CN115044195A - Basalt continuous fiber reinforced nylon composite material and preparation method thereof - Google Patents
Basalt continuous fiber reinforced nylon composite material and preparation method thereof Download PDFInfo
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- CN115044195A CN115044195A CN202210716100.9A CN202210716100A CN115044195A CN 115044195 A CN115044195 A CN 115044195A CN 202210716100 A CN202210716100 A CN 202210716100A CN 115044195 A CN115044195 A CN 115044195A
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- 239000004677 Nylon Substances 0.000 title claims abstract description 63
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- 238000002360 preparation method Methods 0.000 title claims description 10
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- 239000006057 Non-nutritive feed additive Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims description 35
- 238000002844 melting Methods 0.000 claims description 24
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- 238000002156 mixing Methods 0.000 claims description 24
- 239000008187 granular material Substances 0.000 claims description 22
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- 238000007598 dipping method Methods 0.000 claims description 9
- 238000001125 extrusion Methods 0.000 claims description 7
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 claims description 6
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- VCUFZILGIRCDQQ-KRWDZBQOSA-N N-[[(5S)-2-oxo-3-(2-oxo-3H-1,3-benzoxazol-6-yl)-1,3-oxazolidin-5-yl]methyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C1O[C@H](CN1C1=CC2=C(NC(O2)=O)C=C1)CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F VCUFZILGIRCDQQ-KRWDZBQOSA-N 0.000 description 1
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Classifications
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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
- 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
-
- 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
-
- 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
- C08J2377/06—Polyamides derived from polyamines and polycarboxylic acids
-
- 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
- C08J2469/00—Characterised by the use of polycarbonates; Derivatives of polycarbonates
-
- 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
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
-
- 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
- C08J2481/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing sulfur with or without nitrogen, oxygen, or carbon only; Polysulfones; Derivatives of such polymers
- C08J2481/02—Polythioethers; Polythioether-ethers
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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
- C08K7/10—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
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/28—Glass
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- Chemical & Material Sciences (AREA)
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
The invention provides a basalt continuous fiber reinforced nylon composite material which comprises the following raw materials in parts by weight: 50-80 parts of nylon resin; 20-50 parts of basalt continuous fibers; 1-5 parts of a compatibilizer; 0.5-5 parts of hollow microspheres; 1-5 parts of an elastomer; 0.1-5 parts of a processing aid. The basalt fiber/nylon composite material provided by the invention has excellent acid and alkali corrosion resistance, is large in use temperature range, is lighter without influencing mechanical properties, and is suitable for outdoor and underwater in coastal areas.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a basalt continuous fiber reinforced nylon composite material and a preparation method thereof.
Background
Nylon (PA for short) is a generic name for a class of polyamide compounds, including aliphatic PA, aliphatic-aromatic PA and aromatic PA. The most representative nylon composite materials are nylon 6 and nylon 66, which have good wear resistance, strength and toughness and are commonly used in the fields of automobiles, electronics, unmanned planes, engineering plastics, civil yarns and the like. However, nylon has the disadvantages of high water absorption, poor low-temperature impact toughness, poor dimensional stability and the like.
The existing nylon modification technology has the advantages that the mechanical property of a nylon material can be improved, the water absorption property of nylon can be improved, and the excellent comprehensive performance of the nylon as engineering plastics can be better exerted besides blending and copolymerization and fiber reinforcement modification. The existing fiber reinforced nylon mainly comprises short fiber reinforced nylon mainly comprising glass fiber/nylon.
The basalt continuous fiber is a special fiber material made of natural basalt ore. The fiber-reinforced polypropylene fiber has the characteristics of high strength, high modulus, good temperature resistance, oxidation resistance, radiation resistance, acid and alkali resistance, heat insulation and sound insulation, good filterability, high compressive strength, high shear strength, strong applicability, light weight and the like, is fibrous and soft in appearance, and can be processed into various fabrics; compared with glass fiber, the basalt continuous fiber has higher strength, higher durable temperature range, higher modulus and stronger acid-base corrosion resistance. Therefore, the basalt is used as the reinforcing fiber to reinforce the resin, so that the problem of corrosion of the glass fiber reinforced plastic material in coastal areas can be effectively solved.
