CN118109046A - Preparation method of nylon 66 material - Google Patents
Preparation method of nylon 66 material Download PDFInfo
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- CN118109046A CN118109046A CN202410231705.8A CN202410231705A CN118109046A CN 118109046 A CN118109046 A CN 118109046A CN 202410231705 A CN202410231705 A CN 202410231705A CN 118109046 A CN118109046 A CN 118109046A
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- nylon
- auxiliary agent
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- polytetrafluoroethylene
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- 239000000463 material Substances 0.000 title claims abstract description 116
- 229920002302 Nylon 6,6 Polymers 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- -1 polypropylene Polymers 0.000 claims abstract description 97
- 239000000835 fiber Substances 0.000 claims abstract description 59
- 239000004743 Polypropylene Substances 0.000 claims abstract description 58
- 229920001155 polypropylene Polymers 0.000 claims abstract description 58
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 29
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 27
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 27
- 239000002270 dispersing agent Substances 0.000 claims abstract description 24
- 229920005989 resin Polymers 0.000 claims abstract description 22
- 239000011347 resin Substances 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 239000000126 substance Substances 0.000 claims abstract description 9
- 238000001125 extrusion Methods 0.000 claims abstract description 7
- 238000005469 granulation Methods 0.000 claims abstract description 7
- 230000003179 granulation Effects 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N monopropylene glycol Natural products CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 21
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 20
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical group [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 20
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 20
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 20
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 20
- 238000001816 cooling Methods 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 14
- 239000008116 calcium stearate Substances 0.000 claims description 14
- 235000013539 calcium stearate Nutrition 0.000 claims description 14
- IPNFHEWNDOORKH-UHFFFAOYSA-N 6-methylheptyl 2-hydroxybenzoate Chemical compound CC(C)CCCCCOC(=O)C1=CC=CC=C1O IPNFHEWNDOORKH-UHFFFAOYSA-N 0.000 claims description 12
- 239000004115 Sodium Silicate Substances 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 12
- 235000010290 biphenyl Nutrition 0.000 claims description 12
- 239000004305 biphenyl Substances 0.000 claims description 12
- 239000004202 carbamide Substances 0.000 claims description 12
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims description 12
- 229960004063 propylene glycol Drugs 0.000 claims description 12
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 12
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 12
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 12
- 239000010445 mica Substances 0.000 claims description 11
- 229910052618 mica group Inorganic materials 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 8
- 229910001220 stainless steel Inorganic materials 0.000 claims description 8
- 239000010935 stainless steel Substances 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 5
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims description 3
- 235000013772 propylene glycol Nutrition 0.000 claims description 3
- 239000002253 acid Substances 0.000 abstract description 9
- 239000003513 alkali Substances 0.000 abstract description 9
- 238000013329 compounding Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 23
- 230000000052 comparative effect Effects 0.000 description 11
- 239000004677 Nylon Substances 0.000 description 7
- 229920001778 nylon Polymers 0.000 description 7
- 239000002904 solvent Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 230000001105 regulatory effect Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000032683 aging Effects 0.000 description 4
- 239000008187 granular material Substances 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- VCCBEIPGXKNHFW-UHFFFAOYSA-N biphenyl-4,4'-diol Chemical group C1=CC(O)=CC=C1C1=CC=C(O)C=C1 VCCBEIPGXKNHFW-UHFFFAOYSA-N 0.000 description 3
- 238000005461 lubrication Methods 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000005856 abnormality Effects 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 230000003712 anti-aging effect Effects 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000032798 delamination Effects 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 2
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000012745 toughening agent Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000006231 channel black Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 235000019359 magnesium stearate Nutrition 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 1
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 229920006126 semicrystalline polymer Polymers 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 229920006352 transparent thermoplastic Polymers 0.000 description 1
Classifications
-
- 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
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/322—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
- D06M13/402—Amides imides, sulfamic acids
- D06M13/432—Urea, thiourea or derivatives thereof, e.g. biurets; Urea-inclusion compounds; Dicyanamides; Carbodiimides; Guanidines, e.g. dicyandiamides
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The invention discloses a preparation method of a nylon 66 material, which comprises the following steps: (1) Placing the modified polypropylene fiber, polytetrafluoroethylene, an auxiliary agent and nylon 66 resin into a high-speed mixer to be uniformly mixed to obtain a mixed material; (2) And (3) mixing the uniformly mixed material obtained in the step (1) and the dispersing agent again, and then placing the mixture into a double-screw extruder for extrusion granulation to obtain the nylon 66 material. According to the method, the modified polypropylene fiber, the polytetrafluoroethylene and the auxiliary agent are added, and the nylon 66 material prepared through reasonable compounding has good tensile property, thermal stability and acid and alkali resistance, and is very suitable for the field of chemical equipment.
