CN107955367B - High-fatigue-resistance nylon composite material for office chair and preparation method thereof - Google Patents

High-fatigue-resistance nylon composite material for office chair and preparation method thereof Download PDF

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CN107955367B
CN107955367B CN201711190228.1A CN201711190228A CN107955367B CN 107955367 B CN107955367 B CN 107955367B CN 201711190228 A CN201711190228 A CN 201711190228A CN 107955367 B CN107955367 B CN 107955367B
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polyamide
inorganic mineral
mineral powder
parts
silane coupling
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CN107955367A (en
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王晓群
尹城龙
黄珂伟
陈家锋
肖敏
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HANGZHOU JINZHOU POLYMER TECHNOLOGY CO LTD
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HANGZHOU JINZHOU POLYMER TECHNOLOGY CO LTD
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/02Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/92Measuring, controlling or regulating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92504Controlled parameter
    • B29C2948/92704Temperature
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Abstract

A high fatigue resistance nylon composite material for office chairs and a preparation method thereof belong to the technical field of high polymer materials. The nylon composite material is prepared by melting and extruding polyamide, a chain extender, an auxiliary agent and inorganic mineral powder modified by a silane coupling agent through a double-screw extruder. The method has the advantages of simple operation and convenient processing, and the material has excellent mechanical properties, good appearance, low production cost and other excellent properties.

Description

High-fatigue-resistance nylon composite material for office chair and preparation method thereof
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a high fatigue resistance nylon composite material for office chairs and a preparation method thereof.
Background
Nylon 6 is one of the engineering plastics prepared by polycondensing caprolactam. At present, the product has a wider application and larger dosage due to the lower melting point and wider processing technology range; meanwhile, the lubricating oil has the characteristics of good self-lubricating property, excellent oil resistance, heat resistance, high mechanical strength and the like, so that the lubricating oil is widely applied to products in various industries.
However, nylon 6 has its significant disadvantages, such as higher water absorption and poor dimensional stability of the product parts. In order to meet the market demand, overcome the inherent defects of nylon 6, and improve the physical properties and reduce the development cost of nylon 6 become common concerns.
Inorganic fillers are increasingly used in polymer modified materials due to their low cost and excellent special properties. For example, Asahikase corporation developed 40% glass fiber filled nylon 6 composites; the golden hair company developed a 40% kaolin filled nylon 66 composite. Although the above products meet some requirements, their further scope of application is limited by the drawbacks and technical bottlenecks of their inorganic fillers. Such as warpage, severe wear to the mold, and surface whitening of glass fiber filled nylon 6 composites, especially thin-walled parts. Although the 40% kaolin-filled nylon 66 composite material improves the problem of buckling deformation and improves the impact strength, inorganic mineral powder such as kaolin is a hydrophilic and oleophobic non-metallic mineral, and the compatibility between unmodified inorganic filler and high molecular interfaces such as nylon is poor, so that the elongation at break of the composite material is low, so that the formed product has poor bending resistance and is easy to break and break, the service cycle and the service conditions of the product are greatly reduced, particularly the product which is repeatedly bent and used by people like a small table board on an office chair is fed back by the market, and whether the toughness of the product concerned by customers is enough is greatly related to the elongation at break of the material and not just the impact strength in the traditional sense. Meanwhile, because inorganic mineral powder has addition saturation in resin and self oil absorption characteristics, the appearance of the surface of the highly-filled mineral powder nylon can generate a lot of whitish silver filaments, so the mineral powder nylon cannot be used as an appearance part. Therefore, in order to meet the market demand, the development of a nylon composite material with high strength, high fatigue resistance and good appearance is a matter which needs to be solved urgently.
Disclosure of Invention
Aiming at the problems in the prior art and aiming at solving the problems, the technical scheme of the high fatigue resistance nylon composite material for the office chair is designed and provided, the scheme has the advantages of simple operation and convenient processing, and the material has excellent mechanical properties, good appearance, low production cost and other excellent properties.
In order to achieve the purpose, the invention adopts the technical scheme that:
the high fatigue-resistant nylon composite material for the office chair is characterized in that: the nylon composite material is prepared by melting and extruding polyamide, a chain extender, an auxiliary agent and inorganic mineral powder modified by a silane coupling agent through a double-screw extruder.
