[go: up one dir, main page]
More Web Proxy on the site http://driver.im/

CN109233270A - Utilize the halogen-free flame-retardant nylon 6 material and preparation method thereof of 6 waste silk of polyamide fibre production - Google Patents

Utilize the halogen-free flame-retardant nylon 6 material and preparation method thereof of 6 waste silk of polyamide fibre production Download PDF

Info

Publication number
CN109233270A
CN109233270A CN201811117099.8A CN201811117099A CN109233270A CN 109233270 A CN109233270 A CN 109233270A CN 201811117099 A CN201811117099 A CN 201811117099A CN 109233270 A CN109233270 A CN 109233270A
Authority
CN
China
Prior art keywords
halogen
free flame
nylon
polyamide fibre
waste silk
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811117099.8A
Other languages
Chinese (zh)
Inventor
萧丽芬
郑健
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fujian Jinjiang Technology Co Ltd
Original Assignee
Fujian Jinjiang Technology Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fujian Jinjiang Technology Co Ltd filed Critical Fujian Jinjiang Technology Co Ltd
Priority to CN201811117099.8A priority Critical patent/CN109233270A/en
Publication of CN109233270A publication Critical patent/CN109233270A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/16Nitrogen-containing compounds
    • C08K5/34Heterocyclic compounds having nitrogen in the ring
    • C08K5/3467Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
    • C08K5/3477Six-membered rings
    • C08K5/3492Triazines
    • C08K5/34928Salts
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/10Esters; Ether-esters
    • C08K5/101Esters; Ether-esters of monocarboxylic acids
    • C08K5/103Esters; Ether-esters of monocarboxylic acids with polyalcohols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/13Phenols; Phenolates
    • C08K5/134Phenols containing ester groups
    • C08K5/1345Carboxylic esters of phenolcarboxylic acids
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/49Phosphorus-containing compounds
    • C08K5/51Phosphorus bound to oxygen
    • C08K5/52Phosphorus bound to oxygen only
    • C08K5/521Esters of phosphoric acids, e.g. of H3PO4
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/49Phosphorus-containing compounds
    • C08K5/51Phosphorus bound to oxygen
    • C08K5/52Phosphorus bound to oxygen only
    • C08K5/524Esters of phosphorous acids, e.g. of H3PO3
    • C08K5/526Esters of phosphorous acids, e.g. of H3PO3 with hydroxyaryl compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/22Halogen free composition
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00Properties characterising the ingredient of the composition
    • C08L2207/20Recycled plastic

Landscapes

  • 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)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Abstract

The invention belongs to composite polymer material fields, are related to a kind of halogen-free flame-retardant nylon 6 material and preparation method thereof using the production of 6 waste silk of polyamide fibre.Raw material including following parts by weight is made: 6 80~92.5 parts of nylon, 7~15 parts of halogen-free flame retardants, 0.1~2 part of carbon forming agent, 0.1~2 part of lubricant, 0.3~1 part of antioxidant of recycling;The recycling nylon 6 is 6 waste silk of polyamide fibre particle made of granule machine, relative viscosity 2.47.Graininess is made by granule machine in 6 waste silk of polyamide fibre, granular recycling nylon 6, halogen-free flame retardants, carbon forming agent, lubricant and antioxidant, which are uniformly mixed, to be added to double screw extruder, can obtain halogen-free flame-retardant nylon 6 material after water cooling, air-dried, pelletizing.This method simple process, enables waste material to recycle, low in cost;It is suitable with using the modified obtained halogen-free flame-retardant nylon 6 of virgin material using the properties of waste modified obtained halogen-free flame-retardant nylon 6.