Description
Technical Field
The invention relates to the technical field of preparation of high polymer materials, in particular to a preparation method of a nylon 66 material.
Background
Nylon 66 (Nylon 66) is one of the most widely used Nylon products that were developed the earliest with the greatest yields. The nylon 66 is a colorless transparent thermoplastic resin formed by polycondensation of adipic acid and hexamethylenediamine, is a polycrystalline semi-crystalline polymer, and is easy to be oriented because a large number of polar amide bonds exist on the molecular chain of the nylon 66, and the nylon is easy to absorb water to form hydrogen bonds in the main chain. Nylon 66 as one kind of engineering plastic has excellent mechanical performance, oil resistance, wear resistance, self lubrication, etc. and is used widely in automobile, electronic and electric, packing material, etc. and in addition, it has wide application in cosmetics, adhesive, etc.
For nylon 66 materials, the materials can be greatly degraded under high-temperature processing conditions and severe service environments due to poor long-term heat aging resistance. The main improvement mode of the heat aging resistance of the nylon 66 at present is to blend the prepared nylon 66 with an antioxidant, a heat stabilizer and the like, so that the heat aging resistance of the nylon 66 is improved. Patent CN201210295603.X discloses an anti-aging lubrication nylon 66 material with moderate rigidity and toughness, which adopts inorganic powder, an antiwear agent, a toughening agent, an anti-aging auxiliary agent, an internal lubrication processing auxiliary agent and the like to carry out composite modification on the nylon 66 material, and at least comprises (weight percent) nylon 66-100 parts; 5-25 parts of a toughening agent; 5-50 parts of talcum powder; 2-10 parts of molybdenum disulfide; 2-5 parts of channel black. The nylon 66 material prepared by the process has good ageing resistance, but the high temperature resistance of the nylon 66 material is to be improved.
Patent CN202010128564.9 discloses a heat-conducting nylon 66 material and its preparation method, which is prepared by 69.1-89.8% nylon 66, 10-30% heat-conducting modifier, 0.1-0.3% lubricant and 0.1-0.6% antioxidant according to weight percentage, wherein the heat-conducting modifier is 4,4' -dihydroxybiphenyl modified nylon, and the 4,4' -dihydroxybiphenyl modified nylon is prepared by reflux reaction of nylon 66 and 4,4' -dihydroxybiphenyl with potassium carbonate in DMF solution. The nylon 66 material has better mechanical properties while realizing heat conduction, and in the actual use process, the nylon material has better properties and can be applied to various fields with harsh conditions, for example, substances such as acidic water or alkaline water possibly exist in reaction equipment of some oil refineries or chemical plant workshops, so that various materials used by related equipment are required to be capable of tolerating acid and alkali.
Disclosure of Invention
Aiming at the problems of the prior art that the high temperature resistance of the synthetic nylon 66 material is to be improved and the acid and alkali resistance is poor, the invention provides a preparation method of the nylon 66 material.
In order to solve the technical problems, the invention provides the following technical scheme:
The preparation method of the nylon 66 material comprises the following steps:
(1) Placing the modified polypropylene fiber, polytetrafluoroethylene, an auxiliary agent and nylon 66 resin into a high-speed mixer to be uniformly mixed to obtain a mixed material; (2) And (3) mixing the uniformly mixed material obtained in the step (1) and the dispersing agent again, and then placing the mixture into a double-screw extruder for extrusion granulation to obtain the nylon 66 material. Further, 40-58 parts of nylon 66 resin, 2-10 parts of polytetrafluoroethylene, 0.1-3 parts of auxiliary agent and 13-25 parts of modified polypropylene fiber.
