CN111574731A - Preparation method of modified carbon fiber reinforced nylon particles - Google Patents
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- CN111574731A CN111574731A CN202010495437.2A CN202010495437A CN111574731A CN 111574731 A CN111574731 A CN 111574731A CN 202010495437 A CN202010495437 A CN 202010495437A CN 111574731 A CN111574731 A CN 111574731A
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
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- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
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Abstract
The invention provides a preparation method of a modified carbon fiber-reinforced nylon composite material, wherein nylon, hyperbranched polymer, modified carbon fiber, coupling agent, flame retardant, antioxidant and lubricant are used as raw materials in the preparation method, and nylon particles are obtained by a simple and convenient method; the composite material particle has high tensile strength, bending strength and impact resistance.
Description
Technical Field
The invention relates to the field of polymer material science, in particular to modified carbon fiber reinforced nylon particles and a preparation method thereof.
Background
With the increasing maturity of the application of the carbon fiber reinforced thermosetting composite material, the carbon fiber reinforced thermoplastic composite material gradually moves from the aerospace field to various civil fields such as industrial machinery, high-end medical treatment, rail transit, electronic and electric appliances and the like. Compared with the traditional thermosetting carbon fiber composite material, the thermoplastic composite material such as nylon series has the remarkable characteristics of high toughness, high impact resistance, damage tolerance, unlimited prepreg storage period, short molding period, recyclability, easiness in repair and the like, and has the advantages of environmental protection, high efficiency and high performance. With the increasing application of thermoplastic composite materials, especially nylon series, in the civil field, the market demand for their functions is also increasing, and therefore, a single-performance thermoplastic material, for example, cannot meet the market demand, and therefore, a thermoplastic resin functional material with composite functions needs to be continuously developed, so that the thermoplastic resin functional material has the characteristics of high strength, good toughness, wear resistance, cold resistance, oil resistance, water resistance, aging resistance, weather resistance and the like, and meanwhile, the thermoplastic resin functional material has many excellent functions of high waterproofness, moisture permeability, wind resistance, cold resistance, antibacterial property, mildew resistance, warmth retention, ultraviolet resistance, energy release and the like according to different application fields. The common method for modifying the resin is as follows. The existing modification method is mainly carried out on the basis of the aspects of chemistry, blending, filling reinforcement, carbon fiber reinforcement and the like.
However, in the case of a reinforcing fiber composite material of reinforcing fibers such as carbon fibers and nylon, it is an important factor to ensure the uniformity of the material properties to uniformly disperse the reinforcing fibers therein. This is because, if the degree of dispersion of the fibers in the composite material is low, and if there are regions with a large amount of resin and regions with a large amount of fibers, when a molded article produced using the composite material is subjected to stress, the stress concentrates on uneven portions and damage may occur. Therefore, the carbon fiber reinforced nylon composite material with uniform distribution is prepared, so that the composite material has excellent performances of high toughness, high impact resistance, damage tolerance and the like, and has important application value.
Disclosure of Invention
Aiming at the defects in the prior art, the invention mainly aims to provide modified carbon fiber reinforced nylon composite particles with good mechanical property, high toughness, high impact resistance, strong wear resistance and long service life and a preparation method thereof.
Specifically, the object of the present invention can be achieved by:
a preparation method of modified carbon fiber reinforced nylon composite particles comprises the following steps:
step 1, dissolving a hyperbranched polymer in an organic solvent, soaking carbon fibers in the solution, and removing the solvent after ultrasonic treatment to obtain modified carbon fibers;
step 2, feeding nylon, modified carbon fiber and hyperbranched polymer, heating and melting, stirring and mixing at a high speed, adding the coupling agent, the flame retardant, the antioxidant and the lubricant, and then continuing stirring and mixing;
and 3, adding the obtained mixed material into a hopper of a double-screw extruder, and extruding and granulating to obtain the modified carbon fiber reinforced nylon composite material particles.
Preferably, the hyperbranched polymer in step 1 and step 2 is selected from hyperbranched polyphenylene ether, hyperbranched polyglycidyl ether or hyperbranched polyester.
Preferably, the carbon fiber chopped fibers in the step 1 are selected from T300, T400 or T600 carbon fibers.
Preferably, the feeding amount of each component in the step 2 is 30-60 parts of nylon, 10-20 parts of hyperbranched polymer, 30-40 parts of modified carbon fiber, 0.5-3 parts of coupling agent, 0.1-2 parts of flame retardant, 0.1-2 parts of antioxidant and 0.1-2 parts of lubricant.