Compared with short fiber reinforced technology, the long fiber reinforced thermoplastic composite material (LFT) technology can reduce the damage to the fiber to a greater extent, thereby keeping higher fiber length and fiber content, leading the long fiber uniformly dispersed in a formed product to easily travel to a three-dimensional network structure, and leading the stress borne by the composite material to be better dispersed in the fiber.
The chemical components of the glass fiber of the existing glass fiber/nylon composite material are easily subjected to chemical corrosion of OH & lt- & gt and Cl & lt- & gt ions, so that the glass fiber is easily damaged in a high-salt and high-humidity environment, the fiber reinforcement fails, and nylon absorbs water to cause local damage, so that the long-term lasting performance of the glass fiber/nylon composite material in coastal areas and marine areas cannot be maintained.
The existing mature short fiber reinforced technology has the disadvantages of serious fiber damage, poor length uniformity, low fiber content and poor fiber dispersion capability, and easily causes the local performance loss of the reinforced composite material, increases the loss and reduces the yield.
Therefore, it is very necessary to develop a novel basalt continuous fiber reinforced nylon composite material.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present invention is to provide a basalt continuous fiber reinforced nylon composite material, which has good high temperature resistance, high water absorption rate and good mechanical properties.
The invention provides a basalt continuous fiber reinforced nylon composite material which comprises the following raw materials in parts by weight:
preferably, the nylon resin is selected from one or more of nylon 6, nylon 66, nylon 610, nylon 11 and nylon 12.
Preferably, the compatibilizer is one or more of MAH cyclic anhydride type and maleic anhydride.
Preferably, the basalt continuous fiber is one or more of BS, BF, BM, BAS and BTR; the basalt continuous fiber and the basalt continuous fiber BF are general types: sichuan humble BF815-2400, Guizhou Shixin BF22-2400, and Taian Hao pine xwy-14.
Preferably, the hollow bead is one or more of 3M K1, IM16K, S15, IM30K, K20, S38HS, Zhongmei ZM-K25 or AStrong 2046H;
the elastomer is one or more of nylon 12, polycarbonate or PPS;
the processing aid is one or more of a lubricant, a dispersant, an anti-aging agent, a defoaming agent or an antistatic agent.
Preferably, the basalt continuous fiber reinforced nylon composite material comprises the following raw materials in parts by weight:
the preparation method of the basalt continuous fiber reinforced nylon composite material provided by the invention is characterized by comprising the following steps:
A) mixing nylon resin and a compatibilizer to obtain a first premix;
B) extruding the first premix to obtain an extruded material; melting, dipping, drawing and shearing the extruded material and the preheated basalt continuous fiber to obtain composite granules;
C) mixing the composite granules, the hollow microspheres, the elastomer and the processing aid to obtain a second premix; and injection molding the second premix to obtain the composite material.
Preferably, the traction speed in the step B) is 8-12 m/min.
Preferably, the length of the composite granules in the step B) is 10-20 mm.
Preferably, the parameters of the extrusion in step B) are: the temperature of each section of a charging barrel of the double-screw extruder is 235-255 ℃; the rotating speed of the screw is 50-80 r/min; the feeding speed is 4-8 r/min;
preferably, the preheating temperature of the basalt fibers in the step B) is 150-200 ℃;
preferably, the temperature of the four areas of the dipping die in the step B) is 270-290 ℃.
The molding is one or more of injection molding, compression molding or extrusion molding.
Compared with the prior art, the invention provides a basalt continuous fiber reinforced nylon composite material, which comprises the following raw materials in parts by weight: 50-80 parts of nylon resin; 20-50 parts of basalt continuous fibers; 1-5 parts of a compatibilizer; 0.5-5 parts of hollow microspheres; 1-5 parts of an elastomer; 0.1-5 parts of a processing aid. The basalt fiber/nylon composite material provided by the invention has excellent acid and alkali corrosion resistance, is large in use temperature range, is lighter without influencing mechanical properties, and is suitable for outdoor and underwater in coastal areas.
