CN108587139B - Anti-pollution reinforced nylon composite material, preparation method thereof and application thereof in preparation of bathroom products - Google Patents
Anti-pollution reinforced nylon composite material, preparation method thereof and application thereof in preparation of bathroom products Download PDFInfo
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- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/10—Reinforcing macromolecular compounds with loose or coherent fibrous material characterised by the additives used in the polymer mixture
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
- C08K5/526—Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/14—Glass
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L29/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
- C08L29/02—Homopolymers or copolymers of unsaturated alcohols
- C08L29/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/02—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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic 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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Abstract
The invention discloses an anti-pollution reinforced nylon composite material, a preparation method thereof and an anti-pollution reinforced nylon composite material applied to preparation of bathroom products, wherein the reinforced nylon composite material comprises raw materials of nylon, inorganic filler and polyvinyl alcohol, and the nylon is selected from nylon 6. The invention discloses an anti-pollution reinforced nylon composite material, which avoids the problem of precipitation caused by the addition of a small-molecule antibacterial agent by adding polyvinyl alcohol; the prepared reinforced nylon composite material has long-term pollution resistance, excellent mechanical property and thermal aging resistance, and can be used for preparing bathroom products.
Description
Technical Field
The invention relates to the field of nylon composite materials and preparation thereof, in particular to an anti-pollution reinforced nylon composite material, a preparation method thereof and application thereof in preparation of bathroom products.
Background
Sanitary products include faucets, water pipes, basins and the like, which are used in environments with high humidity, high heat and high pressure and are beautiful. Therefore, the material has high requirements on rigidity and toughness, easy cleaning, environmental protection, temperature resistance and surface electroplating.
At present, most of materials for bathroom products are made of three materials, namely ceramic, metal and plastic. Wherein, the ceramic has large brittleness and is easy to break; the metals mainly adopt stainless steel and copper, but the metals contain heavy metal lead, so that the environment is not environment-friendly. Based on the significant defects of the above two materials, the preparation of bathroom products by using plastics is the focus of current research.
The common plastic for the bathroom comprises polypropylene, which is one of the most common general plastics, has low price, mechanical properties basically meeting the use requirements of the bathroom material, but the appearance of the plastic can be electroplated after special treatment, and the plastic is easy to cause pollution after long-time use, so the plastic is not an ideal choice. At present, there are also studies to improve the antibacterial property by adjusting the formulation. For example, chinese patent publication No. CN 106397965a discloses an antibacterial polypropylene material and a preparation method thereof, wherein the antibacterial polypropylene material comprises the following raw materials: 75-80 parts of polypropylene, 7-10 parts of a composite antibacterial agent, 4-8 parts of activated carbon, 2-5 parts of chlorinated polypropylene and 0.2-0.5 part of polyethylene wax, wherein the composite antibacterial agent comprises the following specific components: 15-25 parts of nano zeolite, 20-30 parts of polyhexamethylene guanidine, 12-22 parts of N- (trichloromethylthio) phthalimide and 1-1.2 parts of nano silver powder. The polypropylene material prepared by the formula has a good antibacterial effect and is suitable for manufacturing sanitary ware. However, the formula has more components and is complex and not suitable for actual production; and the formulation still cannot solve the problem that polypropylene is difficult to electroplate.
Therefore, the development of other kinds of plastics for bathroom materials is a problem to be solved.
The nylon has the advantages of light weight, no toxicity, corrosion resistance, excellent processing and forming, good mechanical property and the like, and is widely applied to the industrial fields of modern automobiles, electric appliances and the like. In addition, the nylon has large surface polarity, and can be electroplated without special treatment, thereby providing possibility for applying the nylon in bathroom products.
As disclosed in chinese patent publication No. CN 102351462 a, a kunlun spar composite material, a sanitary equipment made of the kunlun spar composite material and a preparation method thereof are disclosed, the kunlun spar composite material comprises the following raw materials: kunlun spar, thermoplastic polymer, high-efficiency additive and antioxidant 1010. In the formula of the Kunlun spar composite material provided in embodiment 3, the adopted thermoplastic polymer is polyamide PA, the Kunlun spar comprises titanium dioxide, calcium carbonate and attapulgite, and the high-efficiency auxiliary agent comprises a flow modifier TAF, a fluorescent whitening agent and aramid fibers. The sanitary ware prepared by injection molding has the texture, strength and toughness of ceramic-like materials, but the strength of the material cannot be guaranteed, and the material is used for a long time, and an auxiliary agent in the material is easy to separate out, so that the sanitary ware is extremely harmful to the health of a human body.