Preferably, the nylon PA in the step 2 is selected from one of PA66, PA66/6, PA610 or PA12 or any combination thereof.
Preferably, the coupling agent in step 2 is selected from one of gamma-aminopropyltriethoxysilane, gamma-aminopropyltrimethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, gamma-glycidoxypropyltrimethoxysilane, or a combination thereof.
Preferably, the flame retardant in step 2 is selected from silicon based flame retardants, preferably inorganic silicon flame retardants.
Preferably, the antioxidant in step 2 is selected from N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexamethylenediamine or pentaerythritol [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
Preferably, the lubricant in step 2 is selected from polyethylene wax, zinc stearate or magnesium stearate.
Preferably, the heating temperature in step 2 is greater than 160 ℃, preferably between 160 ℃ and 260 ℃.
Preferably, the high-speed stirring time in the step 2 is at least 0.5h, and preferably 0.5h to 2 h; the time for continuous stirring is at least 0.5h, and preferably 0.5 h-2 h.
Preferably, the temperature for extrusion granulation in step 3 is 160-200 ℃.
The invention has the following beneficial effects:
1. according to the preparation process, the supermolecule polymer modified carbon fiber and nylon are mixed to prepare the composite material, and the composite material can enable the carbon fiber to be distributed more uniformly, so that the composite material has more excellent mechanical properties.
2. The preparation process provided by the invention is simple, convenient and flexible, and is suitable for industrial popularization and use.
Detailed Description
The invention will now be further described with reference to specific examples. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
The carbon fibers used in the examples of the present invention are commercially available products; the hyperbranched polymer may be purchased from a commercially available product, or may be prepared by a method described in a conventional literature, and other materials not described may be purchased.
Example 1
Step 1, dissolving 10g of hyperbranched polyphenylene oxide in 500ml of acetone, soaking 20g of carbon fiber T300 in the solution, ultrasonically mixing for 5 hours at 40 ℃, and performing rotary evaporation to remove acetone to obtain modified carbon fiber;
step 2, adding 50 parts of nylon 66, 35 parts of the modified carbon fiber obtained in the step 1 and 15 parts of hyperbranched polyphenylene oxide into a mixing device, heating to a temperature above 200 ℃ to a molten state, and stirring at a high speed for 1.5 hours at the temperature; then adding 2 parts of gamma-glycidoxypropyltrimethoxysilane, 1 part of inorganic silicon flame retardant, 0.5 part of N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexamethylenediamine and 0.5 part of polyethylene wax, and continuing stirring at high speed for mixing for 1 hour;
and 3, adding the obtained mixed material into a double-screw extruder, controlling the temperature in a conveying channel to be 160-200 ℃, and extruding and granulating the material by a die as required to obtain the modified carbon fiber reinforced nylon composite material.
Example 2
Step 1, dissolving 10g of hyperbranched polyglycidyl ether in 500ml of methanol, soaking 20g of carbon fiber T400 in the solution, ultrasonically mixing the solution at 50 ℃ for 5 hours, and performing rotary evaporation to remove methanol to obtain modified carbon fiber;
step 2, adding 60 parts of PA66/6, 30 parts of modified carbon fibers prepared in the step 1 and 10 parts of hyperbranched polyglycidyl ether into a mixing device, heating to more than 200 ℃ to a molten state, and stirring at a high speed for 2 hours at the temperature; then adding 2 parts of gamma- (methacryloyloxy) propyl trimethoxy silane, 1 part of inorganic silicon flame retardant, 2 parts of [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester and 1 part of zinc stearate, and continuously stirring and mixing at high speed for 1 h;
and 3, adding the obtained mixed material into a double-screw extruder, controlling the temperature in a conveying channel to be 160-200 ℃, and extruding and granulating the material by a die as required to obtain the modified carbon fiber reinforced nylon composite material.
Example 3
Step 1, dissolving 10g of hyperbranched polyphenylene oxide in 500ml of acetone, soaking 20g of carbon fiber T600 in the solution, ultrasonically mixing for 5 hours at 40 ℃, and performing rotary evaporation to remove acetone to obtain modified carbon fiber;
step 2, adding 50 parts of PA610, 35 parts of modified carbon fiber prepared in the step 1 and 20 parts of hyperbranched polyphenylene oxide into a mixing device, heating to more than 200 ℃ to a molten state, and stirring at a high speed for 2 hours at the temperature; then adding 0.5 part of gamma-aminopropyltriethoxysilane, 1 part of inorganic silicon flame retardant, 0.5 part of N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexamethylenediamine and 1 part of magnesium stearate, and continuously stirring and mixing for 1h at a high speed;
and 3, adding the obtained mixed material into a double-screw extruder, controlling the temperature in a conveying channel to be 160-200 ℃, and extruding and granulating the material by a die as required to obtain the modified carbon fiber reinforced nylon composite material.