Description

Utilize the halogen-free flame-retardant nylon 6 material and preparation method thereof of 6 waste silk of polyamide fibre production
Technical field
The invention belongs to composite polymer material fields, are related to a kind of halogen-free flame-retardant nylon 6 produced using 6 waste silk of polyamide fibre Material and preparation method thereof.
Background technique
China is only second to terylene to the demand of the civilian silk of polyamide fibre 6, but during the spinning process, often due to broken end, The reasons such as equipment cleaning generate more waste silk, and waste silk amount accounts for about the 2-5% of 6 civilian outputs of polyamide fibre.Some patents point at present It is other that these waste silks have been carried out with different processing, but all without reaching maximum economic benefit with energy consumption as few as possible.Example As 103467378 A of Chinese patent CN by 6 waste silk of polyamide fibre by heating melting, phosphoric acid depolymerization, oxidation, alkalization, filtering, concentration, Rectifying and crystallization obtain monomer caprolactam, and this method process is complicated, energy consumption is huge, economic benefit is lower;Chinese patent CN 6 waste silk of polyamide fibre by crushing, screening, melting extrusion, water cooling, pelletizing and is dried to obtain nylon 6 after the recovery by 104818548 A Slice, can be further used for requiring lower spinning or engineering plastics, and this method is from the discharge port of screw extruder to underwater The outlet of pelletizing is intended to using nitrogen protection, and energy consumption is larger, and economic benefit is general;1065472 A of Chinese patent CN is by polyamide fibre 6 Waste silk and rare-earth cerium compound by dissolution, neutralize, be precipitated, washing, drying, it is dry, be ground up, sieved and be packaged to be performance with The comparable polyamide 6 modification regeneration powder of polyamide 1010 powder is used as spraying raw material, and this method technique is relatively simple, cost Cheap, economic results in society are more significant.
Fire-retardant Nylon 6 due to good wearability, chemical resistance, heat resistance, impact resistance, self-lubrication and Property easy to process, is widely used in electronic electric equipment and household electrical appliance etc..It is applied to the fire retardant master of fire-retardant Nylon 6 at present There are halogenated flame retardant, phosphorus flame retardant, nitrogenated flame retardant, metal compounds flame retardant etc..Wherein, halogenated flame retardant is (with bromine Based on system) high-efficient, additive amount it is few and moderate, usage amount accounts for about the 80% of fire retardant total amount.But halogenated flame retardant A large amount of toxic fumes and corrosive gas can be generated in burning, in addition part bromide fire retardant is the problem of dioxin It is forbidden to use by European Union RoSH instruction.Therefore exploitation flame retarding efficiency is high, and 6 product of nylon of environment friendly halogen-free fireproof just becomes to compel in eyebrow Eyelash.
Summary of the invention
The technical problems to be solved by the present invention are: providing a kind of halogen-free flame-retardant nylon 6 material produced using 6 waste silk of polyamide fibre Material and preparation method thereof, the halogen-free flame-retardant nylon 6 material good physical properties produced reach V-0 grades of flame retardant rating, simultaneously Production cost is reduced again.
In order to solve the above-mentioned technical problem, a kind of the technical solution adopted by the present invention are as follows: nothing produced using 6 waste silk of polyamide fibre Halogen flame-retardant nylon 6 material, the raw material including following parts by weight are made: 6 80~92.5 parts of nylon of recycling, halogen-free flame retardants 7~15 Part, 0.1~2 part of carbon forming agent, 0.1~2 part of lubricant, 0.3~1 part of antioxidant;
The recycling nylon 6 is 6 waste silk of polyamide fibre particle made of granule machine, relative viscosity 2.47.
The present invention also provides a kind of preparation method of above-mentioned halogen-free flame-retardant nylon 6 material using the production of 6 waste silk of polyamide fibre, packets Include following steps:
Granular recycling nylon 6 is made by granule machine in step 1,6 waste silk of polyamide fibre, and the recycling nylon 6 glues relatively Degree is 2.47;
Step 2 weighs 6 80~92.5 parts of the resulting recycling nylon of step 1,7~15 parts of halogen-free flame retardants, carbon forming agent 0.1 Twin-screw extrusion is added in 0.3~1 part of~2 parts, 0.1~2 part of lubricant and antioxidant mixing 10min, mixed material In the main feed hopper of machine;
The temperature of the double screw extruder of step 3, setting procedure 2 is 210~250 DEG C, the spiral shell of the double screw extruder Bar draw ratio is 32~58, and the engine speed of the double screw extruder is 300~500r/min;
Step 4, the material squeezed out by double screw extruder obtain halogen-free flame-retardant nylon 6 by water cooling, air-dried, pelletizing.
The beneficial effects of the present invention are: 6 waste silks of polyamide fibre of the invention after the granulation of granule machine, it is opposite for strict control Viscosity is 2.47, viscosity be 2.47 recycling nylon 6 be conducive to improve product injection molding when mobility, reduce injection time, production Product easy mold release, and product crystalline rate can be improved etc., it is widely used in the fields such as auto industry, electronics, machinery, recycles nylon 6 It is used directly for halogen-free flameproof modification, performance and the use modified nylon 6 of virgin material of halogen-free flameproof modification of nylon 6 obtained Physical property is suitable, tensile strength 63MPa, bending strength 98MPa, bending modulus 5301MPa, notch impact strength 4.9KJ/ m2, reach V-0 grades of flame retardant rating, the requirement with electronic electric equipment and household electrical appliance etc. can be met.The present invention will Waste reclamation is turned waste into wealth, and process is simple, and energy consumption is very low, low in cost, has huge economic results in society.
