CN111019338A - Ultra-high specific gravity polyamide material and preparation method and application thereof - Google Patents
Ultra-high specific gravity polyamide material and preparation method and application thereof Download PDFInfo
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- CN111019338A CN111019338A CN201911344062.3A CN201911344062A CN111019338A CN 111019338 A CN111019338 A CN 111019338A CN 201911344062 A CN201911344062 A CN 201911344062A CN 111019338 A CN111019338 A CN 111019338A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/02—Making granules by dividing preformed material
- B29B9/06—Making granules by dividing preformed material in the form of filamentary material, e.g. combined with extrusion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
- B29C48/375—Plasticisers, homogenisers or feeders comprising two or more stages
- B29C48/39—Plasticisers, homogenisers or feeders comprising two or more stages a first extruder feeding the melt into an intermediate location of a second extruder
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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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
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
Abstract
The invention belongs to the technical field of modification of polymer composite materials, and particularly relates to an ultrahigh specific gravity polyamide material and a preparation method and application thereof. The ultra-high specific gravity polyamide material mainly comprises the following components in percentage by mass: 5-20 wt% of polyamide resin, 5-10 wt% of polyethylene resin, 60-90 wt% of metal tungsten powder, 0.3-1 wt% of dispersing agent and 0.1-1 wt% of antioxidant. The ultra-high specific gravity polyamide material provided by the invention has the characteristics of excellent processing performance, balanced physical and mechanical properties and high specific gravity, can be formed into a product by an injection molding process, and can be applied to replace a metal material to manufacture a balancing weight of an instrument.
Description
Technical Field
The invention belongs to the technical field of modification of polymer composite materials, and particularly relates to an ultrahigh specific gravity polyamide material and a preparation method and application thereof.
Background
The high specific weight plastic is a typical application of replacing metal with plastic, and adopts high molecular material as base material, and adds high specific weight metal powder as filler, and utilizes the combination of different weight mixing ratios and materials to regulate the specific weight and physical and mechanical properties of the product. In recent years, high specific gravity materials have important applications in electromagnetic shielding and radiation protection because of the low temperature machine-shaping capability.
The invention patent CN100549071C discloses a preparation method of a new metal and plastic composite material. The patent discloses that a nontoxic radiation-proof shielding material with adjustable density and capable of injection molding is obtained by carrying out continuous heating ball milling, double-screw mixing, double-roller extrusion open mixing, cooling and granulating on 60-95 wt% of metal tungsten powder, 5-40 wt% of resin, 0.02-1 wt% of stearic acid and the like. The process can prepare the polymer composite materials with different filling ratios, but has the problems of complex preparation process and difficult material molding under the condition of overhigh filling degree.
The invention patent CN103824605A discloses a plastic metal alloy composite material and a method for preparing a section bar by using the material, and the method obtains the composite material filled with high metal powder by a physical and chemical mixed radiation crosslinking mode for manufacturing a radiation-proof device. However, the product obtained by the process cannot be produced by an injection molding process, and the production efficiency is low.
The invention patent CN100595232C discloses a production method of high specific gravity resin, which comprises the steps of mixing tungsten powder, nylon PA powder and an auxiliary agent which are subjected to surface treatment in a double-screw extruder by a melting mixing extrusion molding process, feeding materials in a sectional metering manner, extruding the materials into sheets through a parallel streamline inner cavity die, and crushing the sheets to obtain high specific gravity resin particles. The technology can obtain the nylon composite material filled with the tungsten powder with high ratio, but the process is complex, the strength of the obtained product is low, and the application of the product is limited.
Disclosure of Invention
In order to overcome the defects and shortcomings in the prior art, the invention aims to provide the ultra-high specific gravity polyamide material. The material has simple process and balanced processing performance and physical and mechanical properties.
The invention also aims to provide a preparation method of the ultra-high specific gravity polyamide material.
The invention further aims to provide application of the ultra-high specific gravity polyamide material.
