (80. + -. 2) × (10. + -. 0.2) × (4. + -. 0.2). Soaking a sample in water, and placing the sample in a high-low temperature alternating test box for treatment for 48h, wherein the temperature is set to be between 10 and 50 ℃ in a cyclic change manner within the first 24 h, the temperature change speed is 20 ℃/10min, and the temperature is set to be between-10 and 30 ℃ in a cyclic change manner within the last 24 h, and the temperature change speed is 20 ℃/10min. The treated sample is dried and cooled to room temperature, and then the bending strength after water absorption is tested according to the GB/T9341-2008 standard, and the bending speed is 20mm/min.
Notched impact strength after water absorption
Testing according to GB/T1843-2008 standard; the prepared sample size was (mm): (80. + -.2) × (10. + -. 0.2) × (4. + -. 0.2), the radius of the bottom of the notch (mm) is 0.25. + -. 0.05, and the notch retention thickness (mm) is 8.0. + -. 0.2. Soaking a sample in water, and placing the sample in a high-low temperature alternating test box for treatment for 48h, wherein the temperature is set to be between 10 ℃ and 50 ℃ for 24 h before, the temperature change speed is 20 ℃/10min, and the temperature is set to be between-10 ℃ and 30 ℃ for 24 h after, and the temperature change speed is 20 ℃/10min. The treated sample was dried and cooled to room temperature, and the notched impact strength after water absorption was determined according to GB/T1843-2008.
And (3) testing the frictional wear performance:
in the combined sample of 3cm x 2cm x 0.5cm prepared by injection molding, the abrasion resistance was tested by means of a multifunctional friction abrasion tester (model UMT-2, CETR, usa); dual sample is steel 440-C, the rotating speed is 400r/min, the load is 100N, and the experimental time is 1h. In the experiment, the friction factor of each sample is measured for 3 times, the average value is taken, and then the abrasion loss m is measured according to a weighing method 1 。
And (3) treating the sample subjected to the frictional wear performance test in a salt spray corrosion test box, wherein the test is cyclically changed at the temperature of-20 ℃ to 120 ℃, the temperature change speed is 15 ℃/10min, and the mist reduction amount is 0.5mL/80cm × h, and the nozzle pressure is 100kPa. Spraying 5% sodium chloride and 5% HCl in water, taking out sample after 10 days, standing at 60 deg.C for 24 hr, cooling to room temperature, performing friction and wear performance test, and measuring wear amount m 2 。
TABLE 2 composition Performance test Table
The experiment shows that the composition prepared by the invention has low friction wear amount, and under the condition that the surface has scratch wear, the abrasion resistance is also obviously better than that of the comparative example 1, the examples 7-9 and the comparative example 2 after the simulated aging experiment, thereby proving that the composition prepared by the invention has excellent abrasion resistance.
Meanwhile, the mechanical properties of the composition before and after water absorption are inspected, the mechanical properties of the composition are detected after the composition is soaked in water for 48 hours in a temperature change manner and dried, and the result shows that the comprehensive mechanical properties of the composition are also obviously superior to those of the compositions of comparative example 1, examples 7-9 and comparative example 2. The composition prepared by the invention can be widely applied to components working in a humid environment, and is particularly suitable for the production field of water-stop sheets.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (6)
1. An impact-resistant composition is characterized by comprising the following components in parts by weight:
47.4-66.7 parts of polyamide;
17.7-27.1 parts of maleic anhydride grafted polypropylene;
13-23 parts of glass fiber powder;
0.8-1.1 parts of organic nucleating agent;
0.2-0.4 part of antioxidant;
0.2-0.4 part of light stabilizer;
0.2-0.5 part of cross-linking agent;
the polyamide is prepared by the following method:
mixing the following components in parts by weight: dissolving 1 mol ratio of adipic acid and hexamethylenediamine in an aqueous solution, adding azetidine-2-carboxylic acid, uniformly mixing, wherein the addition amount of the azetidine-2-carboxylic acid is 0.8-1wt% of the adipic acid, carrying out polycondensation reaction at 250-260 ℃ and 1.5MPa, and simultaneously pumping water in a reaction system for reaction for 8 hours to obtain polyamide;
the specification of the glass fiber powder is 500-800 meshes;
the organic nucleating agent is selected from benzene phosphonate or fatty acid amide;
the polypropylene has a melt flow rate of less than 5g/10min, as measured according to ASTM D1238 at 230 ℃ under 2.16 kg.
2. The impact-resistant composition of claim 1, wherein:
the maleic anhydride grafted polypropylene is prepared by the following method:
mixing 100 parts by weight of polypropylene and 1-1.5 parts by weight of maleic anhydride, adding 0.4-1 part of di-tert-butyl peroxide and 0.5-1 part of styrene, uniformly mixing, adding into a screw extruder, and performing extrusion granulation to obtain the maleic anhydride grafted polypropylene.
3. The impact-resistant composition of claim 1 or 2, wherein:
the antioxidant is selected from one or more of pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], dilauryl thiodipropionate, tris (4-nonylphenyl) phosphite and triphenyl phosphite.
4. The impact-resistant composition of claim 1 or 2, wherein:
the light stabilizer is hindered amine light stabilizer or benzoate ultraviolet absorbent, and the cross-linking agent is methyl orthosilicate or trimethoxy silane.
5. The impact-resistant composition of claim 4, wherein:
the light stabilizer is 2, 6-tetramethyl-4-piperidine stearate.
6. A process for the preparation of an impact-resistant composition according to any one of claims 1 to 5, characterized in that it comprises the following steps:
the polyamide, the maleic anhydride grafted polypropylene, the glass fiber powder, the organic nucleating agent, the antioxidant, the light stabilizer and the crosslinking agent are uniformly mixed according to the weight ratio, and are extruded by a double-screw extruder, the temperature of the double-screw extruder is set to be 180-200 ℃, and the composition is obtained by granulation.
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