Specific embodiment
To explain the technical content, the achieved purpose and the effect of the present invention in detail, it is explained below in conjunction with embodiment.
The most critical design of the present invention is: 6 waste silk of polyamide fibre becomes particle, its relative viscosity of strict control by granule machine It is 2.47, so that recycling nylon 6 is used directly for, halogen-free flameproof is modified, and the performance of halogen-free flameproof modification of nylon 6 obtained is excellent It is good, reach V-0 grades of flame retardant rating.
The present invention provides a kind of halogen-free flame-retardant nylon 6 material produced using 6 waste silk of polyamide fibre, the original including following parts by weight Material is made: 6 80~92.5 parts of nylon of recycling, and 7~15 parts of halogen-free flame retardants, 0.1~2 part of carbon forming agent, 0.1~2 part of lubricant, 0.3~1 part of antioxidant;
The recycling nylon 6 is 6 waste silk of polyamide fibre particle made of granule machine, relative viscosity 2.47.
As can be seen from the above description, the beneficial effects of the present invention are: 6 waste silk of polyamide fibre of the invention is granulated by granule machine Afterwards, its relative viscosity of strict control is 2.47, and the recycling nylon 6 that viscosity is 2.47 is conducive to improve flowing when product injection molding Property, reduce injection time, product easy mold release, and product crystalline rate can be improved etc., be widely used in auto industry, electronics, machine The fields such as tool, recycling nylon 6 are used directly for halogen-free flameproof and are modified, the performance and use of halogen-free flameproof modification of nylon 6 obtained The physical property of the modified nylon 6 of virgin material is suitable, tensile strength 63MPa, bending strength 98MPa, bending modulus 5301MPa, notch impact strength 4.9KJ/m2, reach V-0 grades of flame retardant rating, can meet and electronic electric equipment and household The requirement of electric appliance etc..The present invention turns waste into wealth waste reclamation, and process is simple, and energy consumption is very low, low in cost, tool There are huge economic results in society.
The viscosity of the slice of 6 high-speed spinning of polyamide fibre is strict controlled in 2.47, and the viscosity of the waste silk generated is also 2.47, is returning During receiving waste silk, the change of its physical aspect is only carried out by granule machine, becomes graininess from filiform, does not change it Viscosity, therefore the relative viscosity of obtained recycling nylon 6 is still 2.47, which can carry out actual measurement by viscosimeter.
Further, the halogen-free flame retardants is compound in triazine class, and the halogen-free flame retardants is melamine cyanurate Salt, phosphate, guanidine salt or dicyandiamide salt.
Further, the halogen-free flame retardants is melamine cyanurate.
Further, the carbon forming agent is phosphate or phosphate derivative.
Further, the carbon forming agent is pentaerythritol phosphate.
Further, the lubricant is ethylene-acrylic acid copolymer wax, calcium stearate, silicone powder, pentaerythrite stearic acid One or more of ester.
Further, the lubricant is pentaerythritol stearate.
Further, the antioxidant is antioxidant 1010, antioxidant 1098, antioxidant 944, irgasfos 168 and antioxygen One or more of agent 1790.
Further, the antioxidant is antioxidant 1010 (four [β-(3,5- di-tert-butyl-hydroxy phenyl) and antioxygens Agent 168 (three [2,4- di-tert-butyl-phenyl] phosphite esters) is that 1:1 compounding is made according to mass ratio.
The present invention also provides a kind of preparation method of above-mentioned halogen-free flame-retardant nylon 6 material using the production of 6 waste silk of polyamide fibre, packets Include following steps:
Granular recycling nylon 6 is made by granule machine in step 1,6 waste silk of polyamide fibre, and the recycling nylon 6 glues relatively Degree is 2.47;
Step 2 weighs 6 80~92.5 parts of the resulting recycling nylon of step 1,7~15 parts of halogen-free flame retardants, carbon forming agent 0.1 Twin-screw extrusion is added in 0.3~1 part of~2 parts, 0.1~2 part of lubricant and antioxidant mixing 10min, mixed material In the main feed hopper of machine;
The temperature of the double screw extruder of step 3, setting procedure 2 is 210~250 DEG C, the spiral shell of the double screw extruder Bar draw ratio is 32~58, and the engine speed of the double screw extruder is 300~500r/min;
Step 4, the material squeezed out by double screw extruder obtain halogen-free flame-retardant nylon 6 by water cooling, air-dried, pelletizing.