The purpose of the invention is realized by the following technical scheme:
an ultra-high specific gravity polyamide material is mainly composed of the following components in percentage by mass:
the sum of the mass percentages of the components is 100 percent.
The polyamide resin (PA) of the present invention is a resin base material containing an amide group in a repeating unit of a molecular main chain, and comprises: at least one of PA6, PA66, PA12, PA1012 and the like, wherein PA6 or PA12 is preferred, and PA6 is most preferred.
The amount of the polyamide resin added is 5 to 20 wt%, preferably 10 wt%.
The polyethylene resin is a thermoplastic resin prepared by polymerizing ethylene, wherein high-density polyethylene (HDPE) is preferred;
the addition amount of the polyethylene resin is 5-10 wt%.
The metal tungsten powder of the invention is metal tungsten powder with a certain size obtained by a hydrogenation reduction method, the particle size of the powder is preferably 4-7 μm, wherein W-9 and W-10 type tungsten powder (W-9 and W-10 respectively represent tungsten powder with the particle size of 4.50-4.99 μm and 5.00-6.99 μm) are preferred.
The dispersing agent is a macromolecular aid capable of improving the dispersibility of the inorganic filler in the polyamide base material, wherein the fluorine-containing polymer processing aid PPA is preferred in the invention.
The amount of the dispersant added is 0.3 to 1 wt%, preferably 0.5 wt%.
The antioxidant is prepared from the following components in percentage by mass of 1098 and 168: 2, and mixing the components.
The addition amount of the antioxidant is 0.4-1 wt%, and preferably 0.6 wt%.
The invention also comprises a preparation method of the ultra-high specific gravity polyamide material, which specifically comprises the following steps:
(1) weighing polyamide resin, polyethylene resin, a dispersing agent and an antioxidant according to a formula, and then adding the polyamide resin, the polyethylene resin, the dispersing agent and the antioxidant into a high-speed stirrer to stir for 5-10 minutes;
(2) adding the uniformly stirred materials into a single-screw extruder for preprocessing, controlling the temperature of each heating section of the extruder to be 180-250 ℃, and controlling the screw rotation speed of a main machine to be 200-300 r/min;
(3) adding the preprocessed material of the single screw into a main feeding port of a double-screw extruder connected in two, and adding the metal tungsten powder into the double-screw extruder through a side feeding port in a metering feeding mode to perform melt blending; the basic temperature of each zone of the double-screw extruder is 180-250 ℃, and the screw rotating speed of the main machine is 300-400 r/min;
(4) and extruding the materials by a double-screw extruder, and then carrying out water ring granulation and air cooling on the materials to obtain the ultra-high specific gravity polyamide material.
The ultra-high specific gravity polyamide material can be used for preparing products with different shapes and high specific gravity through a processing mode of injection molding. The product can be used for replacing metal materials to manufacture balancing weights of instruments and meters.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the formula design is optimized, and the surface treatment process of the metal tungsten powder is reduced;
(2) the processing method of double connection of the single-screw extruder and the double-screw extruder is adopted, so that the processing technology of the high-specific-gravity polyamide material is simplified;
(3) the balance of the processing performance and the physical and mechanical performance of the material is improved by optimizing the formula design;
(4) the ultra-high specific gravity polyamide material provided by the invention has the characteristics of excellent processing performance, balanced physical and mechanical properties and high specific gravity, can be formed into a product by an injection molding process, and can be applied to replace a metal material to manufacture a balancing weight of an instrument.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto. The raw materials related to the invention can be directly purchased from the market. For process parameters not specifically noted, reference may be made to conventional techniques.
Example 1
The preparation method of the ultra-high specific gravity polyamide material comprises the following specific steps:
(1) weighing raw materials according to the formula, 10 wt% of polyamide resin PA6 (Xinhui Meida PA6M2000), 5 wt% of high-density polyethylene (medium petrochemical HDPE2200J), 0.5 wt% of fluoropolymer processing aid PPA (3M, FX5920), 0.6 wt% of antioxidant (Ciba, 1098/168) and 83.9 wt% of metal tungsten powder. Then adding polyamide resin PA6 (New Meda PA6M2000), high density polyethylene (medium petrochemical HDPE2200J), fluoropolymer processing aid PPA (3M, FX5920) and antioxidant (Ciba, 1098/168) into a high-speed stirrer, and stirring for 5-10 minutes at the main engine rotating speed of 300 revolutions per minute.
