CN111040435A - Nylon carbon fiber composite powder material and preparation method thereof - Google Patents
Nylon carbon fiber composite powder material and preparation method thereof Download PDFInfo
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- 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
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
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- 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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- 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
- C08J2377/06—Polyamides derived from polyamines and polycarboxylic acids
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
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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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
Abstract
The invention provides a preparation method of a nylon carbon fiber composite powder material, which comprises the following steps: carrying out electrochemical oxidation treatment on the carbon fiber, and then carrying out cleaning, drying and filament winding processes to obtain the surface-treated carbon fiber; drying the surface-treated carbon fiber again, and continuously passing the carbon fiber through a thermal reaction furnace taking ammonia gas as a gas medium, wherein the ammonia gas is introduced in a direction opposite to the conveying direction of the carbon fiber in the reaction furnace to obtain modified carbon fiber; carrying out double-helix extrusion on modified carbon fiber and nylon resin, granulating to obtain nylon carbon fiber granules, and carrying out deep cooling crushing on the nylon carbon fiber granules to obtain nylon carbon fiber powder, wherein the nylon resin accounts for 30-70 parts, and the modified carbon fiber accounts for 50-30 parts; the following components in parts by mass: 90-95 parts of nylon carbon fiber powder, 0.1-1.5 parts of antioxidant and 0.1-1.5 parts of flow aid are added into a stirrer, and are uniformly mixed and sieved to prepare the nylon carbon fiber composite powder material, wherein the mechanical property and the wear resistance of the nylon material are improved by the carbon fiber reinforced nylon powder.
Description
Technical Field
The invention belongs to the technical field of additive manufacturing, and particularly relates to a nylon carbon fiber composite powder material and a preparation method thereof.
Background
Selective laser sintering is a method for manufacturing three-dimensional objects by selectively fusing layers of powder, which allows to obtain a three-dimensional entity without using tooling, by laser sintering only a plurality of superposed layers of powder according to a three-dimensional image of the object to be produced. This process is mainly performed using thermoplastic polymers, and patents US6136948 and WO9606881 describe in detail such a process for manufacturing three-dimensional objects using powdered polymers. The technology is applied to the fields of aerospace, medical treatment, footwear, industrial design, buildings and the like.
The nylon material is used as a semi-crystalline material, and the nylon has good mechanical property, low density, light weight, good chemical stability, wear resistance and friction reduction, and is widely applied by a selective laser sintering technology. However, with the continuous expansion of the application field of nylon parts, the requirements of mechanical parts on engineering materials and friction and wear performance are higher and higher, and more mechanical parts require that engineering plastic composite materials have high strength, rigidity and dimensional stability and also have excellent friction and wear performance.
In order to improve the material performance and overcome the disadvantages of nylon materials, chemical and physical modification of nylon is adopted. The physical modification is mainly to add various fillers to enhance various properties, and the fillers include fibers, inorganic particles, organic particles and the like. The carbon fiber composite material has the characteristics of small density and high rigidity. The carbon fiber composite material has the function of carbon fiber reinforced engineering plastics, and when the composite material is applied to mechanical parts, the composite material is required to have excellent comprehensive performance, particularly excellent mechanical property, wear resistance and stable product size. However, after the unmodified carbon fiber and nylon are molded, the adhesion force is poor, so that the stress transmission between the nylon and the fiber in an interface phase region is poor, and the fiber reinforcement effect cannot be achieved.