Example 4
Step 1, dissolving 10g of hyperbranched polyurethane in 500ml of methanol, soaking 20g of carbon fiber T600 in the solution, ultrasonically mixing the solution at 50 ℃ for 5 hours, and performing rotary evaporation to remove acetone to obtain modified carbon fiber;
step 2, adding 30 parts of PA12 and 40 parts of modified carbon fiber obtained in the step 1 and 10 parts of hyperbranched polyurethane into a mixing device, heating to a temperature above 200 ℃ to a molten state, and stirring at a high speed for 2 hours at the temperature; adding 3 parts of gamma-aminopropyltrimethoxysilane, 2 parts of an inorganic silicon flame retardant, 0.1 part of N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine and 2 parts of polyethylene wax, and continuously stirring and mixing for 1 hour at a high speed;
and 3, adding the obtained mixed material into a double-screw extruder, controlling the temperature in a conveying channel to be 160-200 ℃, and extruding and granulating the material by a die as required to obtain the modified carbon fiber reinforced nylon composite material.
Example 5
Step 1, dissolving 10g of hyperbranched polyglycidyl ether in 500ml of methanol, soaking 20g of carbon fiber T300 in the solution, ultrasonically mixing the solution at 50 ℃ for 5 hours, and performing rotary evaporation to remove acetone to obtain modified carbon fiber;
step 2, adding 50 parts of PA66 and 40 parts of the modified carbon fiber obtained in the step 1 and 10 parts of hyperbranched polyglycidyl ether into a mixing device, heating to more than 200 ℃ to a molten state, and stirring at a high speed for 2 hours at the temperature; then adding 1.5 parts of gamma-aminopropyltriethoxysilane, 2 parts of inorganic silicon flame retardant, 0.1 part of N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine and 0.1 part of polyethylene wax, and continuing stirring at high speed for mixing for 1 h;
and 3, adding the obtained mixed material into a double-screw extruder, controlling the temperature in a conveying channel to be 160-200 ℃, and extruding and granulating the material by a die as required to obtain the modified carbon fiber reinforced nylon composite material.
Comparative example 1
Step 1, dissolving 10g of hyperbranched polyphenylene oxide in 500ml of acetone, soaking 20g of carbon fiber T300 in the solution, ultrasonically mixing for 5 hours at 40 ℃, and performing rotary evaporation to remove acetone to obtain modified carbon fiber;
step 2, adding 50 parts of nylon 66 and 35 parts of the modified carbon fiber obtained in the step 1 into mixing equipment, heating to a temperature above 200 ℃ to a molten state, and stirring at a high speed for 1.5 hours at the temperature; then adding 2 parts of gamma-glycidoxypropyltrimethoxysilane, 1 part of inorganic silicon flame retardant, 0.5 part of N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexamethylenediamine and 0.5 part of polyethylene wax, and continuing stirring at high speed for mixing for 1 hour;
and 3, adding the obtained mixed material into a double-screw extruder, controlling the temperature in a conveying channel to be 160-200 ℃, and extruding and granulating the material by a die as required to obtain the modified carbon fiber reinforced nylon composite material.
Comparative example 2
Step 1, adding 50 parts of nylon 66, 35 parts of carbon fiber and 15 parts of hyperbranched polyphenylene oxide into mixing equipment, heating to more than 200 ℃ to a molten state, and stirring at a high speed for 1.5 hours at the temperature; then adding 2 parts of gamma-glycidoxypropyltrimethoxysilane, 1 part of inorganic silicon flame retardant, 0.5 part of N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexamethylenediamine and 0.5 part of polyethylene wax, and continuing stirring at high speed for mixing for 1 hour;
and 2, adding the obtained mixed material into a double-screw extruder, controlling the temperature in a conveying channel to be 160-200 ℃, and extruding and granulating the material by a die as required to obtain the modified carbon fiber reinforced nylon composite material.