Further, the mass of the dispersing agent is 1-3% of the mass of the mixture, and the dispersing agent is sodium pyrophosphate and polyethylene glycol 400.
Further, the preparation method of the modified polypropylene fiber comprises the following steps:
preparing sodium metasilicate, urea and deionized water into a mixed solution, putting polypropylene fibers into the mixed solution, then placing the mixed solution into a stainless steel reaction kettle for treatment at 100-120 ℃ for 4-7h, taking out the mixed solution after the treatment is finished, cooling to room temperature, and drying for later use.
Further, the mass ratio of the sodium metasilicate to the urea is 100:1-6.
Further, the auxiliary agent comprises isooctyl salicylate, diphenyl azide phosphate, 1, 2-propylene glycol, mica and calcium stearate. Further, the mass ratio of the isooctyl salicylate to the diphenyl azide phosphate to the 1, 2-propylene glycol to the mica to the calcium stearate is 100:1-8:15-36:0.1-1:5-10.
Further, the temperature of the double-screw extruder is 360-370 ℃, the screw rotating speed is 90-120 r/min, the feeding rotating speed is 10-15 r/min, the nylon 66 material is obtained through melt extrusion and water-cooling bracing granulation. Nylon 66 material obtained according to the above preparation method.
The nylon 66 material prepared by the preparation method is applied to the field of chemical equipment.
The invention has the following beneficial effects:
1. According to the nylon 66 material provided by the invention, based on the original nylon 66 resin, the modified polypropylene fiber is added, so that the tensile property of the nylon 66 material is effectively improved, and the mechanical property of the nylon 66 material is greatly improved; by adding polytetrafluoroethylene and an auxiliary agent and reasonably compounding, the acid and alkali resistance and the thermal stability of the nylon 66 material are effectively improved, the high-stability application requirements of products such as coil frameworks, sealing rings and the like used in chemical plant equipment on plastic materials can be completely met, and the nylon 66 material has good market application value.
2. According to the nylon 66 material provided by the invention, the dispersing agent is added in the mixing process, so that the materials can be well mixed, the modified polypropylene fibers, the polytetrafluoroethylene and the auxiliary agent can be fully dispersed, and the difference of the performances of the nylon 66 materials in the same batch in the follow-up process caused by uneven material mixing in the melting process is avoided.
3. The preparation method of the nylon 66 material provided by the invention has the advantages that the raw material components are convenient to obtain, the preparation process is simple, and the preparation cost of the whole nylon 66 material is effectively reduced.
Drawings
FIG. 1 is a graph showing the results of thermal deformation temperature detection of nylon 66 materials provided by the invention.
Detailed Description
The preparation method of the nylon 66 material provided by the invention comprises (1) placing modified polypropylene fiber, polytetrafluoroethylene, an auxiliary agent and nylon 66 resin into a high-speed mixer to be uniformly mixed to obtain a mixed material; (2) And (3) mixing the uniformly mixed material obtained in the step (1) and the dispersing agent again, and then placing the mixture into a double-screw extruder for extrusion granulation to obtain the nylon 66 material.
According to the method provided by the invention, in a preferred case, the method for modifying polypropylene fibers: preparing a solution containing sodium metasilicate and urea, wherein a solvent is deionized water, then placing polypropylene fibers into the prepared solution, then placing the polypropylene fibers into a stainless steel reaction kettle for treatment at 100-120 ℃ for 4-7 hours, taking out the polypropylene fibers after the treatment is finished, cooling to room temperature and drying for standby, wherein the mass ratio of the sodium metasilicate to the urea is 100:1-6, and the specific drying is carried out in a common oven under the condition of drying at 90 ℃ for 2 hours.