The high fatigue-resistant nylon composite material for the office chair is characterized in that: the nylon composite material is prepared from the following raw materials in parts by weight: 50-70 parts of polyamide, 30-60 parts of inorganic mineral powder, 1-3 parts of chain extender and 1-2 parts of auxiliary agent.
The high fatigue-resistant nylon composite material for the office chair is characterized in that: the polyamide is as follows: polyamide 6 having a viscosity of 2.8 and a melting point of 215 ℃ and polyamide 612 having a viscosity of 2.0 and a melting point of 120 ℃.
The high fatigue-resistant nylon composite material for the office chair is characterized in that: the inorganic mineral powder is one or more than one compound of mica, wollastonite, talcum powder, calcium carbonate, barium sulfate, kaolin and alumina which are modified by a silane coupling agent with the granularity of 4000 meshes or more.
The high fatigue-resistant nylon composite material for the office chair is characterized in that: the chain extender comprises: one or more than one mixture of epoxy compound, alternating copolymer of maleic anhydride and ethylene and isocyanate, and preferably chain extender which plays a role in three-dimensional crosslinking in polyamide resin.
the high fatigue resistance nylon composite material for office chairs is characterized in that the silane coupling agent is one or a mixture of more than one of glycidoxypropyltrimethoxysilane, aminopropyltriethoxysilane and vinyl tri (β -methoxyethoxy) silane.
The high fatigue-resistant nylon composite material for the office chair is characterized in that: the auxiliary agent is one or a mixture of more than one of an antioxidant, a weather-resistant agent and a flow modifier;
the antioxidant comprises one or more than one of β (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, 1,3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) 2,4, 6-trimethylbenzene and 4,4' -butylidene bis (6-tert-butyl-3-methylphenol) (330);
the weather-resistant agent comprises: one or more of 2- (2' -hydroxy-3 ',5' -bis (a, a-dimethylbenzyl) phenyl) benzotriazole, 2- (2' -hydroxy-3 ',5' -di-tert-butylphenyl) -benzotriazole, 2' -methylenebis (4-tert-octyl-6-benzotriazolylphenol), and mixtures thereof;
the flow modifier comprises: one or more than one of amino-terminated aromatic hyperbranched polyester and carboxyl-terminated aromatic hyperbranched polyester.
The preparation method of the high fatigue resistance nylon composite material for the office chair is characterized by comprising the following steps:
(1) treating the surface of inorganic mineral powder by using a silane coupling agent, namely adding 80-90 parts of inorganic mineral powder and 10-20 parts of alcohol into a mixing machine, stirring and mixing at a low speed for 2-5 minutes to ensure that the alcohol is fully absorbed by the inorganic mineral powder, then adding 1-3 parts of the silane coupling agent into the mixing machine, heating to 80-90 ℃, stirring at a high speed for 10-20 minutes, hydrolyzing the silane coupling agent under the action of heating and alcohol, performing coupling reaction with hydroxyl on the surface of the inorganic mineral powder, and drying powder at 90-100 ℃ in a powder drying device to obtain silane coupling agent modified inorganic mineral powder;
(2) mixing polyamide 6, chain extender and silane coupling agent modified inorganic mineral powder by 45-60 parts of polyamide, 1-3 parts of chain extender and 30-60 parts of inorganic mineral powder for 10-20 minutes by a mixer to obtain a uniform mixture;
(3) heating each section of the double-screw extruder to 220-260 ℃, putting the mixture into a main feeding barrel of the double-screw extruder, respectively putting 1-2 parts of an auxiliary agent and 6125-10 parts of polyamide into a side feeding barrel 1 and a side feeding barrel 2, setting the feeding speed of each barrel according to the yield of 150-200 kg/h, extruding material filaments by the double-screw extruder, cooling, air-drying and dicing to obtain the polyamide modified material, wherein the temperature of 7 sections and later is reduced by 20 ℃ after the double-screw extruder works for 10-20 minutes.
The preparation method of the high fatigue resistance nylon composite material for the office chair is characterized by comprising the following steps of: in the step (1), the low-speed stirring speed is 450r/min, the alcohol is industrial alcohol with the purity of 95%, and the high-speed stirring speed is 1200 r/min.
The preparation method of the high fatigue resistance nylon composite material for the office chair comprises the following steps that (3) a double-screw extruder is a 50-machine extruder, a side feeding port is arranged on the edge of a 6-zone of the double-screw extruder, and the selected double screws are formed by combining screws with strong shearing; the cooling device for cooling is a circulating water tank with the temperature of 50-80 ℃; the equipment for granulating is a granulator with the rotating speed set to 600-800 r/min.