In following embodiment and comparative example composite-material formula, following part is parts by weight, and 6 waste silk of polyamide fibre is Fu Jianjin The preceding spinning of river Science and Technology Ltd. and the mixing of the rear tetra- kinds of waste silks of POY, HOY, FDY, DTY for spinning production (include light, semi-gloss, complete Delustring three classes waste silk), the virgin material bright chip trade mark is JC1005, Fujian Jinjiang Technology Co., Ltd.'s production;Virgin material semi-gloss slice The trade mark is JA2004, Fujian Jinjiang Technology Co., Ltd.'s production;The virgin material full-dull polyester trade mark is ZD3002, Fujian Zhong Jin green wood Expect Co., Ltd's production;Halogen-free flame retardants trade mark HT-231, Jinan Taixing Fine Chemicals Co., ltd's production;Carbon forming agent PEPA, The production of Guangzhou Xi Jia Chemical Co., Ltd.;The lubricant trade mark is PETS-4, the production of Liaocheng Rui Jie Chemical Co., Ltd.;Antioxidant 1010, irgasfos 168, the bright Chemical Co., Ltd.'s production of Nanjing Holley.The present invention produces halogen-free reinforced nylon using 6 waste silk of polyamide fibre 6 materials mould YSTL granule machine and Nanjing Jieya Extruding Equipment Co., Ltd.'s production of Machinery Co., Ltd.'s production using Zhangjiagang hundred million SHJ-63 (draw ratio 40) double screw extruder production.
Embodiment 1
A kind of halogen-free flame-retardant nylon 6 material produced using 6 waste silk of polyamide fibre, the raw material including following parts by weight are made: being returned Receive 6 80 parts of nylon, 7 parts of halogen-free flame retardants, 0.1 part of carbon forming agent, 0.1 part of lubricant, 0.3 part of antioxidant;
The halogen-free flame retardants is melamine cyanurate, and the carbon forming agent is phosphate, and the lubricant is ethylene- Acrylic acid copolymer wax, the antioxidant are antioxidant 1010;
The recycling nylon 6 is 6 waste silk of polyamide fibre particle made of granule machine, relative viscosity 2.47.
The present invention also provides a kind of preparation method of above-mentioned halogen-free flame-retardant nylon 6 material using the production of 6 waste silk of polyamide fibre, packets Include following steps:
Granular recycling nylon 6 is made by granule machine in step 1,6 waste silk of polyamide fibre, and the recycling nylon 6 glues relatively Degree is 2.47;
Step 2 weighs 6 80 parts of the resulting recycling nylon of step 1,7 parts of halogen-free flame retardants, 0.1 part of carbon forming agent, lubricant 0.1 part is added in the main feed hopper of double screw extruder with 0.3 part of mixing 10min of antioxidant, mixed material;
The temperature of the double screw extruder of step 3, setting procedure 2 is 210~250 DEG C, the spiral shell of the double screw extruder Bar draw ratio is 32~58, and the engine speed of the double screw extruder is 300~500r/min;
Step 4, the material squeezed out by double screw extruder obtain halogen-free flame-retardant nylon 6 by water cooling, air-dried, pelletizing.
Embodiment 2
A kind of halogen-free flame-retardant nylon 6 material produced using 6 waste silk of polyamide fibre, the raw material including following parts by weight are made: being returned Receive 6 88 parts of nylon, 10 parts of halogen-free flame retardants, 1 part of carbon forming agent, 0.5 part of lubricant, 0.5 part of antioxidant;
The halogen-free flame retardants is melamine cyanurate, and the carbon forming agent is pentaerythritol phosphate, the lubrication Agent is pentaerythritol stearate, and it with irgasfos 168 is that 1:1 compounds system according to mass ratio that the antioxidant, which is antioxidant 1010, At;
The recycling nylon 6 is 6 waste silk of polyamide fibre particle made of granule machine, relative viscosity 2.47.
The present invention also provides a kind of preparation method of above-mentioned halogen-free flame-retardant nylon 6 material using the production of 6 waste silk of polyamide fibre, packets Include following steps:
Granular recycling nylon 6 is made by granule machine in step 1,6 waste silk of polyamide fibre, and the recycling nylon 6 glues relatively Degree is 2.47;
Step 2 weighs 6 88 parts of the resulting recycling nylon of step 1,10 parts of halogen-free flame retardants, 1 part of carbon forming agent, lubricant 0.5 part is added in the main feed hopper of double screw extruder with 0.5 part of mixing 10min of antioxidant, mixed material;
Each warm area temperature of step 3,2 double screw extruder of setting procedure: 210 DEG C of an area, two 230 DEG C of areas, three 240 DEG C of areas, Four 245 DEG C of areas, five 230 DEG C of areas, six 230 DEG C of areas, seven 245 DEG C of areas, eight 240 DEG C of areas, nine 240 DEG C of areas set double screw extruder Twin-screw draw ratio be 40, set engine speed as 400 turns/min;
Step 4, the material squeezed out by double screw extruder obtain halogen-free flame-retardant nylon 6 by water cooling, air-dried, pelletizing.
Embodiment 3
A kind of halogen-free flame-retardant nylon 6 material produced using 6 waste silk of polyamide fibre, the raw material including following parts by weight are made: being returned Receive 6 92.5 parts of nylon, 15 parts of halogen-free flame retardants, 2 parts of carbon forming agent, 2 parts of lubricant, 1 part of antioxidant;
The halogen-free flame retardants is melamine cyanurate, and the carbon forming agent is pentaerythritol phosphate, the lubrication Agent is pentaerythritol stearate, and it with irgasfos 168 is that 1:1 compounds system according to mass ratio that the antioxidant, which is antioxidant 1010, At;
The recycling nylon 6 is 6 waste silk of polyamide fibre particle made of granule machine, relative viscosity 2.47.
The present invention also provides a kind of preparation method of above-mentioned halogen-free flame-retardant nylon 6 material using the production of 6 waste silk of polyamide fibre, packets Include following steps:
Granular recycling nylon 6 is made by granule machine in step 1,6 waste silk of polyamide fibre, and the recycling nylon 6 glues relatively Degree is 2.47;
Step 2 weighs 6 92.5 parts of the resulting recycling nylon of step 1,15 parts of halogen-free flame retardants, 2 parts of carbon forming agent, lubricant 2 parts are added in the main feed hopper of double screw extruder with 1 part of mixing 10min of antioxidant, mixed material;