Detailed Description
The invention provides a basalt continuous fiber reinforced nylon composite material and a preparation method thereof, and a person skilled in the art can use the contents to reference the text and appropriately improve the process parameters to realize the basalt continuous fiber reinforced nylon composite material. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the scope of the invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and applications described herein, as well as other suitable variations and combinations, may be made to implement and use the techniques of this invention without departing from the spirit and scope of the invention.
The invention provides a basalt continuous fiber reinforced nylon composite material which comprises the following raw materials in parts by weight:
the above parts by weight are equivalent to the weight percent when the total amount is 100.
The basalt continuous fiber reinforced nylon composite material provided by the invention comprises 50-80 parts by weight of nylon resin; specifically, it may be 50, 60, 70 or 80 parts by weight; or a point value between any of the above.
The nylon is one or a mixture of more of nylon 6, nylon 66, nylon 610, nylon 11 and nylon 12.
The method specifically comprises the following steps: mitsubishi 1010C2, Pasteur B29HM01, U.S. Dupont 73G20L, Germany VESTAMID L1670, Germany Apec 2097, and the like.
The basalt fiber reinforced nylon resin adopted by the invention has the characteristics of good chemical stability, corrosion resistance, high mechanical strength, high temperature use interval and the like. The problem that the corrosion condition of the glass fiber reinforced resin in a high-salt and high-humidity environment affects the performance and stability of the material can be solved.
The basalt continuous fiber reinforced nylon composite material provided by the invention comprises 20-50 parts by weight of basalt continuous fibers; specifically, it may be 20, 30, 40, or 50 parts by weight; or a point value between any of the above.
The basalt continuous fiber is one or more of BS, BF, BM, BAS and BTR.
The method specifically comprises the following steps: the Szechwan courtyard is BF815-2400, BF811-2400, BF826-2400, Zhejiang Shijin BCR13-264 and 101T5, etc.
The basalt continuous fiber reinforced nylon composite material provided by the invention comprises 1-5 parts by weight of a compatibilizer; preferably, the compatibilizer is 3-5 parts by weight; specifically, the weight ratio of the monomer to the monomer can be 3, 4 or 5; or a point value between any of the above.
The compatibilizer is one or more of MAH cyclic anhydride type and maleic anhydride.
The method specifically comprises the following steps: zixiangtengda maleic anhydride, aldichm 625, jinghao 9905, french arkomalotader 3210, etc.
The basalt continuous fiber reinforced nylon composite material provided by the invention comprises 0.5-5 parts by weight of hollow microspheres; preferably 2 to 4 parts by weight; specifically, the weight ratio of the component (A) to the component (B) can be 2, 3 or 4; or a point value between any of the above.
The hollow microspheres are hollow glass microspheres and floating beads.
The method specifically comprises the following steps: 3M K1, IM16K, S15, IM30K, K20, S38HS, Zhongmei ZM-K25, AStrong 2046H.
The basalt continuous fiber reinforced nylon composite material provided by the invention comprises 1-5 parts by weight of an elastomer; preferably 2 to 5 parts by weight; specifically, the weight ratio of the monomer to be used may be 2, 3, 4 or 5 parts; or a point value between any of the above.
The elastomer of the invention is: nylon 12, polycarbonate, PPS.
The method specifically comprises the following steps: acalma 6333 france, eggett degusse 47h, EMS TR-55LX, dupont TPEE Hytrel 3078, kraton G1657, bayer 9415, germany.
The invention improves the problem of reduction of elongation at break of the product caused by introducing the fiber by using a small amount of elastomer for blending, solves the problem of increase of the integral density of the material caused by that the density of the basalt fiber is slightly larger than that of the glass fiber by using a small amount of hollow microspheres, and simultaneously blends the melt viscosity to ensure that the basalt fiber is smoother and more stable in the continuous production process.