Compared with the prior art, the invention has the following advantages and excellent effects:
1) the processing method of the modified inorganic mineral powder adopted by the invention is simple and strong in operability, and meanwhile, the process can improve the grafting rate and the distribution uniformity of the modified inorganic mineral powder under the same dosage of the silane coupling agent, and uniformly covers a layer of organic polymer film on the surface of the inorganic mineral powder, so that the lipophilicity of the modified inorganic mineral powder is increased to the maximum extent, and the adding proportion of the modified inorganic mineral powder in nylon and the mechanical property of a composite material are greatly improved.
2) The polyamide 6 and the polyamide 612 used in the present invention have their particularity, and it is preferable that the polyamide 6 has a viscosity of 2.8 and a melting point of 215 ℃ and the polyamide 612 has a viscosity of 2.0 and a melting point of 120 ℃. In the composite material, polyamide 6 plays a role of resin coating, polyamide 612 plays a role of a surface improver, polyamide 612 with lower viscosity and temperature is easier to extend to the surface of a product part in the injection molding process, and an apparent resin layer is formed on the surface of the part, so that the phenomenon of silver wire whitening caused by too high powder addition is greatly improved in appearance, and compared with a material without polyamide 612, the composite material has better and wider coloring and dyeing effects, so that the product is finally formed into a sandwich biscuit form with a reinforced middle structure and a good surface appearance, and meanwhile, different from a polyamide breaking agent in the current market, polyamide 612 is a high-molecular polymer and belongs to a polyamide series, so that the composite material has better compatibility with polyamide 6, and the physical strength of the composite material cannot be reduced; meanwhile, the hyperbranched polymer and the polyamide 612 added into the compound act synergistically to better disperse the inorganic mineral powder and improve the fluidity and the surface gloss of a compound system of the compound.
3) The extrusion process operation adopts side feeding and sectional feeding, the mixed inorganic mineral powder, polyamide 6 and chain extender are fed from a main feeding port, the materials are melted and blended in a screw area of a 1-5 section, and the physical blending and the chemical reaction are realized, so that the uniform mixing of the modified inorganic mineral powder and the polyamide 6 can be better realized by using the temperature setting method and the rotating speed setting method of the extruder in the 1-5 section, and meanwhile, the amino group on the silane coupling agent combined with the inorganic mineral powder can react with the carboxyl group on the polyamide to play a role in chemical bonding; the coupling agent thin layer covered on the surface of the inorganic mineral powder can also play a role of uniformly dispersing on the polyamide 6, and the surface stress between the inorganic mineral powder and the polyamide 6 is reduced. Therefore, the addition amount of the chain extender is improved to the maximum extent, meanwhile, the chain extender and the polyamide 6 start a three-dimensional crosslinking chemical reaction in a section of 1-5, the chemical crosslinking reaction can be generated in a short time by setting the extrusion temperature and the screw rotation speed, a microscopic local network structure is formed, the inorganic mineral powder is wrapped by the polyamide 6 with the local network structure, and a good effect of strengthening and toughening is achieved. At the same time, polyamide 612 is fed from the side feed port of zone 6, and only physical mixing of the materials is performed. By adopting the side feeding method, the cross-linking reaction of the polyamide 612 and the modified inorganic mineral powder and the chain extender which have already reacted can be effectively inhibited, the polyamide 612 is not captured by the networked polyamide 6, and the polyamide 612 can be exerted in the injection molding process only by adopting the sectional feeding mode. This also provides a new design concept for laminated sheet profiles, namely one-shot injection moulding.
4) The extrusion process operation adopts a time-interval temperature control method, namely, the temperature of the section 7 of the double-screw extruder and the subsequent temperature is reduced by 20 ℃ on the original basis after extrusion granulation is carried out for 10-20 minutes. The reason is that the viscosity of the composite material added with the modified inorganic mineral powder is relatively high when the composite material is melted and mixed in the screw, the heat generated by friction with the screw is more obvious than common general materials such as polypropylene and the like, and the instantaneous temperature of the material and the wall of the screw is very high under the high-pressure environment in the barrel of the extruder, so that the decomposition of resin is easily caused, and the apparent performance is reduced. And after 10-20 minutes, the temperature of the zone 7-10 of the extruder is reduced, so that the degradation of the resin can be effectively reduced.