Each warm area temperature of step 3,2 double screw extruder of setting procedure: 210 DEG C of an area, two 230 DEG C of areas, three 240 DEG C of areas, Four 245 DEG C of areas, five 230 DEG C of areas, six 230 DEG C of areas, seven 245 DEG C of areas, eight 240 DEG C of areas, nine 240 DEG C of areas set double screw extruder Twin-screw draw ratio be 40, set engine speed as 400 turns/min;
Step 4, the material squeezed out by double screw extruder obtain halogen-free flame-retardant nylon 6 by water cooling, air-dried, pelletizing.
Comparative example 1
88 parts of virgin material there are into light nylon 6 slice, 10 parts of halogen-free flame retardants, 1 part of carbon forming agent, 0.5 part of lubricant 10min is stirred in 0.5 part of antioxidant addition low-speed mixer, said mixture is added to the main feeding of double screw extruder In hopper, processing temperature setting is as follows: 210 DEG C of an area, two 230 DEG C of areas, three 240 DEG C of areas, four 245 DEG C of areas, five 230 DEG C of areas, and six 230 DEG C of area, seven 245 DEG C of areas, eight 240 DEG C of areas, nine 240 DEG C of areas;Engine speed is set as 400 turns/min.
Comparative example 2
By 88 parts of virgin material semi-gloss nylon 6 slice, 10 parts of halogen-free flame retardants, 1 part of carbon forming agent, 0.5 part of lubricant 10min is stirred in 0.5 part of antioxidant addition low-speed mixer, said mixture is added to the main feeding of double screw extruder In hopper, processing temperature setting is as follows: 210 DEG C of an area, two 230 DEG C of areas, three 240 DEG C of areas, four 245 DEG C of areas, five 230 DEG C of areas, and six 230 DEG C of area, seven 245 DEG C of areas, eight 240 DEG C of areas, nine 240 DEG C of areas;Engine speed is set as 400 turns/min.
Comparative example 3
By 88 parts of virgin material full-dull nylon 6 slice, 10 parts of halogen-free flame retardants, 1 part of carbon forming agent, 0.5 part of lubrication Agent and 0.5 part of antioxidant, which are added in low-speed mixer, stirs 10min, and the master that double screw extruder is added in said mixture is fed Expect in hopper, processing temperature setting is as follows: 210 DEG C of an area, two 230 DEG C of areas, three 240 DEG C of areas, four 245 DEG C of areas, five 230 DEG C of areas, Six 230 DEG C of areas, seven 245 DEG C of areas, eight 240 DEG C of areas, nine 240 DEG C of areas;Engine speed is set as 400 turns/min.
Performance test
The pellet that Examples 1 to 3 and comparative example 1~3 prepare is put into convection oven, it is 4 hours dry at 90 DEG C, Then dried pellet is made standard batten in injection (mo(u)lding) machine, 80 DEG C of mold temperature.
Mechanics Performance Testing: tensile property test is carried out by ISO 527, and specimen size is 150 × 10 × 4mm, stretches speed Degree is 10mm/min;Bending property test is carried out by ISO 178, and specimen size is 80 × 10 × 4mm, rate of bending 2mm/ Min, span 64mm;Simply supported beam notch impact strength is carried out by ISO 179, and specimen size is 55 × 6 × 4mm, notch depth For the one third of sample thickness.Flame retardant property test: for vertical combustion according to UL94 standard, sample 3.2mm is thick.
The comprehensive performance of material by test resulting tensile strength, bending strength, bending modulus, notch impact strength with And vertical combustion is evaluated.The performance of embodiment and comparative example is compared as follows table:
It can be seen that from the embodiment 2 and comparative example 1, comparative example 2, the results of property of comparative example 3 of upper table using polyamide fibre 6 The physical properties such as modified obtained tensile strength, bending strength, the notch impact strength of halogen-free flame-retardant nylon 6 of waste silk reclaimed materials are excellent It is good, and reached V-0 grades of flame retardant rating, the requirement with electronic electric equipment and household electrical appliance etc. can be met.And And environmental protection is not only contributed to be modified using 6 waste silk reclaimed materials of polyamide fibre, resource makes full use of, and low in cost, society It can remarkable in economical benefits.
In conclusion the halogen-free flame-retardant nylon 6 material and its preparation side provided by the invention using the production of 6 waste silk of polyamide fibre Method, 6 waste silk of polyamide fibre is after the granulation of granule machine, its relative viscosity of strict control is 2.47, and the recycling nylon 6 that viscosity is 2.47 has Mobility, reduction injection time, product easy mold release when conducive to raising product injection molding, and product crystalline rate can be improved etc., extensively General to be applied to the fields such as auto industry, electronics, machinery, recycling nylon 6 is used directly for halogen-free flameproof and is modified, Halogen obtained The performance of flame-retardant modified nylon 6 is suitable with the physical property of the modified nylon 6 of virgin material, tensile strength 63MPa, and bending is strong Spend 98MPa, bending modulus 5301MPa, notch impact strength 4.9KJ/m2, reach V-0 grades of flame retardant rating, can meet and electricity The requirement of sub- electrical equipment and household electrical appliance etc..The present invention turns waste into wealth waste reclamation, and process is simple, energy consumption It is very low, it is low in cost, there are huge economic results in society.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair Equivalents made by bright description are applied directly or indirectly in relevant technical field, are similarly included in this hair In bright scope of patent protection.