The basalt continuous fiber reinforced nylon composite material provided by the invention comprises 0.1-5 parts by weight of processing aid. Preferably 0.5 to 4 parts by weight; more preferably 0.5 to 0.6 parts by weight. Specifically, it may be 0.5 to 0.6 part by weight; or a point value between any of the above.
The processing aid is one or more of a lubricant, a dispersing agent, an anti-aging agent, a defoaming agent or an antistatic agent.
The method specifically comprises the following steps: EBS, Lonicera 114N, Germany, Honeywell A-C540, erucamide, Sichuan morning silicone powder, Decasteca E525, 1098, 168, 9228, XUHUAC BYK-057, AKN-3357, etc.
In a part of preferred embodiments of the present invention, the basalt continuous fiber reinforced nylon composite material comprises the following raw materials in parts by weight:
wherein: each part of the processing aid comprises the following raw materials in percentage by weight:
the basalt fiber reinforced nylon is adopted in the invention, so that the corrosion resistance and mechanical property of the nylon are obviously enhanced, the use scene of the material is widened, and the material can reach the expected performance under lighter weight, thereby saving the cost. Compared with the existing glass fiber reinforced nylon, the same performance is achieved under the condition that the mass fraction is lower than 10%, and the performance is attenuated by less than 5% under the long-term seawater soaking. The corrosion performance of the nylon composite material is obviously enhanced, and the density of the product is reduced.
The preparation method of the basalt continuous fiber reinforced nylon composite material provided by the invention is characterized by comprising the following steps:
A) mixing nylon resin and a compatibilizer to obtain a first premix;
B) extruding the first premix to obtain an extruded material; melting and dipping the extruded material and the basalt continuous fiber, drawing and shearing to obtain composite granules;
C) mixing the composite granules, the hollow microspheres, the elastomer and the processing aid to obtain a second premix; and forming the second premix to obtain the product.
The components and the specific proportion of the components are clearly described in the invention, and the details are not repeated.
The preparation method of the basalt continuous fiber reinforced nylon composite material provided by the invention comprises the steps of mixing the nylon resin, the compatibilizer to obtain a first premix.
The invention is not limited to the specific manner of mixing, as is well known to those skilled in the art.
And extruding the first premix through a double-screw extruder to obtain an extruded material. The parameters of the extrusion of the invention are as follows: the temperature of each section of a charging barrel of the double-screw extruder is 235-255 ℃; the rotating speed of the screw is 50-80 r/min; the feeding speed is 4-8 r/min;
and melting and impregnating the extruded material and the basalt continuous fiber.
Drying the basalt continuous fibers by a preheating device; the preheating temperature is 150-200 ℃; a first pre-mixed melt is extruded into a melt impregnation die. And (3) passing the dried basalt continuous fiber into a melting dipping die, wherein the temperature of the four regions of the dipping die is 270-290 ℃.
And (3) continuously producing at the speed of 2-12 m/min by a tractor to obtain the continuous composite master batch.
And cutting the obtained composite master batch into composite granules with uniform length of 10-20 mm by a shearing machine.
And mixing the composite granules, the hollow microspheres, the elastomer and the processing aid to obtain a second premix. The invention is not limited to the specific manner of mixing, as is well known to those skilled in the art.
And forming the second premix to obtain the basalt continuous fiber reinforced nylon composite material.
The molding is one or more of injection molding, compression molding or extrusion molding.
The invention utilizes LFT technology to reinforce resin to realize high content of reinforced Fiber, so that the reinforcing effect is maximized, and the defects of short Fiber residual length, relatively poor reinforcing effect, low Fiber content and the like in the traditional SFT technology are overcome. The specific method comprises the following steps: the thermoplastic melt is continuously fed through an extruder into a dipping die, and the continuous fiber strand is drawn through a dipping die containing a number of godets, the dipping process being carried out while the fiber strand is in contact with the melt. The basalt reinforced nylon resin granules obtained by the LFT technology have more purposes, and can be produced into products by three modes: the product with uniform mixing, stable structure and strong comprehensive performance can be obtained by different production modes, such as direct injection molding, direct compression molding and direct extrusion molding.