Performance testing
Tensile properties of the composite material of the invention: the composite materials prepared in the examples and comparative examples were processed into tensile test specimens according to GB/T1447-2005 tensile Property test method, and the tensile strength and the loading speed were measured at 2mm/min, and 6 specimens were tested per group.
The impact resistance of the composite material of the invention is tested: according to GB/T1043-1993 method for testing impact of rigid plastic simply supported beams, the composite materials prepared in the examples and the comparative examples are processed into type 1 test samples, and the impact strength is tested after A type notches.
The bending property of the composite material is tested as follows: the composite materials prepared in examples and comparative examples were processed into bending test specimens respectively according to GB/T3356-1999 method for testing bending properties of unidirectional fiber reinforced plastics, and the bending strength and the loading speed were measured at 2mm/min, and 6 specimens were tested per group.
Table 1 mechanical property testing of modified carbon fiber reinforced nylon
| Test sample | Tensile Strength (MPa) | Flexural Strength (MPa) | Impact Strength (KJ/m)2) |
| Example 1 | 213 | 306 | 21.5 |
| Example 2 | 196 | 279 | 19.8 |
| Example 3 | 192 | 281 | 18.7 |
| Example 4 | 179 | 262 | 18.1 |
| Example 5 | 181 | 269 | 17.9 |
| Comparative example 1 | 129 | 206 | 13.2 |
| Comparative example 2 | 116 | 189 | 11.5 |
Claims (10)
1. A preparation method of modified carbon fiber reinforced nylon composite particles is characterized by comprising the following steps:
step 1, dissolving a hyperbranched polymer in an organic solvent, soaking carbon fibers in the solution, and removing the solvent after ultrasonic treatment to obtain modified carbon fibers;
step 2, feeding nylon, modified carbon fiber and hyperbranched polymer, heating and melting, stirring and mixing at a high speed, adding the coupling agent, the flame retardant, the antioxidant and the lubricant, and then continuing stirring and mixing;
and 3, adding the obtained mixed material into a hopper of a double-screw extruder, and extruding and granulating to obtain the modified carbon fiber reinforced nylon composite material particles.
2. The method according to claim 1, wherein the hyperbranched polymer in step 1 and step 2 is selected from hyperbranched polyphenylene oxide, hyperbranched polyglycidyl ether, or hyperbranched polyester.
3. The method according to claim 1, wherein the carbon fiber chopped fiber in step 1 is preferably a T300, T400 or T600 type carbon fiber.
4. The preparation method according to claim 1, wherein the feeding amount of each component in the step 2 is 30-60 parts of nylon, 10-20 parts of hyperbranched polymer, 30-40 parts of modified carbon fiber, 0.5-3 parts of coupling agent, 0.1-2 parts of flame retardant, 0.1-2 parts of antioxidant and 0.1-2 parts of lubricant.
5. The method for preparing the nylon of claim 1, wherein the nylon PA in the step 2 is selected from one or any combination of PA66, PA66/6, PA610 and PA 12.
6. The method according to claim 1, wherein the coupling agent in step 2 is selected from one or a combination of γ -aminopropyltriethoxysilane, γ -aminopropyltrimethoxysilane, γ - (methacryloyloxy) propyltrimethoxysilane, γ -glycidoxypropyltrimethoxysilane.
7. The method according to claim 1, wherein the flame retardant in step 2 is selected from silicon-based flame retardants, preferably inorganic silicon flame retardants; the antioxidant is selected from N, N' -bis- (3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionyl) hexanediamine or [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester; the lubricant is selected from polyethylene wax, zinc stearate or magnesium stearate.
8. The method of claim 1, wherein the heating temperature in step 2 is greater than 160 ℃, preferably 160 ℃ to 260 ℃.
9. The preparation method according to claim 1, wherein the high-speed stirring time in the step 2 is at least 0.5h, preferably 0.5h to 2 h; the time for continuous stirring is at least 0.5h, and preferably 0.5 h-2 h.
10. The method according to claim 1, wherein the temperature in the extrusion granulation in step 3 is 160 to 200 ℃.
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| CN202010495437.2A CN111574731A (en) | 2020-06-03 | 2020-06-03 | Preparation method of modified carbon fiber reinforced nylon particles |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113214641A (en) * | 2021-04-14 | 2021-08-06 | 深圳市高科塑化有限公司 | Light carbon fiber reinforced PA material and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113214641A (en) * | 2021-04-14 | 2021-08-06 | 深圳市高科塑化有限公司 | Light carbon fiber reinforced PA material and preparation method thereof |
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Application publication date: 20200825 |