Claims (10)

1. a kind of halogen-free flame-retardant nylon 6 material produced using 6 waste silk of polyamide fibre, which is characterized in that the original including following parts by weight Material is made: 6 80~92.5 parts of nylon of recycling, and 7~15 parts of halogen-free flame retardants, 0.1~2 part of carbon forming agent, 0.1~2 part of lubricant, 0.3~1 part of antioxidant;
The recycling nylon 6 is 6 waste silk of polyamide fibre particle made of granule machine, relative viscosity 2.47.
2. the halogen-free flame-retardant nylon 6 material according to claim 1 produced using 6 waste silk of polyamide fibre, which is characterized in that described Halogen-free flame retardants is compound in triazine class, and the halogen-free flame retardants is melamine cyanurate, phosphate, guanidine salt or dicyandiamide Salt.
3. the halogen-free flame-retardant nylon 6 material according to claim 1 produced using 6 waste silk of polyamide fibre, which is characterized in that described Halogen-free flame retardants is melamine cyanurate.
4. the halogen-free flame-retardant nylon 6 material according to claim 1 produced using 6 waste silk of polyamide fibre, which is characterized in that described Carbon forming agent is phosphate or phosphate derivative.
5. the halogen-free flame-retardant nylon 6 material according to claim 1 produced using 6 waste silk of polyamide fibre, which is characterized in that described Carbon forming agent is pentaerythritol phosphate.
6. the halogen-free flame-retardant nylon 6 material according to claim 1 produced using 6 waste silk of polyamide fibre, which is characterized in that described Lubricant is one or more of ethylene-acrylic acid copolymer wax, calcium stearate, silicone powder, pentaerythritol stearate.
7. the halogen-free flame-retardant nylon 6 material according to claim 1 produced using 6 waste silk of polyamide fibre, which is characterized in that described Lubricant is pentaerythritol stearate.
8. the halogen-free flame-retardant nylon 6 material according to claim 1 produced using 6 waste silk of polyamide fibre, which is characterized in that described Antioxidant is one or more of antioxidant 1010, antioxidant 1098, antioxidant 944, irgasfos 168 and antioxidant 1790.
9. the halogen-free flame-retardant nylon 6 material according to claim 1 produced using 6 waste silk of polyamide fibre, which is characterized in that described It is that 1:1 is compounded and is made that antioxidant, which is antioxidant 1010 with irgasfos 168 according to mass ratio,.
10. a kind of system of the halogen-free flame-retardant nylon 6 material using the production of 6 waste silk of polyamide fibre any according to claim 1~9 Preparation Method, which comprises the following steps:
Granular recycling nylon 6 is made by granule machine in step 1,6 waste silk of polyamide fibre, and the relative viscosity of the recycling nylon 6 is 2.47;
Step 2 weighs 6 80~92.5 parts of the resulting recycling nylon of step 1,7~15 parts of halogen-free flame retardants, carbon forming agent 0.1~2 Double screw extruder is added in 0.3~1 part of part, 0.1~2 part of lubricant and antioxidant mixing 10min, mixed material In main feed hopper;
The temperature of the double screw extruder of step 3, setting procedure 2 is 210~250 DEG C, and the screw rod of the double screw extruder is long Diameter ratio is 32~58, and the engine speed of the double screw extruder is 300~500r/min;
Step 4, the material squeezed out by double screw extruder obtain halogen-free flame-retardant nylon 6 by water cooling, air-dried, pelletizing.
CN201811117099.8A 2018-09-25 2018-09-25 Utilize the halogen-free flame-retardant nylon 6 material and preparation method thereof of 6 waste silk of polyamide fibre production Pending CN109233270A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811117099.8A CN109233270A (en) 2018-09-25 2018-09-25 Utilize the halogen-free flame-retardant nylon 6 material and preparation method thereof of 6 waste silk of polyamide fibre production