Disclosure of Invention
The invention discloses an anti-pollution reinforced nylon composite material, which avoids the problem of precipitation caused by the addition of a small-molecule antibacterial agent by adding polyvinyl alcohol; the prepared reinforced nylon composite material has long-term pollution resistance, excellent mechanical property and thermal aging resistance, and can be used for preparing bathroom products.
The specific technical scheme is as follows:
an anti-pollution reinforced nylon composite material comprises raw materials of nylon, inorganic filler and polyvinyl alcohol; the nylon is selected from nylon 6.
Polyvinyl alcohol (PVA) has stable chemical property, and due to the existence of a large number of hydroxyl groups, the surface tension is large, the hydrophilicity is strong, so that the surface of the film has good pollution resistance, but pure PVA is easy to swell in water, has poor mechanical property and is difficult to process.
The nylon 6 has reasonable price, both rigidity and toughness, high surface polarity and better thermal aging performance, and is an ideal bathroom material.
According to the invention, the components with specific contents are combined, and the surface polarity of the composite material is greatly increased and the long-term anti-pollution performance of the composite material is also improved on the premise of ensuring the mechanical property by adding the industrial material PVA and screening specific nylon varieties.
In order to obtain a further advantageous effect of the invention, the following is preferably performed:
the relative viscosity of the nylon 6 is 2.4-2.8, and the melt index is 15-50 g/10min (GB/T3682-2000); more preferably, the melt index is 30-40 g/10min, and concretely, Xinhui Meida M2400 is adopted.
The inorganic filler is selected from chopped alkali-free glass fiber, wollastonite, talcum powder and the like. Preferably, the diameter of the glass fiber is 10 μm, the length of the glass fiber is 4.5mm, the surface impregnating agent is of a silane type, and 301HP short fiber produced by Chongqing glass fiber is specifically adopted.
The polyvinyl alcohol has a dynamic viscosity of 10-30 mPa · s and an alcoholysis degree of 92-98%. Further preferably, the viscosity is 22 to 30 mPas, the alcoholysis degree is 95 to 98%, and the density is 1.27 to 1.31g/cm3Specifically, PVA1798 produced by Anhui Wei group is adopted.
According to the preferable raw material variety, the anti-pollution reinforced nylon composite material further preferably comprises the following raw materials in percentage by weight:
635-65% of nylon;
30-60% of inorganic filler;
0.5-10% of polyvinyl alcohol.
Preferably, the raw material composition also comprises other auxiliary agents, and the auxiliary agents are selected from one or two of an antioxidant and a lubricant. The antioxidant is phosphite esters, preferably antioxidant 168; the lubricant is a stearate, preferably calcium stearate.
In percentage by weight, the anti-pollution reinforced nylon composite material preferably comprises the following raw materials:
most preferably, the anti-pollution reinforced nylon composite material comprises the following raw materials:
the invention also discloses a preparation method of the anti-pollution reinforced nylon composite material, which comprises the following steps:
uniformly mixing nylon 6, polyvinyl alcohol and other auxiliaries, adding the mixture into a double-screw extruder from a main feeding hopper, adding an inorganic filler into the double-screw extruder from a side feeding hopper, extruding the mixture by the double-screw extruder, and then carrying out water cooling, grain cutting and drying on the extruded mixture to obtain the anti-pollution reinforced nylon composite material.
Preferably, the mixing is carried out in a blender, provided that: the rotating speed is 500-800 r/min, and the time is 5-8 min; further preferably 700 rpm for 6 min.
The temperatures of the double-screw extruder from the feeding section to the first temperature area to the ninth temperature area of the machine head are respectively set to be 230-240 ℃, 240-250 ℃, 230-240 ℃, 220-230 ℃, 210-220 ℃ and the temperature of the die head is 220-230 ℃. More preferably 240 ℃, 250 ℃, 240 ℃, 230 ℃, 220 ℃, and 235 ℃ of the die head.
The anti-pollution reinforced nylon composite material prepared by the method has long-term anti-pollution performance, no micromolecules are separated out, the mechanical property and the heat-resisting aging performance are excellent, and the anti-pollution reinforced nylon composite material can be used for preparing bathroom products.