The invention provides a basalt continuous fiber reinforced nylon composite material which comprises the following raw materials in parts by weight: 50-80 parts of nylon resin; 20-50 parts of basalt continuous fibers; 1-5 parts of a compatibilizer; 0.5-5 parts of hollow microspheres; 1-5 parts of an elastomer; 0.1-5 parts of a processing aid. The basalt fiber/nylon composite material provided by the invention has excellent acid and alkali corrosion resistance, is large in use temperature range, is lighter without influencing mechanical properties, and is suitable for outdoor and underwater in coastal areas.
In order to further illustrate the present invention, the following describes in detail a basalt continuous filament reinforced nylon composite material and a preparation method thereof provided by the present invention with reference to examples.
Examples 1 to 4
The preparation method comprises the following steps: during processing, organic raw materials including the nylon resin matrix and the compatibilizer are mixed to obtain a first premixed melting material; drying the basalt continuous fibers by a preheating device; a first pre-mixed melt is extruded into a melt impregnation die. Enabling the dried basalt continuous fibers to pass through a melting impregnation die, and continuously producing the basalt continuous fibers under the traction of a front tractor at the speed of 2-12 m/min to obtain the continuous composite master batch; cutting the obtained composite master batch into composite granules with uniform length of 10-20 mm by a shearing machine; mixing the obtained composite granules, the hollow microspheres and the elastomer as inner raw materials to obtain a second premixed melting material; and preparing the second premixed melt into the required finished product of the wuyan fiber-nylon resin composite material through direct injection molding, direct compression molding and direct extrusion molding.
Example 1:
step 1: firstly, mixing organic raw materials including the nylon 6 resin matrix and the solubilizer according to the proportion in the table 1 to obtain a first premixed melt, wherein the temperature of a fourth zone of the charging barrel is as follows: 236 ℃, 242 ℃, 247 ℃, 252 ℃, the screw rotation speed is 65r/min, and the feeding speed is 5 r/min;
step 2: drying the basalt continuous fibers by a preheating device, wherein the preheating temperature is 182 ℃;
and step 3: extruding the first premixed melt obtained in the step 1 into a melting impregnation die, wherein the temperature of the four regions of the impregnation die is 273 ℃, 277 ℃, 284 ℃ and 286 ℃;
and 4, step 4: continuously producing the dried basalt continuous fibers in a melting impregnation die by a front tractor at the speed of 8m/min to obtain the continuous composite master batch;
and 5: cutting the composite master batch obtained in the step 4 into composite granules with uniform length of 10mm by a shearing machine;
step 6: mixing the composite granules obtained in the step 5, the hollow microspheres and the elastomer as inner raw materials to obtain a second premixed melting material;
and 7: and (4) preparing the second premixed melting material obtained in the step (6) into a test shape through pultrusion to obtain a finished product of the Wuyan fiber-unsaturated resin composite material.
Example 2:
step 1: firstly, mixing organic raw materials including the nylon 6 resin matrix and the solubilizer according to the proportion in the table 1 to obtain a first premixed melt, wherein the temperature of a fourth zone of the charging barrel is as follows: 238 ℃, 243 ℃, 248 ℃, 253 ℃, the screw rotation speed is 65r/min, and the feeding speed is 5 r/min;
step 2: drying the basalt continuous fibers by a preheating device, wherein the preheating temperature is 185 ℃;
and step 3: extruding the first premixed melt obtained in the step 1 into a melting impregnation die, wherein the temperature of a fourth zone of the impregnation die is 274 ℃, 279 ℃, 284 ℃ and 286 ℃;
and 4, step 4: continuously producing the dried basalt continuous fibers in a melting impregnation die by a front tractor at the speed of 9m/min to obtain the continuous composite master batch;
and 5: cutting the composite master batch obtained in the step 4 into composite granules with uniform length of 10mm by a shearing machine;
step 6: mixing the composite granules obtained in the step 5, the hollow microspheres and the elastomer as inner raw materials to obtain a second premixed melting material;
and 7: and (4) preparing the second premixed melt obtained in the step (6) into a test shape through pultrusion to obtain a required finished product of the wurtzite fiber-unsaturated resin composite material.