According to the method provided by the invention, in a preferred case, 40-58 parts of nylon 66 resin, 2-10 parts of polytetrafluoroethylene, 0.1-3 parts of auxiliary agent and 13-25 parts of modified polypropylene fiber are calculated according to the parts by mass of the modified polypropylene fiber, the polytetrafluoroethylene, the auxiliary agent and the nylon 66 resin.
According to the method provided by the invention, the mass of the dispersing agent is 1-3% of the mass of the mixed material, and the dispersing agent is sodium pyrophosphate and polyethylene glycol 400, wherein the mass ratio of the sodium pyrophosphate to the polyethylene glycol 400 in the dispersing agent can be used under the condition that the total mass is determined, and the quantity of the sodium pyrophosphate and the polyethylene glycol 400 has little influence on the subsequent preparation process and the performance of the obtained nylon 66 material, but the two dispersing agents are preferably used simultaneously, and the aim is only to facilitate the full dispersion of the components in the nylon 66 and ensure that the components are uniformly mixed.
According to the method provided by the invention, the auxiliary agent comprises isooctyl salicylate, diphenyl azide phosphate, 1, 2-propylene glycol, mica and calcium stearate in a preferred mode.
According to the method provided by the invention, the mass ratio of the isooctyl salicylate, the diphenyl azide phosphate, the 1, 2-propylene glycol, the mica and the calcium stearate is 100:1-8:15-36:0.1-1:5-10 in a preferred case.
According to the method provided by the invention, under the preferable condition, the temperature of the double-screw extruder is 360-375 ℃, the screw rotating speed is 90-120 r/min, the feeding rotating speed is 10-15 r/min, the lateral feeding rotating speed is 10r/min, and the nylon 66 material is obtained through melt extrusion and water-cooling bracing granulation.
According to the method provided by the invention, the temperatures of the first to eighth zones of the twin-screw extruder are set as follows: 360 ℃,365 ℃,375 ℃,370 ℃,375 ℃,370 ℃,375 ℃,370 ℃. Varying the temperature of the various zones of the twin screw extruder can significantly affect the properties of the final nylon 66 material.
The nylon 66 material prepared by the method provided by the invention.
According to the method provided by the invention, the method further comprises the steps of water-cooling and granulating the finally extruded material, and then drying to obtain the product, wherein the drying temperature is 85-95 ℃.
The technical scheme of the present invention will be clearly and completely described in the following in connection with specific embodiments.
The chemicals described in the examples of the present invention, such as sodium metasilicate, urea, isooctyl salicylate, diphenyl azide phosphate, and 1, 2-propanediol, are commercially available directly from the commercial sources, and nylon 66 resins used are available from Zhejiang Huafeng synthetic resins, inc., under the designation EP158.
Example 1
Preparation of modified Polypropylene fiber
Preparing a modified solution according to the mass ratio of sodium metasilicate to urea of 100:6, wherein the solvent is deionized water, immersing polypropylene fibers (purchased from Tianyi engineering fiber Co., ltd., polypropylene monofilament fibers) into the prepared modified solution, then placing the polypropylene fibers in a stainless steel reaction kettle for treatment at 110 ℃ for 5 hours, taking out the modified solution after the treatment is completed, cooling to room temperature, and then placing the modified solution in an oven for drying at 90 ℃ for 2 hours for later use.
Preparation of nylon 66 material
Firstly, the modified polypropylene fiber, polytetrafluoroethylene, an auxiliary agent and nylon 66 resin are mixed according to the weight parts: 50 parts of nylon 66 resin, 2 parts of polytetrafluoroethylene, 1 part of an auxiliary agent and 15 parts of modified polypropylene fiber, wherein the auxiliary agent comprises isooctyl salicylate, diphenyl azide phosphate, 1, 2-propylene glycol, mica and calcium stearate, and the corresponding mass ratio is 100:5:20:1:5. And (5) placing the materials into a high-speed mixer for 5 minutes, and uniformly mixing to obtain a mixed material.
And weighing sodium pyrophosphate and polyethylene glycol 400 as dispersing agents, wherein the total mass of the sodium pyrophosphate and the polyethylene glycol 400 is 3% of the total mass of the uniformly mixed materials, the mass ratio of the sodium pyrophosphate to the polyethylene glycol 400 is 1:1, mixing the mixed materials and the dispersing agents again for 2 minutes, placing the materials in a double-screw extruder for heating and melting, cooling by water, drawing into granules, and drying at 85 ℃ to obtain the nylon 66 material.