Compared with the prior art, the invention has the following advantages:
according to the invention, the inorganic filler is used for reinforcing PA6, and the excellent compatibility of PVA and PA6 is used, so that the surface polarity of the material is greatly increased on the premise of ensuring the mechanical property, the long-term pollution resistance of the material is improved, meanwhile, the micromolecules are basically not separated out, and the heat-resistant aging performance of the PA6 composite material is improved.
The preparation method of the PA6 reinforced material is simple, the industrial production is consistent with the existing common PA reinforced material, the subsequent large-scale production is easy to control, and the PA6 reinforced material has good economic benefit.
Detailed Description
The following examples and comparative examples are further illustrated in connection with the present invention.
In the formulations of the compositions of the examples and comparative examples, the PA6 was PA6 manufactured by Nippon Mada under the trade name M2400 and had a melt flow rate of 38g/10 min. The glass fiber is produced by international composite material for Chongqing, and the brand is 301 HP. The PVA is produced by Anhui vitamin group, and the commodity brand is PVA 1798. The antioxidant is 168 produced by Jinhai Yabao company. The lubricant is calcium stearate produced by Hangzhou grease chemical company.
The preparation method comprises the following steps:
adding a certain amount of nylon 6, PVA, an antioxidant and a lubricant into a stirring pot, uniformly mixing for 5min, then adding into a double-screw extruder from a main feeding hopper, and adding glass fiber into the double-screw extruder from a side feeding hopper. The temperatures of the twin-screw extruder from the feed zone to the first temperature zone to the ninth temperature zone of the head were set to 240 ℃, 250 ℃, 240 ℃, 230 ℃, 220 ℃ respectively, and the temperature of the die was 235 ℃. And extruding the mixture by a double-screw extruder, and then cooling, granulating and drying to obtain the anti-pollution reinforced nylon composite material.
The glass fiber reinforced nylon composite materials obtained in the examples and the comparative examples are processed into test sample bars through injection molding, and mechanical property test is carried out on the test sample bars. The specific test method is as follows:
tensile properties were tested according to ISO 527-2; bending performance testing was performed according to ISO 178; the impact strength of the notch of the simply supported beam is carried out according to ISO 179; the water absorption test was performed according to ISO 1110; surface tension is tested by adopting a dyne pen; the contact angle between the material and pure water was measured using a contact angle measuring instrument.
The test specimens were subjected to a long-term heat aging test. The specific test method is as follows:
the long term thermal stability of the samples was evaluated by exposing the test samples to a hot air aging oven at 150 ℃. The heat aging resistance test time for the composites disclosed herein was 1000 hours. After the test specimens were aged in a hot air cabinet, the tensile strength was tested according to ISO 527-2 test method; and testing the notch impact strength of the simply supported beam according to the ISO 179 testing method. And comparing the detection result after thermal aging with the unexposed reference substance to obtain the retention rate of each mechanical test item, so that the long-term heat-resistant stability of various components can be evaluated.
The test samples were subjected to a precipitation test and an anti-contamination test. The specific test method is as follows:
the method for measuring the precipitation rate comprises the following steps: taking a sample plate with the thickness of 3mm, weighing and recording as m0Standing the sample at 85 deg.C and 85% RH for 1000 hr, taking out, cleaning the surface, baking at 120 deg.C for 48 hr, weighing and recording as m, and separating out rate%0-m)/m0. The method for measuring the deposition rate of the pollutants comprises the following steps: first, 5L of 10g/L Bovine Serum Albumin (BSA) solution was prepared, and the comparative examples and examples were injection-molded into a circular tube shape and weighed as m0、m1、m2、m3、m4、m5、m6And connecting water pipes at two ends of the water pump with a water pump and a BSA solution in parallel, and starting the water pump to continuously run for 100 hours. Removing each round tube, baking at 120 deg.C for 48 hr, weighing, and recording as m0′、m1′、m2′、m3′、m4′、m5′、m6'. Comparative example pollutant deposition rate%0′-m0)/m0And so on for the examples. The method for measuring the decontamination rate comprises the following steps: firstly, preparing 5L of EDTA solution with pH of 11 solution, and respectively weighing the weight m of the round tube0′、m1′、m2′、m3′、m4′、m5′、m6' As the original weight, the water pipes connected at both ends were also connected in parallel with a water pump and EDTA solution, and the water pump was operated continuously for 100 hours. Removing each round tube, baking at 120 deg.C for 48 hr, weighing, and recording as m0″、m1″、m2″、m3″、m4″、m5″、m6". Comparative example decontamination factor% (% m)0′-m0″)/m0', examples, and so on.