Example 3:
step 1: firstly, mixing organic raw materials including the nylon 6 resin matrix and the solubilizer according to the proportion in the table 1 to obtain a first premixed melt, wherein the temperature of a fourth zone of the charging barrel is as follows: 239 ℃, 244 ℃, 249 ℃, 254 ℃, 65r/min screw rotation speed and 5r/min feeding speed;
step 2: drying the basalt continuous fibers by a preheating device, wherein the preheating temperature is 190 ℃;
and step 3: extruding the first premixed melt obtained in the step 1 into a melting impregnation die, wherein the temperature of a fourth zone of the impregnation die is 275 ℃, 279 ℃, 284 ℃ and 288 ℃;
and 4, step 4: enabling the dried basalt continuous fibers to pass through a melting impregnation die, and continuously producing the basalt continuous fibers under the traction of a front tractor at the speed of 10.5m/min to obtain the continuous composite master batch;
and 5: cutting the composite master batch obtained in the step 4 into composite granules with uniform length of 10mm by a shearing machine;
step 6: mixing the composite granules obtained in the step 5, the hollow microspheres and the elastomer as inner raw materials to obtain a second premixed melting material;
and 7: and (4) preparing the second premixed melt obtained in the step (6) into a test shape through pultrusion to obtain a required finished product of the wurtzite fiber-unsaturated resin composite material.
Example 4:
step 1: firstly, mixing organic raw materials including the nylon 6 resin matrix and the solubilizer according to the proportion in the table 1 to obtain a first premixed melt, wherein the temperature of a fourth zone of the charging barrel is as follows: the temperature of 240 ℃, 245 ℃, 250 ℃, 255 ℃, the screw rotation speed of 65r/min and the feeding speed of 5 r/min;
step 2: drying the basalt continuous fibers by a preheating device, wherein the preheating temperature is 195 ℃;
and step 3: extruding the first premixed melt obtained in the step 1 into a melting impregnation die, wherein the temperature of the four regions of the impregnation die is 275 ℃, 282 ℃, 287 ℃ and 290 ℃;
and 4, step 4: enabling the dried basalt continuous fibers to pass through a melting impregnation die, and continuously producing the basalt continuous fibers under the traction of a front tractor at the speed of 12m/min to obtain the continuous composite master batch;
and 5: cutting the composite master batch obtained in the step 4 into composite granules with uniform length of 10mm by a shearing machine;
step 6: mixing the composite granules obtained in the step 5, the hollow microspheres and the elastomer as inner raw materials to obtain a second premixed melting material;
and 7: and (4) preparing the second premixed melt obtained in the step (6) into a test shape through pultrusion to obtain a required finished product of the wurtzite fiber-unsaturated resin composite material.
Comparative example 1:
step 1: firstly, mixing organic raw materials including the nylon 6 resin matrix and the solubilizer according to the proportion in the table 1 to obtain a first premixed melt, wherein the temperature of a fourth zone of the charging barrel is as follows: 235 ℃, 240 ℃, 245 ℃, 250 ℃, the screw rotation speed is 65r/min, and the feeding speed is 5 r/min;
step 2: drying the basalt continuous fibers by a preheating device, wherein the preheating temperature is 180 ℃;
and step 3: extruding the first premixed melt obtained in the step 1 into a melting impregnation die, wherein the temperature of a fourth area of the impregnation die is 270 ℃, 275 ℃, 280 ℃ and 285 ℃;
and 4, step 4: enabling the dried basalt continuous fibers to pass through a melting impregnation die, and continuously producing the basalt continuous fibers under the traction of a front tractor at the speed of 7m/min to obtain the continuous composite master batch;
and 5: cutting the composite master batch obtained in the step 4 into composite granules with uniform length of 10mm by a shearing machine;
step 6: mixing the composite granules obtained in the step 5, the hollow microspheres and the elastomer as inner raw materials to obtain a second premixed melting material;
and 7: and (4) preparing the second premixed melt obtained in the step (6) into a test shape through pultrusion to obtain a required finished product of the wurtzite fiber-unsaturated resin composite material.