The operating parameters of the twin-screw extruder were set as follows: the temperatures of the first to eighth zones of the twin-screw extruder were set as follows: 360 ℃,365 ℃,375 ℃,370 ℃,375 ℃,370 ℃,375 ℃,370 ℃ and the temperature of the machine head is regulated to 370 ℃, the rotating speed of the screw is 90-120 r/min, the feeding rotating speed is 15r/min, and the lateral feeding rotating speed is 10r/min.
Example 2
Preparation of modified Polypropylene fiber
According to the mass ratio of sodium metasilicate to urea of 100:1 preparing a modified solution, wherein the solvent is deionized water, immersing polypropylene fibers (purchased from Tianyi engineering fiber Co., ltd., polypropylene monofilament fibers) into the prepared modified solution, then placing the polypropylene fibers in a stainless steel reaction kettle for treatment at 120 ℃ for 4 hours, taking out the polypropylene fibers after the treatment is completed, cooling the polypropylene fibers to room temperature, and then placing the polypropylene fibers in an oven for baking at 90 ℃ for 2 hours for later use.
Preparation of nylon 66 material
Firstly, the modified polypropylene fiber, polytetrafluoroethylene, an auxiliary agent and nylon 66 resin are mixed according to the weight parts: 50 parts of nylon 66 resin, 2 parts of polytetrafluoroethylene, 1 part of an auxiliary agent and 15 parts of modified polypropylene fiber, wherein the auxiliary agent comprises isooctyl salicylate, diphenyl azide phosphate, 1, 2-propylene glycol, mica and calcium stearate, and the corresponding mass ratio is 100:5:20:1:5. And (5) placing the materials into a high-speed mixer for 5 minutes, and uniformly mixing to obtain a mixed material.
And weighing sodium pyrophosphate and polyethylene glycol 400 as dispersing agents, wherein the total mass of the sodium pyrophosphate and the polyethylene glycol 400 is 3% of the total mass of the uniformly mixed materials, the mass ratio of the sodium pyrophosphate to the polyethylene glycol 400 is 1:1, mixing the mixed materials and the dispersing agents again for 2 minutes, placing the materials in a double-screw extruder for heating and melting, cooling by water, drawing into granules, and drying at 85 ℃ to obtain the nylon 66 material.
The operating parameters of the twin-screw extruder were set as follows: the temperatures of the first to eighth zones of the twin-screw extruder were set as follows: 360 ℃,365 ℃,375 ℃,370 ℃,375 ℃,370 ℃,375 ℃,370 ℃ and the temperature of the machine head is regulated to 370 ℃, the rotating speed of the screw is 90-120 r/min, the feeding rotating speed is 15r/min, and the lateral feeding rotating speed is 10r/min.
Example 3
Preparation of modified Polypropylene fiber
Preparing a modified solution according to the mass ratio of sodium metasilicate to urea of 100:6, wherein the solvent is deionized water, immersing polypropylene fibers (purchased from Tianyi engineering fiber Co., ltd., polypropylene monofilament fibers) into the prepared modified solution, then placing the polypropylene fibers in a stainless steel reaction kettle for treatment at 120 ℃ for 4 hours, taking out the modified solution after the treatment is completed, cooling to room temperature, and then placing the modified solution in an oven for drying at 90 ℃ for 2 hours for later use.
Preparation of nylon 66 material
Firstly, the modified polypropylene fiber, polytetrafluoroethylene, an auxiliary agent and nylon 66 resin are mixed according to the weight parts: 40 parts of nylon 66 resin, 10 parts of polytetrafluoroethylene, 1 part of an auxiliary agent and 20 parts of modified polypropylene fiber, wherein the auxiliary agent comprises isooctyl salicylate, diphenyl azide phosphate, 1, 2-propylene glycol, mica and calcium stearate, and the corresponding mass ratio is 100:1:36:1:8. And (5) placing the materials into a high-speed mixer for 5 minutes, and uniformly mixing to obtain a mixed material.