5) The invention adopts the common use of inorganic mineral powder, polyamide and other raw materials to prepare the high fatigue-resistant polyamide material, improves the toughness, repeated bending property and good surface appearance of the product on the premise of ensuring high rigidity of the product, expands the application range of the product, realizes the replacement of steel by plastic and light weight, and is particularly used for parts such as office chairs and the like which need large gravity compression and bending for a long time.
Detailed Description
The present invention is further illustrated by the following examples. The parts used in the invention are parts by weight.
In the present invention, the polyamide 612 is mainly used for improving the appearance of the composite material without sacrificing the polyamide 6 per se; the chain extender mainly forms a local three-dimensional cross-linking network of polyamide 6, plays a role in coating inorganic mineral powder and further improves the mechanical property of the material; the method of side feeding mouth feeding and time-sharing temperature control of the double screw extruder is mainly to give play to the maximum mechanical property and the appearance effect of the composite material. The double-screw extruder adopted by the invention is a 50-screw extruder, the side feeding port is arranged on the edge of the 6-zone of the double-screw extruder, and the selected double screws are formed by combining the screws with strong shearing; the cooling device for cooling is a circulating water tank with the temperature of 50-80 ℃; the equipment for granulating is a granulator with the rotating speed set to 600-800 r/min.
Comparative example
(1) Polyamide 6, inorganic mineral powder (mica), and a commercially available maleic anhydride grafted ethylene octene copolymer were mixed in a 55: 40: 5, mixing for 10 minutes by a mixer to obtain a uniform mixture;
(2) heating each section of the double-screw extruder to 220-260 ℃, wherein the specific data comprises 220 ℃ in the first zone, 230 ℃ in the second zone, 250 ℃ in the third zone, 255 ℃ in the fourth zone, 250 ℃ in the fifth zone, 255 ℃ in the sixth zone, 255 ℃ in the seventh zone, 250 ℃ in the eighth zone, 250 ℃ in the ninth zone and 260 ℃ in the tenth zone, putting the mixture into a main feeding port, setting the feeding speed of a feeding cylinder according to the output of 150kg/h, extruding material filaments by the double-screw extruder, cooling, air-drying and dicing to obtain the polyamide modified material. Wherein, after extrusion granulation is carried out for 20 minutes, the temperature of the section 7 of the double-screw extruder and the subsequent temperature are reduced by 20 ℃ on the original basis, namely 220 ℃ in the first zone, 230 ℃ in the second zone, 250 ℃ in the third zone, 255 ℃ in the fourth zone, 250 ℃ in the fifth zone, 255 ℃ in the sixth zone, 235 ℃ in the seventh zone, 230 ℃ in the eighth zone, 230 ℃ in the ninth zone and 240 ℃ in the tenth zone.
In the comparative example, one or more of mica, wollastonite, talcum powder, calcium carbonate, barium sulfate, kaolin and alumina can be used as the inorganic mineral powder.
Example 1
(1) Treating the surface of inorganic mineral powder by using an aminated silane coupling agent (glycidyl ether oxypropyltrimethoxysilane), adding 80 parts of inorganic mineral powder (mica) and 20 parts of 95% alcohol into a mixer, stirring at a low speed (450 r/min) for 3 minutes to ensure that the alcohol is fully absorbed by the inorganic mineral powder, then adding 1 part of silane coupling agent into the mixer, heating to 90 ℃, stirring at a high speed (1200 r/min) for 10 minutes, hydrolyzing the silane coupling agent under the action of heating and alcohol, performing coupling reaction with hydroxyl on the surface of the inorganic mineral powder, and drying the powder in powder drying equipment at 100 ℃ to obtain silane coupling agent modified inorganic mineral powder;
(2) polyamide 6, a chain extender (alternating copolymer of maleic anhydride and ethylene) and inorganic mineral powder are mixed according to a ratio of 52:1: mixing the materials for 10 minutes by a mixer according to the proportion of 40 to obtain a uniform mixture;
(3) heating each section of the double-screw extruder to 220-260 ℃, wherein the specific data comprises that the first zone is 220 ℃, the second zone is 230 ℃, the third zone is 250 ℃, the fourth zone is 255 ℃, the fifth zone is 250 ℃, the sixth zone is 255 ℃, the seventh zone is 255 ℃, the eighth zone is 250 ℃, the ninth zone is 250 ℃ and the tenth zone is 260 ℃, putting 93 parts of the mixture into a main feeding barrel of the double-screw extruder, putting 2 parts of an auxiliary agent (β (3, 5-di-tert-butyl-4-hydroxyphenyl) pentaerythritol propionate: 2- (2' -hydroxy-3 ',5' bis (a, a-dimethylbenzyl) phenyl) benzotriazole: amino-terminated aromatic hyperbranched polyester =1:1: 2) and 5 parts of polyamide 612 into a side feeding barrel 1 and a side feeding barrel 2 respectively, setting the output of each feeding barrel according to the formula ratio according to 150kg/h, extruding material wires by the double-screw extruder, cooling, air drying, and granulating to obtain a polyamide modified material, wherein the temperature of 7 sections of the double-screw extruder and the subsequent temperature of the original double-screw extruder are reduced by 20 ℃ on the basis, namely the first zone is 255 ℃, the first zone is 230 ℃, the temperature of the fifth zone is 230 ℃, the sixth zone is 230 ℃, and the ninth zone is 230 ℃.