The formulations of comparative examples and examples are shown in table 1, and the test results of the corresponding mechanical properties and other physical properties of comparative examples and examples are shown in tables 2 and 3:
table 1, formulation table for examples and comparative examples, wt.%
Table 2, test results of examples and comparative examples
TABLE 3 test results of the examples and comparative examples after 1000h heat aging at 170 deg.C
From the test results of examples and comparative examples, it can be seen that the higher the glass fiber content, the smaller the water absorption, and the more stable the article size. The addition of PVA has a slight influence on the water absorption rate and the mechanical property, the mechanical property is improved, the influence on the surface tension and the contact angle is larger, and the surface tension is increased and the contact angle is reduced along with the increase of the content of PVA. Under high temperature and high humidity, PVA molecular chains and PA6 molecular chains are intertwined together, so that the sample strips are not easy to separate out, and no small molecules are separated out basically, so that the long-term use of the sample strips has no influence on human health. With increasing PVA content, less contaminant was deposited on the surface of the injection molded round tube, and the remaining contaminants on the surface of the round tube after cleaning were also less. After the material is subjected to heat aging at 170 ℃ for 1000h, the heat aging resistance of the material is kept better along with the increase of the PVA content.
Claims (5)
1. The application of the anti-pollution reinforced nylon composite material in preparing bathroom products is characterized in that the anti-pollution reinforced nylon composite material comprises the following raw materials in percentage by weight:
635-65% of nylon;
30-60% of inorganic filler;
0.5-10% of polyvinyl alcohol;
the nylon 6 has a relative viscosity of 2.4-2.8 and a melt index of 15-50 g/10min
The viscosity of the polyvinyl alcohol is 10-30 mPa.s, and the alcoholysis degree is 92-98%;
the preparation method of the anti-pollution reinforced nylon composite material comprises the following steps:
uniformly mixing nylon 6, polyvinyl alcohol and other selectively added additives, adding the mixture into a double-screw extruder from a main feeding hopper, adding an inorganic filler into the double-screw extruder from a side feeding hopper, extruding the mixture by the double-screw extruder, and then carrying out water cooling, grain cutting and drying on the extruded mixture to obtain the anti-pollution reinforced nylon composite material;
the temperatures of the double-screw extruder from the feeding section to the first temperature area to the ninth temperature area of the machine head are respectively set to be 230-240 ℃, 240-250 ℃, 230-240 ℃, 220-230 ℃, 210-220 ℃ and the temperature of the die head is 220-230 ℃.
2. Use according to claim 1, characterized in that the inorganic filler is chosen from alkali-free glass fibers, wollastonite or talc.
3. The use of claim 1, wherein the raw material composition further comprises other auxiliary agents selected from one or two of an antioxidant and a lubricant.
4. The application of claim 3, wherein the raw materials comprise, in weight percent:
5. the use according to claim 1, wherein the mixing conditions are: the rotating speed is 500-800 r/min, and the time is 5-8 min.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102597114A (en) * | 2009-07-30 | 2012-07-18 | 纳幕尔杜邦公司 | Heat aging resistant polyamide compositions including polyhydroxy polymers |
| CN103665857A (en) * | 2013-11-11 | 2014-03-26 | 青岛佰众化工技术有限公司 | Glass fiber reinforced polyvinyl alcohol-nylon 66 alloy material |
| CN106366554A (en) * | 2016-08-29 | 2017-02-01 | 合肥会通新材料有限公司 | PVA/ABS (polyvinyl acetate/acrylonitrile-butadiene-styrene) corrosion-resistant, high-tenacity and permanent antistatic composite material and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102597114A (en) * | 2009-07-30 | 2012-07-18 | 纳幕尔杜邦公司 | Heat aging resistant polyamide compositions including polyhydroxy polymers |
| CN103665857A (en) * | 2013-11-11 | 2014-03-26 | 青岛佰众化工技术有限公司 | Glass fiber reinforced polyvinyl alcohol-nylon 66 alloy material |
| CN106366554A (en) * | 2016-08-29 | 2017-02-01 | 合肥会通新材料有限公司 | PVA/ABS (polyvinyl acetate/acrylonitrile-butadiene-styrene) corrosion-resistant, high-tenacity and permanent antistatic composite material and preparation method thereof |
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