Disclosure of Invention
The invention provides a preparation method of a nylon carbon fiber composite powder material, which comprises the following steps:
(1) carrying out electrochemical oxidation treatment on the carbon fiber, and then carrying out cleaning, drying and filament winding processes to obtain the surface-treated carbon fiber;
(2) drying the surface-treated carbon fiber again, and continuously passing the carbon fiber through a thermal reaction furnace taking ammonia gas as a gas medium, wherein the introduction direction of the ammonia gas is opposite to the conveying direction of the carbon fiber in the reaction furnace, so as to obtain modified carbon fiber;
(3) carrying out double-helix extrusion on the modified carbon fiber and nylon resin, granulating to obtain nylon carbon fiber granules, and carrying out deep cooling crushing on the nylon carbon fiber granules to obtain nylon carbon fiber powder, wherein the nylon resin accounts for 30-70 parts, and the modified carbon fiber accounts for 30-50 parts;
(4) the following components in parts by mass: adding 90-95 parts of nylon carbon fiber powder, 0.1-1.5 parts of antioxidant and 0.1-1.5 parts of flow aid into a stirrer, uniformly mixing, and screening to obtain the nylon carbon fiber composite powder material.
Further preferably, the electrochemical oxidation treatment process specifically comprises: the graphite plate is connected with the anode, the carbon fiber is connected with the cathode, the electrolysis voltage is 22V, and the electrolysis time is 2 min.
Further preferably, in the electrochemical oxidation treatment process, the adopted electrolyte is prepared by mixing water and solute according to the proportion of 6-8: 2-4.
Further preferably, the solute is one or more of sulfuric acid, nitric acid, hydrochloric acid, ammonium carbonate and acetic acid.
Further preferably, the reaction temperature of the thermal reaction furnace is 600 ℃, the reaction residence time of the surface-treated carbon fiber in the reaction furnace is 20s, and the flow rate of the ammonia gas is 50L/h.
Further preferably, the carbon fibers have an average diameter of 5 to 15 μm and an average length of 150-200. mu.m.
Further preferably, the nylon resin is one or more of PA6, PA11, PA12, PA66, PA610, PA612, PA1010, PA1012 and PA 1212.
Further preferably, the antioxidant is a composite antioxidant consisting of a hindered phenol antioxidant and a phosphite antioxidant, wherein the hindered phenol antioxidant is preferably one or two of 1, 3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene and 2, 6-di-tert-butyl-4-methyl-phenol, and the phosphite antioxidant is 2 '-ethylbis (4, 6-di-tert-butylphenyl) fluorophosphite and/or tetrakis (2, 4-di-tert-butylphenyl) -4, 4' -biphenyldiphosphite.
Further preferably, the flow aid is fumed silica, fumed alumina or nano titanium dioxide.
The invention also provides a nylon carbon fiber composite powder material, which is prepared by the preparation method of the nylon carbon fiber composite powder material.
The invention provides a nylon carbon fiber composite powder material and a preparation method thereof, and the nylon carbon fiber composite powder material has the following beneficial effects:
1. the carbon fiber reinforced nylon powder improves the mechanical property and the wear resistance of the nylon material, and simultaneously expands the application field of the nylon powder;
2. the amide groups are connected to the modified carbon fibers, so that the functional groups of the carbon fibers can form hydrogen bonds with amide bonds of nylon, the binding force between the nylon and the carbon fibers is increased, and the reinforcing effect of the carbon fibers on the nylon is improved;
3. the carbon fiber is coated in the nylon by a double-helix extrusion method, so that after the nylon is sintered by using selective laser, the mechanical embedding force of the nylon and the carbon fiber is stronger, the reinforcing effect is better than that of other blending modes, and the mechanical property of a formed workpiece is better.
Detailed Description
The present invention is described in further detail below by way of specific examples.