In this embodiment, the inorganic mineral powder may also be one or more of mica, wollastonite, talc, calcium carbonate, barium sulfate, kaolin, and alumina.
Example 2
(1) Treating the surface of inorganic mineral powder by using an aminated silane coupling agent (aminopropyltriethoxysilane), adding 80 parts of inorganic mineral powder (mica) and 20 parts of 9% alcohol into a mixing machine, stirring at a low speed (450 r/min) for 3 minutes to ensure that the alcohol is fully absorbed by the inorganic mineral powder, then adding 2 parts of silane coupling agent into the mixing machine, heating to 90 ℃, stirring at a high speed (1200 r/min) for 10 minutes, hydrolyzing the silane coupling agent under the action of heating and alcohol, performing coupling reaction with hydroxyl on the surface of the inorganic mineral powder, and drying the powder in powder drying equipment at 100 ℃ to obtain silane coupling agent modified inorganic mineral powder;
(2) mixing polyamide 6, a chain extender (an epoxy compound: maleic anhydride and ethylene alternating copolymer =1: 1) and inorganic mineral powder in a mixer according to a ratio of 52:1:40 for 10 minutes to obtain a uniform mixture;
(3) heating each section of the double-screw extruder to 220-260 ℃, wherein the specific data comprises that a first zone is 220 ℃, a second zone is 230 ℃, a third zone is 250 ℃, a fourth zone is 255 ℃, a fifth zone is 250 ℃, a sixth zone is 255 ℃, a seventh zone is 255 ℃, an eighth zone is 250 ℃, a ninth zone is 250 ℃ and a tenth zone is 260 ℃, 93 parts of the mixture are put into a main feeding barrel of the double-screw extruder, 2- (2' -hydroxy-3 ',5' -di-tert-butylphenyl) -benzotriazole: carboxyl-terminated aromatic hyperbranched polyester =1:1: 2) 2 parts of an auxiliary agent (1, 3, 5-tri (3, 5-di-tert-butyl-4-hydroxybenzyl) and 5 parts of polyamide 612 are respectively put into a side feeding barrel 1 and a side feeding barrel 2, the feeding speeds of the feeding barrels are set according to the formula proportion and the output of 150kg/h, extruding material wires by a double-screw extruder, cooling, air-drying and granulating to obtain the polyamide modified material, wherein after extruding and granulating for 20 minutes, the temperature of the section 7 of the double-screw extruder and the subsequent temperature are reduced by 20 ℃ on the original basis, namely, the temperature of the section I is 220 ℃, the temperature of the section II is 230 ℃, the temperature of the section III is 250 ℃, the temperature of the section IV is 255 ℃, the temperature of the section V is 250 ℃, the temperature of the section VI is 255 ℃, the temperature of the section VII is 235 ℃, the temperature of the section VIII is 230 ℃, the.
In this embodiment, the inorganic mineral powder may also be one or more of mica, wollastonite, talc, calcium carbonate, barium sulfate, kaolin, and alumina.