And weighing sodium pyrophosphate and polyethylene glycol 400 as dispersing agents, wherein the total mass of the sodium pyrophosphate and the polyethylene glycol 400 is 3% of the total mass of the uniformly mixed materials, the mass ratio of the sodium pyrophosphate to the polyethylene glycol 400 is 1:1, mixing the mixed materials and the dispersing agents again for 2 minutes, placing the materials in a double-screw extruder for heating and melting, cooling by water, drawing into granules, and drying at 85 ℃ to obtain the nylon 66 material.
The operating parameters of the twin-screw extruder were set as follows: the temperatures of the first to eighth zones of the twin-screw extruder were set as follows: 360 ℃,365 ℃,375 ℃,370 ℃,375 ℃,370 ℃,375 ℃,370 ℃ and the temperature of the machine head is regulated to 370 ℃, the rotating speed of the screw is 90-120 r/min, the feeding rotating speed is 15r/min, and the lateral feeding rotating speed is 10r/min.
Example 4
Preparation of modified Polypropylene fiber
Preparing a modified solution according to the mass ratio of sodium metasilicate to urea of 100:6, wherein the solvent is deionized water, immersing polypropylene fibers (purchased from Tianyi engineering fiber Co., ltd., polypropylene monofilament fibers) into the prepared modified solution, then placing the polypropylene fibers in a stainless steel reaction kettle for treatment at 120 ℃ for 4 hours, taking out the modified solution after the treatment is completed, cooling to room temperature, and then placing the modified solution in an oven for drying at 90 ℃ for 2 hours for later use.
Preparation of nylon 66 material
Firstly, the modified polypropylene fiber, polytetrafluoroethylene, an auxiliary agent and nylon 66 resin are mixed according to the weight parts: 58 parts of nylon 66 resin, 10 parts of polytetrafluoroethylene, 0.1 part of auxiliary agent and 13 parts of modified polypropylene fiber, wherein the auxiliary agent is isooctyl salicylate, diphenyl azide phosphate, 1, 2-propylene glycol, mica and calcium stearate, and the corresponding mass ratio is 100:8:15:0.1:10. And (5) placing the materials into a high-speed mixer for 5 minutes, and uniformly mixing to obtain a mixed material.
Sodium pyrophosphate and polyethylene glycol 400 are weighed as dispersing agents, wherein the total mass of the sodium pyrophosphate and the polyethylene glycol 400 is 1% of the total mass of the uniformly mixed materials, and the mass ratio of the sodium pyrophosphate to the polyethylene glycol 400 is 1:1, mixing the mixed material and the dispersing agent for 2 minutes again, placing the mixed material and the dispersing agent in a double-screw extruder for heating and melting, extruding, water-cooling, then bracing and granulating, and drying at 85 ℃ to obtain the nylon 66 material.
The operating parameters of the twin-screw extruder were set as follows: the temperatures of the first to eighth zones of the twin-screw extruder were set as follows: 360 ℃,365 ℃,375 ℃,370 ℃,375 ℃,370 ℃,375 ℃,370 ℃ and the temperature of the machine head is regulated to 370 ℃, the rotating speed of the screw is 90-120 r/min, the feeding rotating speed is 15r/min, and the lateral feeding rotating speed is 10r/min.
Example 5
Preparation of modified Polypropylene fiber
Preparing a modified solution according to the mass ratio of sodium metasilicate to urea of 100:1, wherein the solvent is deionized water, immersing polypropylene fibers (purchased from Tianyi engineering fiber Co., ltd., polypropylene monofilament fibers) into the prepared modified solution, then placing the polypropylene fibers in a stainless steel reaction kettle for treatment at 120 ℃ for 4 hours, taking out the modified solution after the treatment is completed, cooling to room temperature, and then placing the modified solution in an oven for drying at 90 ℃ for 2 hours for later use.