(2) And adding the uniformly stirred materials into a single-screw extruder for preprocessing, controlling the temperature of each heating section of the extruder to be 220 +/-10 ℃, and controlling the screw rotation speed of a main machine to be 250 +/-10 r/min.
(3) After single-screw extrusion, the materials are directly metered into a main feeding port of a double-screw extruder for melt mixing, and 83.9 wt% of metal tungsten powder is fed from a side feeding port of the double-screw extruder in a metering feeding mode. The basic temperature of each zone of the double-screw extruder is 220 +/-10 ℃, and the screw rotating speed of the main machine is 350 +/-10 r/min.
(4) And after the melt blending is finished, the material is subjected to water ring granulation, air cooling and packaging to obtain the ultra-high specific gravity polyamide material.
Example 2
The preparation method of the ultra-high specific gravity polyamide material comprises the following specific steps:
(1) weighing raw materials according to the formula, 10 wt% of polyamide resin PA6 (Xinhui Mada PA6M2000), 10 wt% of high density polyethylene (medium petrochemical HDPE2200J), 0.5 wt% of fluoropolymer processing aid PPA (3M, FX5920), 0.6 wt% of antioxidant (Ciba, 1098/168) and 78.9 wt% of metal tungsten powder. Then adding polyamide resin PA6 (New Meda PA6M2000), high density polyethylene (medium petrochemical HDPE2200J), fluoropolymer processing aid PPA (3M, FX5920) and antioxidant (Ciba, 1098/168) into a high-speed stirrer, and stirring for 5-10 minutes at the main engine rotating speed of 300 revolutions per minute.
(2) And adding the uniformly stirred materials into a single-screw extruder for preprocessing, controlling the temperature of each heating section of the extruder to be 220 +/-10 ℃, and controlling the screw rotation speed of a main machine to be 250 +/-10 r/min.
(3) After single-screw extrusion, the materials are directly metered into a main feeding port of a double-screw extruder for melt mixing, and 79.9 wt% of metal tungsten powder is fed from a side feeding port of the double-screw extruder in a metering feeding mode. The basic temperature of each zone of the double-screw extruder is 220 +/-10 ℃, and the screw rotating speed of the main machine is 350 +/-10 r/min.
(4) And after the melt blending is finished, the material is subjected to water ring granulation, air cooling and packaging to obtain the ultra-high specific gravity polyamide material.
Example 3
The preparation method of the ultra-high specific gravity polyamide material comprises the following specific steps:
(1) weighing raw materials according to the formula, 10 wt% of polyamide resin PA6 (Xinhui Meida PA6M2000), 6 wt% of high-density polyethylene (medium petrochemical HDPE2200J), 0.5 wt% of fluoropolymer processing aid PPA (3M, FX5920), 0.6 wt% of antioxidant (Ciba, 1098/168) and 82.9 wt% of metal tungsten powder. Then adding polyamide resin PA6 (New Meda PA6M2000), high density polyethylene (medium petrochemical HDPE2200J), fluoropolymer processing aid PPA (3M, FX5920) and antioxidant (Ciba, 1098/168) into a high-speed stirrer, and stirring for 5-10 minutes at the main engine rotating speed of 300 revolutions per minute.
(2) And adding the uniformly stirred materials into a single-screw extruder for preprocessing, controlling the temperature of each heating section of the extruder to be 220 +/-10 ℃, and controlling the screw rotation speed of a main machine to be 250 +/-10 r/min.