Example 3
(1) treating the surface of inorganic mineral powder by using an aminated silane coupling agent (vinyl tri (β -methoxyethoxy) silane), adding 80 parts of inorganic mineral powder (mica) and 20 parts of alcohol into a mixing machine, stirring at a low speed (450 r/min) for 3 minutes to ensure that the alcohol is fully absorbed by the inorganic mineral powder, then adding 2 parts of silane coupling agent into the mixing machine, heating to 90 ℃, stirring at a high speed (1200 r/min) for 10 minutes, hydrolyzing the silane coupling agent under the action of heating and alcohol, performing coupling reaction with hydroxyl on the surface of the inorganic mineral powder, and drying the powder in a powder drying device at 100 ℃ to obtain silane coupling agent modified inorganic mineral powder;
(2) polyamide 6 and chain extender (epoxy compound: alternating copolymer of maleic anhydride and ethylene)
: isocyanate =2:1: 1), inorganic mineral powder in a ratio of 51: 2: mixing the materials for 10 minutes by a mixer according to the proportion of 40 to obtain a uniform mixture;
(3) heating each section of the double-screw extruder to 220-260 ℃, wherein the specific data comprises that a first zone is 220 ℃, a second zone is 230 ℃, a third zone is 250 ℃, a fourth zone is 255 ℃, a fifth zone is 250 ℃, a sixth zone is 255 ℃, a seventh zone is 255 ℃, an eighth zone is 250 ℃, a ninth zone is 250 ℃ and a tenth zone is 260 ℃, putting 93 parts of the mixture into a main feeding barrel of the double-screw extruder, putting 2 parts of an auxiliary agent (4, 4 '-butylidene bis (6-tert-butyl-3-methylphenol: 2,2' -methylenebis (4-tert-octyl-6-benzotriazole phenol: carboxyl-terminated aromatic hyperbranched polyester =1:1: 2) and 5 parts of polyamide 612 into a side feeding barrel 1 and a side feeding barrel 2 respectively, setting the feeding speeds of the feeding barrels according to the formula proportion and the output of 150kg/h, extruding the material threads by the double-screw extruder, cooling, and air-drying and granulating to obtain the polyamide modified material, wherein after extrusion granulation is carried out for 20 minutes, the temperature of the section 7 of the double-screw extruder and the subsequent temperature are reduced by 20 ℃ on the original basis, namely 220 ℃ in the first zone, 230 ℃ in the second zone, 250 ℃ in the third zone, 255 ℃ in the fourth zone, 250 ℃ in the fifth zone, 255 ℃ in the sixth zone, 235 ℃ in the seventh zone, 230 ℃ in the eighth zone, 230 ℃ in the ninth zone and 240 ℃ in the tenth zone.
In this embodiment, the inorganic mineral powder may also be one or more of mica, wollastonite, talc, calcium carbonate, barium sulfate, kaolin, and alumina.
Example 4
(1) treating the surface of inorganic mineral powder by using an aminated silane coupling agent (glycidyl ether oxypropyltrimethoxysilane: aminopropyltriethoxysilane: vinyl tris (β -methoxyethoxy) silane =2:1: 1), adding 80 parts of inorganic mineral powder (mica) and 20 parts of alcohol into a mixing machine, stirring at a low speed (450 r/min) for 3 minutes to allow the alcohol to be fully absorbed by the inorganic mineral powder, then adding 2 parts of silane coupling agent into the mixing machine, heating to 90 ℃, stirring at a high speed (1200 r/min) for 10 minutes, hydrolyzing the silane coupling agent under the action of heating and alcohol, performing coupling reaction with hydroxyl on the surface of the inorganic mineral powder, and drying the powder in powder drying equipment at 100 ℃ to obtain silane coupling agent modified inorganic mineral powder;
(2) mixing polyamide 6, a chain extender (isocyanate) and inorganic mineral powder for 10 minutes by a mixer according to the proportion of 46:2:40 to obtain a uniform mixture;
(3) heating each section of the double-screw extruder to 220-260 ℃, wherein the specific data comprises that the first zone is 220 ℃, the second zone is 230 ℃, the third zone is 250 ℃, the fourth zone is 255 ℃, the fifth zone is 250 ℃, the sixth zone is 255 ℃, the seventh zone is 255 ℃, the eighth zone is 250 ℃, the ninth zone is 250 ℃ and the tenth zone is 260 ℃, putting 88 parts of the mixture into a main feeding barrel of the double-screw extruder, putting 2 parts of auxiliary agent (β (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid pentaerythritol ester: 2,2' -methylenebis (4-tert-octyl-6-benzotriazole phenol): amino-terminated aromatic hyperbranched polyester =1:1: 2) and 10 parts of polyamide 612 into a side feeding barrel 1 and a side feeding barrel 2 respectively, setting the feeding speed of each feeding barrel according to the formula proportion and the yield of 150kg/h, extruding material wires by the double-screw extruder, cooling, air drying and dicing to obtain a polyamide modified material, wherein the temperature of the 7 sections and the later sections of the double-screw extruder is reduced by 20 ℃ on the original basis, namely the first zone is 220 ℃, the second zone is 255 ℃, the sixth zone is 230 ℃, the ninth zone is 230 ℃ and the ninth zone is 230 ℃.