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811117099.8A CN109233270A (en) 2018-09-25 2018-09-25 Utilize the halogen-free flame-retardant nylon 6 material and preparation method thereof of 6 waste silk of polyamide fibre production

Publications (1)

Publication Number Publication Date
CN109233270A true CN109233270A (en) 2019-01-18

Family

ID=65056660

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811117099.8A Pending CN109233270A (en) 2018-09-25 2018-09-25 Utilize the halogen-free flame-retardant nylon 6 material and preparation method thereof of 6 waste silk of polyamide fibre production

Country Status (1)

Country Link
CN (1) CN109233270A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111635628A (en) * 2020-05-12 2020-09-08 中广核俊尔(浙江)新材料有限公司 Precipitation-resistant nitrogen-series flame-retardant nylon composite material prepared from waste fishing net wire reclaimed materials
CN112457663A (en) * 2020-10-31 2021-03-09 山东广垠新材料有限公司 Flame-retardant nylon corrugated pipe modified material and preparation method thereof

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1854189A (en) * 2005-04-29 2006-11-01 上海日之升新技术发展有限公司 Thermoplastic non-halogen and fire-retardant reinforced Nylon 6 resin composition
CN102516749A (en) * 2011-12-07 2012-06-27 深圳市科聚新材料有限公司 Polyamide halogen-free flame retardant master batch and preparation method thereof
CN103013104A (en) * 2012-12-26 2013-04-03 上海金发科技发展有限公司 Halogen-free filling flame-retardant nylon 6 composite material and preparation method thereof
CN103509205A (en) * 2013-09-27 2014-01-15 浙江绿宇再生高分子材料有限公司 Recovery process and device for synthetic fiber waste
CN103865256A (en) * 2014-03-11 2014-06-18 广州市聚赛龙工程塑料有限公司 Halogen-free flame retardant nylon 6 with high heat resistance as well as preparation method and application thereof
CN104818548A (en) * 2015-04-24 2015-08-05 长乐力恒锦纶科技有限公司 Recovery process of polyamide 6 spinning waste yarns
CN204550841U (en) * 2015-04-24 2015-08-12 长乐力恒锦纶科技有限公司 A kind of retracting device of polyamide fibre 6 spinning waste silk
WO2016104140A1 (en) * 2014-12-24 2016-06-30 東レ株式会社 Polyamide microparticles