(3) After single-screw extrusion, the materials are directly metered into a main feeding port of a double-screw extruder for melt mixing, and 82.9 wt% of metal tungsten powder is fed from a side feeding port of the double-screw extruder in a metering feeding mode. The basic temperature of each zone of the double-screw extruder is 220 +/-10 ℃, and the screw rotating speed of the main machine is 350 +/-10 r/min.
(4) And after the melt blending is finished, the material is subjected to water ring granulation, air cooling and packaging to obtain the ultra-high specific gravity polyamide material.
Comparative example 1
The preparation method of the ultra-high specific gravity polyamide material comprises the following specific steps:
(1) weighing raw materials according to the formula, 15 wt% of polyamide resin PA6 (New Zeeman PA6M2000), 0.5 wt% of fluoropolymer processing aid PPA (3M, FX5920), 0.6 wt% of antioxidant (Ciba, 1098/168) and 83.9 wt% of metal tungsten powder. Then adding polyamide resin PA6 (New Meda PA6M2000), high density polyethylene (medium petrochemical HDPE2200J), fluoropolymer processing aid PPA (3M, FX5920) and antioxidant (Ciba, 1098/168) into a high-speed stirrer, and stirring for 5-10 minutes at the main engine rotating speed of 300 revolutions per minute.
(2) And adding the uniformly stirred materials into a single-screw extruder for preprocessing, controlling the temperature of each heating section of the extruder to be 220 +/-10 ℃, and controlling the screw rotation speed of a main machine to be 250 +/-10 r/min.
(3) After single-screw extrusion, the materials are directly metered into a main feeding port of a double-screw extruder for melt mixing, and 83.9 wt% of metal tungsten powder is fed from a side feeding port of the double-screw extruder in a metering feeding mode. The basic temperature of each zone of the double-screw extruder is 220 +/-10 ℃, and the screw rotating speed of the main machine is 350 +/-10 r/min.
(4) And after the melt blending is finished, the material is subjected to water ring granulation, air cooling and packaging to obtain the ultra-high specific gravity polyamide material.
Comparative example 2
The preparation method of the ultra-high specific gravity polyamide material comprises the following specific steps:
(1) weighing the raw materials according to the formula, 10 wt% of polyamide resin PA6 (Xinhui Meida PA6M2000), 5 wt% of high-density polyethylene (medium petrochemical HDPE2200J), 0.6 wt% of antioxidant (Ciba, 1098/168) and 84.4 wt% of metal tungsten powder. Then adding polyamide resin PA6 (New Meda PA6M2000), high-density polyethylene (medium petrochemical HDPE2200J) and antioxidant (Ciba, 1098/168) into a high-speed stirrer, and stirring for 5-10 minutes at the main engine rotation speed of 300 revolutions per minute.
(2) And adding the uniformly stirred materials into a single-screw extruder for preprocessing, controlling the temperature of each heating section of the extruder to be 220 +/-10 ℃, and controlling the screw rotation speed of a main machine to be 250 +/-10 r/min.
(3) After single-screw extrusion, the materials are directly metered into a main feeding port of a double-screw extruder for melt mixing, and 84.4 wt% of metal tungsten powder is fed from a side feeding port of the double-screw extruder in a metering feeding mode. The basic temperature of each zone of the double-screw extruder is 220 +/-10 ℃, and the screw rotating speed of the main machine is 350 +/-10 r/min.
(4) And after the melt blending is finished, the material is subjected to water ring granulation, air cooling and packaging to obtain the ultra-high specific gravity polyamide material.
Results of Performance test of the ultra-high specific gravity Polyamide materials prepared in examples 1 to 3 and comparative examples 1 to 2
| Serial number | Appearance of the product | Density of | Fuse finger | Impact strength |
| Standard of merit | / | GB/T1033 | GB/T3682 | GB/T1843 |
| Unit of | / | g/cm3 | g/10min | KJ/m2 |
| Comparative example 1 | Is preferably used | 9.5 | ≥300 | 5 |
| Comparative example 2 | Roughness of | 9.7 | ≥300 | 8 |
| Example 1 | Good effect | 9.5 | ≥300 | 9 |
| Example 2 | Good effect | 9.2 | ≥300 | 9.5 |
| Example 3 | Good effect | 9.3 | ≥300 | 9 |
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The ultra-high specific gravity polyamide material is characterized by comprising the following components in percentage by mass:
the sum of the mass percentages of the components is 100 percent.