In this embodiment, the inorganic mineral powder may also be one or more of mica, wollastonite, talc, calcium carbonate, barium sulfate, kaolin, and alumina.
The following table 1 shows the physical property test control data of the test articles obtained by adding different amounts of the silane coupling agent, the chain extender and the polyamide 612 in examples 1 to 4:
TABLE 1
The experiments confirm that compared with the common reference example without any modification treatment and process improvement, the material of the invention has greatly improved basic physical properties of the material, meets the requirements of high strength and high toughness, has the tensile elongation at break of 38 percent when the addition amount of the inorganic mineral powder reaches 40 percent, and has the tensile elongation at break increased by 7 times under the condition of keeping the mechanical material equivalent compared with the common inorganic mineral powder nylon material added with the toughening agent, and the composite material has excellent surface gloss effect and the gloss is increased by 1 time, so that the material can also be applied to the appearance and functional parts of automobiles, electricians and the like with high performance requirements.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.

Claims (6)

1. The utility model provides a high antifatigue nylon composite for office chair which characterized in that: the nylon composite material is prepared by melting and extruding polyamide, a chain extender, an auxiliary agent and inorganic mineral powder modified by a silane coupling agent as raw materials through a double-screw extruder, and specifically comprises the following steps:
(1) treating the surface of inorganic mineral powder by using a silane coupling agent, namely adding 80-90 parts of inorganic mineral powder and 10-20 parts of alcohol into a mixing machine, stirring and mixing at a low speed for 2-5 minutes to ensure that the alcohol is fully absorbed by the inorganic mineral powder, then adding 1-3 parts of the silane coupling agent into the mixing machine, heating to 80-90 ℃, stirring at a high speed for 10-20 minutes, hydrolyzing the silane coupling agent under the action of heating and alcohol, performing coupling reaction with hydroxyl on the surface of the inorganic mineral powder, and drying powder at 90-100 ℃ in a powder drying device to obtain silane coupling agent modified inorganic mineral powder;
(2) mixing polyamide 6, chain extender and silane coupling agent modified inorganic mineral powder by 45-60 parts of polyamide, 1-3 parts of chain extender and 30-60 parts of inorganic mineral powder for 10-20 minutes by a mixer to obtain a uniform mixture;
(3) heating each section of a double-screw extruder to 220-260 ℃, putting the mixture into a main feeding barrel of the double-screw extruder, respectively putting 1-2 parts of an auxiliary agent and 6125-10 parts of polyamide into a side feeding barrel 1 and a side feeding barrel 2, setting the feeding speed of each barrel according to the yield of 150-200 kg/h, extruding material filaments by the double-screw extruder, cooling, air-drying and dicing to obtain a polyamide modified material, wherein the temperature of 7 sections and later is reduced by 20 ℃ on the original basis after the double-screw extruder works for 10-20 minutes;
the inorganic mineral powder is more than one of mica, wollastonite, talcum powder, calcium carbonate, barium sulfate, kaolin and alumina which are modified by a silane coupling agent with the granularity of 4000 meshes or more;
the chain extender comprises: more than one of epoxy compound, maleic anhydride and ethylene alternating copolymer and isocyanate;
the silane coupling agent is more than one of glycidoxypropyltrimethoxysilane, aminopropyltriethoxysilane and vinyl tri (β -methoxyethoxy) silane;
the auxiliary agent is more than one of an antioxidant, a weather-resistant agent and a flow modifier;
the antioxidant comprises more than one of pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], 1,3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) -2,4, 6-trimethylbenzene and 4,4' -butylidene bis (6-tert-butyl-3-methylphenol);
the weather-resistant agent comprises: 2- (2' -hydroxy-3 ',5' -bis (a, a-dimethylbenzyl) phenyl) benzotriazole, 2- (2' -hydroxy-3 ',5' -di-tert-butylphenyl) -benzotriazole, 2' -methylenebis (4-tert-octyl-6-benzotriazolylphenol);
the flow modifier comprises: more than one of amino-terminated aromatic hyperbranched polyester and carboxyl-terminated aromatic hyperbranched polyester.