Preparation of nylon 66 material
Firstly, the modified polypropylene fiber, polytetrafluoroethylene, an auxiliary agent and nylon 66 resin are mixed according to the weight parts: 58 parts of nylon 66 resin, 10 parts of polytetrafluoroethylene, 3 parts of auxiliary agent and 25 parts of modified polypropylene fiber, wherein the auxiliary agent comprises isooctyl salicylate, diphenyl azide phosphate, 1, 2-propylene glycol, mica and calcium stearate, and the corresponding mass ratio is 100:8:36:1:10. And (5) placing the materials into a high-speed mixer for 5 minutes, and uniformly mixing to obtain a mixed material.
And weighing sodium pyrophosphate and polyethylene glycol 400 as dispersing agents, wherein the total mass of the sodium pyrophosphate and the polyethylene glycol 400 is 3% of the total mass of the uniformly mixed materials, the mass ratio of the sodium pyrophosphate to the polyethylene glycol 400 is 1:1, mixing the mixed materials and the dispersing agents again for 2 minutes, placing the materials in a double-screw extruder for heating and melting, cooling by water, drawing into granules, and drying at 95 ℃ to obtain the nylon 66 material.
The operating parameters of the twin-screw extruder were set as follows: the temperatures of the first to eighth zones of the twin-screw extruder were set as follows: 360 ℃,365 ℃,375 ℃,370 ℃,375 ℃,370 ℃,375 ℃,370 ℃ and the temperature of the machine head is regulated to 370 ℃, the rotating speed of the screw is 90-120 r/min, the feeding rotating speed is 15r/min, and the lateral feeding rotating speed is 10r/min.
Comparative example 1
The modified polypropylene fiber was prepared in the same manner as in example 2; the nylon 66 material was prepared without polytetrafluoroethylene addition, and the procedure was the same as in example 2.
Comparative example 2
The modified polypropylene fiber was prepared in the same manner as in example 2; the preparation of nylon 66 material was carried out without adding calcium stearate in the auxiliary agent, and the other steps were the same as in example 2.
Comparative example 3
The modified polypropylene fiber was prepared in the same manner as in example 2; the calcium stearate in the auxiliary agent in the preparation process of the nylon 66 material is changed into magnesium stearate, and the other materials are the same as in the example 2.
Comparative example 4
Unmodified polypropylene fibers were not added in the preparation process of the nylon 66 material, and the other materials were the same as in example 2.
Evaluation of Nylon 66 Material Performance
Thermal deformation detection instrument: changzhou De Du Jingmi instruments Co., ltd., instrument model: TSWL-RWK thermal deformation Vicat softening point temperature tester, according to ISO 75 published method. The nylon 66 materials prepared in examples 1 to 5 and comparative examples 1 to 4 were examined for heat distortion temperature, respectively, and specific examination results are shown in FIG. 1.
It can be seen from fig. 1 that the addition of polytetrafluoroethylene and calcium stearate significantly improves the thermal stability of the nylon 66 material, and that the addition of the modified polyester fiber has relatively little effect on the thermal stability properties of the prepared nylon 66 material.
Tensile Properties
The test was carried out in accordance with ISO527-2, the stretching speed being 15mm/min and the test temperature being 23 ℃. The nylon 66 materials prepared in examples 1 to 5 and comparative examples 1 to 4 were examined for tensile strength on an electronic tensile tester, respectively, and the specific examination results are shown in Table 1.
TABLE 1
From the above results of the tensile strength test in table 1, it was found that when the components such as unmodified polypropylene fibers and nylon were compounded, the tensile strength of the finally prepared nylon 66 material was significantly reduced, whereas comparative examples 1 to 3 were modified by the addition of polytetrafluoroethylene and an auxiliary agent, but the tensile strength was not particularly significantly reduced.
Acid resistance
The detection standard and method are carried out according to the method disclosed in GB/T11547-2008, the sample is immersed in 5% sulfuric acid solution for 1 week at normal temperature, taken out and dried at 50 ℃ for 2 hours, and then whether the sample and the sample before treatment exist or not is detected: surface tackiness; delamination, warpage or other deformation; partially dissolving; the surface is provided with a substance which is easy to wipe off; bubbling, pit, or other similar defects, etc., and if the above type of change occurs, the failure is determined, and if no abnormality occurs, the failure is determined.