2. The ultra-high specific gravity polyamide material as claimed in claim 1, wherein the polyamide resin comprises: at least one of PA6, PA66, PA12 and PA 1012.
3. The ultra-high specific gravity polyamide material as claimed in claim 1, wherein the polyamide resin is added in an amount of 10 wt%.
4. The ultra-high specific gravity polyamide material as claimed in claim 1, wherein the polyethylene resin is high density polyethylene.
5. The ultra-high specific gravity polyamide material as claimed in claim 1, wherein the metal tungsten powder is a metal tungsten powder of a certain size obtained by a hydrogenation reduction method.
6. The ultra-high specific gravity polyamide material as claimed in claim 1, wherein the dispersant is a fluoropolymer processing aid PPA;
the addition amount of the dispersant is 0.5 wt%.
7. The ultra-high specific gravity polyamide material as claimed in claim 1, wherein the antioxidant is an antioxidant 1098 and an antioxidant 168, and the mass ratio of the antioxidant 1098 to the antioxidant 168 is 1: 2, and mixing;
the addition amount of the antioxidant is 0.4-1 wt%.
8. The method for preparing an ultra-high specific gravity polyamide material as claimed in any one of claims 1 to 7, characterized by comprising the steps of:
(1) weighing polyamide resin, polyethylene resin, a dispersing agent and an antioxidant according to a formula, and then adding the polyamide resin, the polyethylene resin, the dispersing agent and the antioxidant into a high-speed stirrer to stir for 5-10 minutes;
(2) adding the uniformly stirred materials into a single-screw extruder for preprocessing, and controlling the temperature of each heating section of the extruder to be 180-250 ℃;
(3) adding the preprocessed material of the single screw into a main feeding port of the double-screw extruder, and adding the metal tungsten powder into the double-screw extruder through a side feeding port for melt blending; the basic temperature of each zone of the double-screw extruder is 180-250 ℃;
(4) and extruding the materials by a double-screw extruder, and then carrying out water ring granulation and air cooling on the materials to obtain the ultra-high specific gravity polyamide material.
9. The method for preparing an ultrahigh-specific gravity polyamide material according to claim 8, wherein the main machine of the high speed mixer in step (1) rotates at a speed of 300 rpm; the screw rotating speed of the main machine of the single-screw extruder in the step (2) is 200-300 r/min; and (3) the rotating speed of the screws of the main machine of the double-screw extruder is 300-400 r/min.
10. Use of the ultra-high specific gravity polyamide material according to any one of claims 1 to 7 as a replacement for metal materials for making counter-weights for instruments and meters.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112322030A (en) * | 2020-09-10 | 2021-02-05 | 南京聚隆科技股份有限公司 | High-specific-gravity high-hardness strong magnetic attraction nylon material and preparation method thereof |
| CN113234270A (en) * | 2021-05-07 | 2021-08-10 | 江苏聚畔体育用品有限公司 | Mixed metal balancing weight and manufacturing method thereof |
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| JPS62212459A (en) * | 1986-03-12 | 1987-09-18 | Daiseru Hiyurusu Kk | Polyamide resin composition having high specific gravity |
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| JPS62212459A (en) * | 1986-03-12 | 1987-09-18 | Daiseru Hiyurusu Kk | Polyamide resin composition having high specific gravity |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112322030A (en) * | 2020-09-10 | 2021-02-05 | 南京聚隆科技股份有限公司 | High-specific-gravity high-hardness strong magnetic attraction nylon material and preparation method thereof |
| CN113234270A (en) * | 2021-05-07 | 2021-08-10 | 江苏聚畔体育用品有限公司 | Mixed metal balancing weight and manufacturing method thereof |
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