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1854189A (en) * 2005-04-29 2006-11-01 上海日之升新技术发展有限公司 Thermoplastic non-halogen and fire-retardant reinforced Nylon 6 resin composition
CN102516749A (en) * 2011-12-07 2012-06-27 深圳市科聚新材料有限公司 Polyamide halogen-free flame retardant master batch and preparation method thereof
CN103013104A (en) * 2012-12-26 2013-04-03 上海金发科技发展有限公司 Halogen-free filling flame-retardant nylon 6 composite material and preparation method thereof
CN103509205A (en) * 2013-09-27 2014-01-15 浙江绿宇再生高分子材料有限公司 Recovery process and device for synthetic fiber waste
CN103865256A (en) * 2014-03-11 2014-06-18 广州市聚赛龙工程塑料有限公司 Halogen-free flame retardant nylon 6 with high heat resistance as well as preparation method and application thereof
WO2016104140A1 (en) * 2014-12-24 2016-06-30 東レ株式会社 Polyamide microparticles
CN104818548A (en) * 2015-04-24 2015-08-05 长乐力恒锦纶科技有限公司 Recovery process of polyamide 6 spinning waste yarns
CN204550841U (en) * 2015-04-24 2015-08-12 长乐力恒锦纶科技有限公司 A kind of retracting device of polyamide fibre 6 spinning waste silk

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111635628A (en) * 2020-05-12 2020-09-08 中广核俊尔(浙江)新材料有限公司 Precipitation-resistant nitrogen-series flame-retardant nylon composite material prepared from waste fishing net wire reclaimed materials
CN112457663A (en) * 2020-10-31 2021-03-09 山东广垠新材料有限公司 Flame-retardant nylon corrugated pipe modified material and preparation method thereof

Similar Documents

Publication Publication Date Title
CN101875761B (en) Flame-retardant strengthening polythylene terephthalate (PET) material and preparation method thereof
CN110054807B (en) Phosphorus-nitrogen halogen-free flame retardant composition for improving thermal stability by using inorganic metal phosphite and application thereof
CN103627168B (en) A kind of Special halogen-free flame-retardant master batch for nylon and preparation method thereof
CN101280097A (en) Nanometer flame-proof polyethylene glycol terephthalate engineering plastics and preparation thereof
CN112300570B (en) Silicon/phosphorus synergistic flame-retardant polyamide resin
CN106854359A (en) Inexpensive high heat-resistant halogen-free flame-retardant reinforced plastic PA66 composition and preparation method thereof
CN108250566A (en) A kind of low warpage halogen-free expanded flame-retardant Long Glass Fiber Reinforced PP Composite and preparation method thereof
CN104098836A (en) Halogen-free flame-retardant reinforced polypropylene material containing polyamide charring agent and preparation method thereof
CN104231575A (en) Halogen-free and phosphorus-free PBT enhanced composite material and preparation method thereof
CN113754902B (en) Environment-friendly polyamide flame-retardant master batch and preparation method thereof
WO2023020452A1 (en) Halogen-free flame-retardant polypropylene composition, and preparation method therefor and use thereof
CN109233270A (en) Utilize the halogen-free flame-retardant nylon 6 material and preparation method thereof of 6 waste silk of polyamide fibre production
CN101798447A (en) PBT (Polybutylece Terephthalate) special halogen and phosphorus free inflaming retarding plasticizing mother particle and preparation method thereof
CN104262891A (en) Flame-retardant regenerated ABS particle and preparation method thereof
CN106751336A (en) A kind of bromine system flame-retarding HIPS material of high CTI value and preparation method thereof
CN112852149A (en) Flame-retardant antistatic glass fiber reinforced nylon 6 composite material and preparation method thereof
CN107216650A (en) A kind of long glass fiber reinforced halogen-free reinforced nylon compound and preparation method thereof
CN107686637B (en) Preparation method of high-pressure-resistant and high-temperature-resistant composite material
CN102816405A (en) Low-smoke halogen-free flame-retardant thermoplastic elastomer and preparation method thereof
CN107266786B (en) Polypropylene halogen-free flame-retardant master batch and preparation method thereof
CN111621150B (en) Flame-retardant nylon composition and preparation method thereof
CN109233271A (en) Utilize the short glass fiber reinforced nylon 6 material and preparation method thereof of 6 waste silk of polyamide fibre production
CN106633388A (en) Red phosphorus flame-retardant reinforced polypropylene material and preparation method thereof
CN108250573B (en) Thermo-oxidative aging resistant halogen-free environment-friendly flame-retardant polypropylene material and preparation method thereof
CN109705566B (en) Flame-retardant nylon 6 composition and expanded beads thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
CB02 Change of applicant information
CB02 Change of applicant information

Address after: 350209 Airport Industrial Zone, Changle District, Fuzhou City, Fujian Province (Mashan District, Hunan town)

Applicant after: Fujian Yongrong Jinjiang Co., Ltd

Address before: 350209 Pengcheng Road, Changle Airport Industrial Zone, Fuzhou, Fujian 28

Applicant before: FUJIAN JINJIANG TECHNOLOGY Co.,Ltd.

RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20190118