2. The high fatigue resistance nylon composite material for office chairs according to claim 1, wherein the polyamide is: polyamide 6 having a relative viscosity of 2.8 and a melting point of 215 ℃ and polyamide 612 having a relative viscosity of 2.0 and a melting point of 120 ℃.
3. A preparation method of a high fatigue resistance nylon composite material for office chairs is characterized by comprising the following steps:
(1) treating the surface of inorganic mineral powder by using a silane coupling agent, namely adding 80-90 parts of inorganic mineral powder and 10-20 parts of alcohol into a mixing machine, stirring and mixing at a low speed for 2-5 minutes to ensure that the alcohol is fully absorbed by the inorganic mineral powder, then adding 1-3 parts of the silane coupling agent into the mixing machine, heating to 80-90 ℃, stirring at a high speed for 10-20 minutes, hydrolyzing the silane coupling agent under the action of heating and alcohol, performing coupling reaction with hydroxyl on the surface of the inorganic mineral powder, and drying powder at 90-100 ℃ in a powder drying device to obtain silane coupling agent modified inorganic mineral powder;
(2) mixing polyamide 6, chain extender and silane coupling agent modified inorganic mineral powder by 45-60 parts of polyamide, 1-3 parts of chain extender and 30-60 parts of inorganic mineral powder for 10-20 minutes by a mixer to obtain a uniform mixture;
(3) heating each section of a double-screw extruder to 220-260 ℃, putting the mixture into a main feeding barrel of the double-screw extruder, respectively putting 1-2 parts of an auxiliary agent and 6125-10 parts of polyamide into a side feeding barrel 1 and a side feeding barrel 2, setting the feeding speed of each barrel according to the yield of 150-200 kg/h, extruding material filaments by the double-screw extruder, cooling, air-drying and dicing to obtain a polyamide modified material, wherein the temperature of 7 sections and later is reduced by 20 ℃ on the original basis after the double-screw extruder works for 10-20 minutes;
the inorganic mineral powder is more than one of mica, wollastonite, talcum powder, calcium carbonate, barium sulfate, kaolin and alumina which are modified by a silane coupling agent with the granularity of 4000 meshes or more;
the chain extender comprises: more than one of epoxy compound, maleic anhydride and ethylene alternating copolymer and isocyanate;
the silane coupling agent is more than one of glycidoxypropyltrimethoxysilane, aminopropyltriethoxysilane and vinyl tri (β -methoxyethoxy) silane;
the auxiliary agent is more than one of an antioxidant, a weather-resistant agent and a flow modifier;
the antioxidant comprises more than one of pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], 1,3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) -2,4, 6-trimethylbenzene and 4,4' -butylidene bis (6-tert-butyl-3-methylphenol);
the weather-resistant agent comprises: 2- (2' -hydroxy-3 ',5' -bis (a, a-dimethylbenzyl) phenyl) benzotriazole, 2- (2' -hydroxy-3 ',5' -di-tert-butylphenyl) -benzotriazole, 2' -methylenebis (4-tert-octyl-6-benzotriazolylphenol);
the flow modifier comprises: more than one of amino-terminated aromatic hyperbranched polyester and carboxyl-terminated aromatic hyperbranched polyester.
4. The preparation method of the high fatigue resistance nylon composite material for office chairs according to claim 3, wherein the preparation method comprises the following steps: in the step (1), the low-speed stirring speed is 450r/min, the alcohol is industrial alcohol with the purity of 95%, and the high-speed stirring speed is 1200 r/min.
5. The preparation method of the high fatigue resistance nylon composite material for office chairs according to claim 3, wherein the preparation method comprises the following steps: the polyamide is: polyamide 6 having a relative viscosity of 2.8 and a melting point of 215 ℃ and polyamide 612 having a relative viscosity of 2.0 and a melting point of 120 ℃.
6. The preparation method of the high fatigue resistance nylon composite material for office chairs according to claim 3, wherein the twin-screw extruder in the step (3) is a 50-screw extruder, the side feeding port is arranged at the edge of the 6-zone of the twin-screw extruder, and the selected twin-screws are formed by combining screws with strong shearing force; the cooling device for cooling is a circulating water tank with the temperature of 50-80 ℃; the equipment for granulating is a granulator with the rotating speed set to 600-800 r/min.
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