Example one
(1) Carbon fibers having an average diameter of 10um and an average length of 170um were subjected to electrochemical oxidation treatment. The process comprises the steps of connecting a graphite plate with a positive electrode, connecting carbon fibers with a negative electrode, using an electrolyte solution prepared by mixing water and sulfuric acid in a ratio of 6:4, wherein the electrolysis voltage is 22V, and the electrolysis time is 2 min. Then, the carbon fiber with the surface treated is obtained through the processes of cleaning, drying and filament winding;
(2) and drying the surface-treated carbon fiber again, and enabling the carbon fiber to continuously pass through a thermal reaction furnace taking ammonia gas as a gas medium, wherein the reaction temperature of the thermal reaction furnace is 600 ℃, the reaction residence time of the surface-treated carbon fiber in the reaction furnace is 20s, and the flow of the ammonia gas is 50L/h. Obtaining modified carbon fibers;
(3) carrying out double-helix extrusion on 50 parts of modified carbon fiber and 50 parts of nylon 6 resin, granulating to obtain nylon carbon fiber granules, and carrying out deep cooling crushing on the nylon carbon fiber granules to obtain nylon carbon fiber powder;
(4) adding 90 parts of nylon carbon fiber powder, 0.5 part of antioxidant and 0.5 part of flow aid into a stirrer, uniformly mixing, and screening to obtain the nylon carbon fiber composite powder material.
Example two
(1) Carbon fibers having an average diameter of 15um and an average length of 150um were subjected to electrochemical oxidation treatment. The process comprises the steps of connecting a graphite plate with a positive electrode, connecting carbon fibers with a negative electrode, using an electrolyte solution prepared by mixing water and hydrochloric acid in a ratio of 5:5, wherein the electrolysis voltage is 22V, and the electrolysis time is 2 min. Then, the carbon fiber with the surface treated is obtained through the processes of cleaning, drying and filament winding;
(2) and drying the surface-treated carbon fiber again, and enabling the carbon fiber to continuously pass through a thermal reaction furnace taking ammonia gas as a gas medium, wherein the reaction temperature of the thermal reaction furnace is 600 ℃, the reaction residence time of the surface-treated carbon fiber in the reaction furnace is 20s, and the flow of the ammonia gas is 50L/h. Obtaining modified carbon fibers;
(3) carrying out double-helix extrusion on 30 parts of modified carbon fiber and 50 parts of nylon 12 resin, granulating to obtain nylon carbon fiber granules, and carrying out deep cooling crushing on the nylon carbon fiber granules to obtain nylon carbon fiber powder;
(4) adding 90 parts of nylon carbon fiber powder, 0.5 part of antioxidant and 0.5 part of flow aid into a stirrer, uniformly mixing, and screening to obtain the nylon carbon fiber composite powder material.
Example three
(1) Carbon fibers having an average diameter of 15um and an average length of 150um were subjected to electrochemical oxidation treatment. The process comprises the steps of connecting a graphite plate with a positive electrode, connecting carbon fibers with a negative electrode, using an electrolyte solution prepared by mixing water and hydrochloric acid in a ratio of 5:5, wherein the electrolysis voltage is 22V, and the electrolysis time is 2 min. Then, the carbon fiber with the surface treated is obtained through the processes of cleaning, drying and filament winding;
(2) and drying the surface-treated carbon fiber again, and enabling the carbon fiber to continuously pass through a thermal reaction furnace taking ammonia gas as a gas medium, wherein the reaction temperature of the thermal reaction furnace is 600 ℃, the reaction residence time of the surface-treated carbon fiber in the reaction furnace is 20s, and the flow of the ammonia gas is 50L/h. Obtaining modified carbon fibers;
(3) carrying out double-helix extrusion on 50 parts of modified carbon fiber and 50 parts of nylon 12 resin, granulating to obtain nylon carbon fiber granules, and carrying out deep cooling crushing on the nylon carbon fiber granules to obtain nylon carbon fiber powder;
(4) adding 90 parts of nylon carbon fiber powder, 0.5 part of antioxidant and 0.5 part of flow aid into a stirrer, uniformly mixing, and screening to obtain the nylon carbon fiber composite powder material.
TABLE 1 Properties of products made with the nylon carbon fiber composite powder materials of examples one to three
The above-mentioned embodiment only represents one embodiment of the present invention, and it should be noted that, for those skilled in the art, many variations and modifications can be made without departing from the spirit of the present invention, and these embodiments are within the scope of the present invention.