Alkali resistance
Detection standard and method GB/T11547-2008, immersing in 5% sodium hydroxide solution for 1 week, taking out, drying at 50deg.C for 2 hours, and detecting whether the sample and the sample before treatment are present: surface tackiness; delamination, warpage or other deformation; partially dissolving; the surface is provided with a substance which is easy to wipe off; bubbling, pit, or other similar defects, etc., and if the above type of change occurs, the failure is determined, and if no abnormality occurs, the failure is determined.
The nylon 66 materials prepared in examples 1 to 5 and comparative examples 1 to 4 were subjected to the above-mentioned acid resistance and alkali resistance tests, and the test results were finally recorded, as shown in Table 2 below.
TABLE 2
| Detecting items | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Acid resistance | Qualified product | Qualified product | Qualified product | Qualified product | Qualified product | Surface tackiness | With small bubbles | Warp of |
| Alkali resistance | Qualified product | Qualified product | Qualified product | Qualified product | Qualified product | Partial dissolution of | Deformation of | Pit |
According to the detection results of the acid resistance and the alkali resistance of the table 2, the nylon 66 material prepared without polytetrafluoroethylene can be found to have serious abnormal phenomena, such as surface adhesion or partial dissolution, and the acid and alkali resistance of the nylon 66 material can be enhanced by adding dissolved oxygen into the auxiliary agent.
Claims (10)
1. The preparation method of the nylon 66 material is characterized by comprising the following steps of:
(1) Placing the modified polypropylene fiber, polytetrafluoroethylene, an auxiliary agent and nylon 66 resin into a high-speed mixer to be uniformly mixed to obtain a mixed material; (2) And (3) mixing the uniformly mixed material obtained in the step (1) and the dispersing agent again, and then placing the mixture into a double-screw extruder for extrusion granulation to obtain the nylon 66 material.
2. The preparation method of the nylon 66 material according to claim 1, wherein the modified polypropylene fiber, polytetrafluoroethylene, auxiliary agent and nylon 66 resin are 40-58 parts by mass of nylon 66 resin, 2-10 parts by mass of polytetrafluoroethylene, 0.1-3 parts by mass of auxiliary agent and 13-25 parts by mass of modified polypropylene fiber.
3. The method for preparing nylon 66 material according to claim 1, wherein the mass of the dispersing agent in the step (2) is 1-3% of the mass of the mixture, and the dispersing agent is sodium pyrophosphate and polyethylene glycol 400.
4. The method for preparing nylon 66 material according to claim 1 or 2, wherein the method for preparing the modified polypropylene fiber is as follows:
preparing sodium metasilicate, urea and deionized water into a mixed solution, putting polypropylene fibers into the mixed solution, then placing the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining for treatment at 100-120 ℃ for 4-7h, taking out the mixed solution after the treatment is finished, cooling to room temperature, and drying for later use.
5. The method for preparing nylon 66 material according to claim 4, wherein the mass ratio of sodium metasilicate to urea is 100:1-6.
6. The method for preparing nylon 66 material according to claim 1, wherein the auxiliary agent comprises isooctyl salicylate, diphenyl azide phosphate, 1, 2-propanediol, mica and calcium stearate.
7. The method for preparing nylon 66 material according to claim 6, wherein the mass ratio of isooctyl salicylate, diphenyl azide phosphate, 1, 2-propanediol, mica and calcium stearate is 100:1-8:15-36:0.1-1:5-10.
8. The method for preparing nylon 66 material according to claim 1, wherein the temperature of the twin-screw extruder is 360-375 ℃, the screw rotation speed is 90-120 r/min, the feeding rotation speed is 10-15 r/min, and the nylon 66 material is obtained by melt extrusion and water-cooling bracing granulation.
9. Nylon 66 material obtainable by the process for the preparation of a nylon 66 material according to claims 1-8.
10. Use of the nylon 66 material obtained by the preparation method according to any one of claims 1 to 8 in the field of chemical equipment.
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