TABLE 1 EXAMPLES 1-4# AND COMPARATIVE EXAMPLE 1 (wt%)
Comparative example 2
A30% glass fiber reinforced nylon 6 composite material produced by a company of Sichuan province was used as a comparison.
Comparative example 3
43% glass fiber reinforced nylon 6 composite material produced by a company of Zhejiang province was used as a comparison.
Comparative example 4
The 60% glass fiber reinforced nylon 6 composite material produced by a company of Sichuan province was used as a comparison.
The mechanical property test of the material is as follows: tensile properties according to GB/T1040.2-2006, flexural properties according to GB/T9341-2008 and impact properties according to GB/T1843-2008.
Table 2. results of mechanical property test when the embodiment and the control group are not soaked in seawater:
| item | Fiber content | Tensile strength | Bending strength | Impact strength | Dielectric constant of |
| 1# | 20％ | 144MPa | 156MPa | 8.8kJ/m2 | 3.3 |
| 2# | 30％ | 170MPa | 168MPa | 10.7kJ/m 2 | 3.3 |
| 3# | 40％ | 179MPa | 173MPa | 11.9kJ/m 2 | 3.2 |
| 4# | 50％ | 190MPa | 181MPa | 13.2kJ/m 2 | 3.2 |
| Comparative example 1 | 10％ | 100MPa | 135MPa | 8.2kJ/m 2 | 3.5 |
| Comparative example 2 | 30％ | 149MPa | 159MPa | 11.0kJ/m 2 | 3.5 |
| Comparative example 3 | 43％ | 170MPa | 169MPa | 12.0kJ/m 2 | 3.7 |
| Comparative example 4 | 60％ | 192MPa | 181MPa | 13.3kJ/m 2 | 3.8 |
Table 3. mechanical property test results of the embodiment and the control group after soaking for 180 days under seawater condition:
the foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The basalt continuous fiber reinforced nylon composite material is characterized by comprising the following raw materials in parts by weight:
2. the material of claim 1, wherein the nylon resin is selected from one or more of nylon 6, nylon 66, nylon 610, nylon 11, nylon 12.
3. The material of claim 1, wherein the compatibilizer is one or more of MAH cyclic anhydride type and maleic anhydride.
4. The material of claim 1, wherein the basalt continuous filament is one or more of BS, BF, BM, BAS, BTR; the basalt continuous fiber BF general type: sichuan humble BF815-2400, Guizhou Shixin BF22-2400, and Taian Hao pine xwy-14.
5. The material of claim 1, wherein the cenospheres are one or more of 3MK1, IM16K, S15, IM30K, K20, S38HS, zhongmei ZM-K25, or AStrong 2046H;
the elastomer is one or more of nylon 12, polycarbonate or PPS;
the processing aid is one or more of a lubricant, a dispersant, an anti-aging agent, a defoaming agent or an antistatic agent.
6. The material of claim 1, wherein the basalt continuous fiber reinforced nylon composite material comprises the following raw materials in parts by weight:
7. a preparation method of the basalt continuous fiber reinforced nylon composite material as claimed in any one of claims 1 to 6, characterized by comprising the following steps:
A) mixing nylon resin and a compatibilizer to obtain a first premix;
B) extruding the first premix to obtain an extruded material; melting and dipping the extruded material and the basalt continuous fiber, drawing and shearing to obtain composite granules;
C) mixing the composite granules, the hollow microspheres, the elastomer and the processing aid to obtain a second premix; and forming the second premix to obtain the product.
8. The method as claimed in claim 7, wherein the drawing speed in step B) is 8 to 12 m/min.
9. The method according to claim 7, wherein the length of the composite pellet of step B) is 10 to 20 mm.
10. The method of claim 7, wherein the extrusion parameters are
The temperature of each section of a charging barrel of the double-screw extruder is 235-255 ℃; the rotating speed of the screw is 50-80 r/min; the feeding speed is 4-8 r/min.
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