Claims (10)
1. The preparation method of the nylon carbon fiber composite powder material is characterized by comprising the following steps:
(1) carrying out electrochemical oxidation treatment on the carbon fiber, and then carrying out cleaning, drying and filament winding processes to obtain the surface-treated carbon fiber;
(2) drying the surface-treated carbon fiber again, and continuously passing the carbon fiber through a thermal reaction furnace taking ammonia gas as a gas medium, wherein the introduction direction of the ammonia gas is opposite to the conveying direction of the surface-treated carbon fiber in the reaction furnace, so as to obtain modified carbon fiber;
(3) carrying out double-helix extrusion on the modified carbon fiber and nylon resin, granulating to obtain nylon carbon fiber granules, and carrying out deep cooling crushing on the nylon carbon fiber granules to obtain nylon carbon fiber powder, wherein the nylon resin accounts for 30-70 parts, and the modified carbon fiber accounts for 30-50 parts;
(4) the following components in parts by mass: adding 90-95 parts of nylon carbon fiber powder, 0.1-1.5 parts of antioxidant and 0.1-1.5 parts of flow aid into a stirrer, uniformly mixing, and screening to obtain the nylon carbon fiber composite powder material.
2. The preparation method of the nylon carbon fiber composite powder material according to claim 1, wherein the electrochemical oxidation treatment process specifically comprises the following steps: the graphite plate is connected with the anode, the carbon fiber is connected with the cathode, the electrolysis voltage is 22V, and the electrolysis time is 2 min.
3. The preparation method of the nylon carbon fiber composite powder material according to claim 2, wherein in the electrochemical oxidation treatment process, the adopted electrolyte is prepared by mixing water and solute according to a ratio of 6-8: 2-4.
4. The method for preparing the nylon carbon fiber composite powder material according to claim 3, wherein the solute is one or more of sulfuric acid, nitric acid, hydrochloric acid, ammonium carbonate and acetic acid.
5. The method for preparing nylon carbon fiber composite powder material according to claim 4, wherein the reaction temperature of the thermal reaction furnace is 600 ℃, the reaction residence time of the surface-treated carbon fiber in the reaction furnace is 20s, and the flow rate of the ammonia gas is 50L/h.
6. The method for preparing nylon-carbon fiber composite powder material as claimed in claim 5, wherein the carbon fiber has an average diameter of 5-15 μm and an average length of 150-200 μm.
7. The method for preparing the nylon carbon fiber composite powder material according to claim 6, wherein the nylon resin is one or more of PA6, PA11, PA12, PA66, PA610, PA612, PA1010, PA1012 and PA 1212.
8. The method for preparing nylon-carbon fiber composite powder material according to claim 7, wherein the antioxidant is a composite antioxidant comprising a hindered phenol antioxidant and a phosphite antioxidant, wherein the hindered phenol antioxidant is one or two of 1, 3, 5-trimethyl-2, 4, 6-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) benzene and 2, 6-di-tert-butyl-4-methyl-phenol, and the phosphite antioxidant is 2 '-ethylbis (4, 6-di-tert-butylphenyl) fluorophosphite and/or tetrakis (2, 4-di-tert-butylphenyl) -4, 4' -biphenylbis-phosphite.
9. The method for preparing nylon carbon fiber composite powder material according to claim 8, wherein the flow aid is fumed silica, fumed alumina or nano titanium dioxide.
10. A nylon carbon fiber composite powder material characterized by being produced by the method for producing a nylon carbon fiber composite powder material according to any one of claims 1 to 9.
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| CB02 | Change of applicant information | ||
| CB02 | Change of applicant information |
Address after: No. 181, Linyu Road, national high tech Industrial Development Zone, Changsha City, Hunan Province, 410205 Applicant after: Hunan Huashu High Tech Co.,Ltd. Address before: No. 181, Linyu Road, national high tech Industrial Development Zone, Changsha City, Hunan Province, 410205 Applicant before: HUNAN FARSOON HIGH-TECH Co.,Ltd. |
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| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200421 |