CN104804422A - Flame retardant nylon composite with high stability and preparation method of flame retardant nylon composite - Google Patents

Flame retardant nylon composite with high stability and preparation method of flame retardant nylon composite Download PDF

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Publication number
CN104804422A
CN104804422A CN201510191487.0A CN201510191487A CN104804422A CN 104804422 A CN104804422 A CN 104804422A CN 201510191487 A CN201510191487 A CN 201510191487A CN 104804422 A CN104804422 A CN 104804422A
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China
Prior art keywords
nylon
parts
flame retardant
added
improved
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CN201510191487.0A
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Chinese (zh)
Inventor
朱正娟
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Hefei Kangling Curing Technology Co Ltd
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Hefei Kangling Curing Technology Co Ltd
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Priority to CN201510191487.0A priority Critical patent/CN104804422A/en
Publication of CN104804422A publication Critical patent/CN104804422A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/02Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • 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
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/08Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers

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  • 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)

Abstract

The invention discloses a flame retardant nylon composite with high stability. The flame retardant nylon composite is characterized by being prepared from the following raw materials in parts by weight: 8-13 parts of antimonous oxide, 0.4-0.6 part of propylgallate, 0.5-1 part of phosphite ester triphenyl, 4-7 parts of expansive mica, 0.5-1 part of magnesium stearate, 90-100 pars of nylon 6, 2.5-3.2 parts of lithium chloride, 3-9 parts of epoxy resin E51, 10-15 parts of an EVA emulsion, 60-80 parts of ethyl acetate, 1-3 parts of castor oil, 4-7 parts of ethylene/ethanol copolymer powder and 15-30 parts of distilled water. The ethylene/ethanol copolymer covers the surface of a reinforcement body in an active manner, the compatibility between the reinforcement body and the nylon 6 is improved, and the self mechanical property of the nylon 6 is not reduced; by the addition of the antimony trioxide, the usage amount of the fire retardant is reduced, and the flame retardant level of the material is improved; by addition of the expansive mica, the strength and the flame retarding effect of the produce can be improved, the flowability of material processing can be improved, and damage to an instrument is reduced.

Description

Fire-retardant nylon matrix material of a kind of good stability and preparation method thereof
Technical field
Fire-retardant nylon matrix material that the present invention relates to a kind of good stability and preparation method thereof, belongs to nylon production technical field.
Background technology
Nylon 6 is a kind of widely used engineering plastics, there is excellent over-all properties, but also exist that strong alkali-acid resistance is poor, dry state and the shortcoming such as low temperature impact strength is low, water-intake rate is large, and the processing temperature of nylon 6 is higher, improve production cost, high to the requirement of production unit, be unfavorable for scale operation.The low melting point nylon 6 sold in the market is mainly prepared by the method for synthesis by external company, there is complete processing complexity in the method, the shortcomings such as cost is higher, and the domestic research to low melting point is also in laboratory stage, be difficult to realize industrialization scale operation, therefore the nylon 6 obtaining low melting point by modification is emphasis of current research, it has many premium propertiess, but also there is shock strength difference, the shortcomings such as resistance toheat difference, therefore also need by filling on the basis of low melting point nylon 6 matrix, strengthen, copolymerization, the method modification low melting point nylon 6 such as blended, increase the popularity of application.
Along with nylon 6 is widely used in tricot, tire cord, filter cloth, rope, fishnet, trolley part and wrapping material etc., but nylon 6 belongs to meltbility combustible fibre, limiting oxygen index(LOI) is about 21, along with the widespread use of fabric, the potentially dangerous of its fire also becomes increasingly conspicuous, in addition nylon 6 fabric burning easily forms melting, and molten drop easily brings the secondary injury comprising and scald and wait, and therefore becomes focus to the research of flame retardant type nylon 6.
Summary of the invention
Fire-retardant nylon matrix material that the object of this invention is to provide a kind of good stability and preparation method thereof, the epoxy resin of interpolation solves the problem that the low and vicat softening temperature of low melting point nylon 6 subsurface defect, mechanical property reduces.
In order to realize object of the present invention, the present invention is by following scheme implementation:
A fire-retardant nylon matrix material for good stability, is made up of the raw material of following weight part: antimonous oxide 8-13, Tenox PG 0.4-0.6, phosphorous acid ester triphenylmethyl methacrylate 0.5-1, expansion mica 4-7, Magnesium Stearate 0.5-1, nylon 69 0-100, lithium chloride 2.5-3.2, epoxy resin E513-9, EVA emulsion 10-15, ethyl acetate 60-80, Viscotrol C 1-3, ethylene/vinyl alcohol copolymer powder 4-7, distilled water 15-30;
The fire-retardant nylon matrix material of a kind of good stability of the present invention, be made up of following concrete steps:
(1) mixing of ethyl acetate, distilled water and EVA emulsion is added in ultrasonic wave, ultrasonic disperse is even, add antimonous oxide and expansion mica again in 80-90W ultrasonic disperse 10-15 minute, after end, mixture is heated to 70-90 ° of C and keeps 2-3 hour, stirring and refluxing in the process, then stops heating by product filtration, washing, dry for standby;
(2) mix after Viscotrol C thermal dehydration with ethylene/vinyl alcohol copolymer powder, under 180-200 ° of C, activation treatment 10-15 minute is carried out to the product of step (1), be cooled to room temperature after terminating for subsequent use;
(3) by Lithium chloride (anhydrous) and nylon 6 dry 7-8 hour under 120 ° of C and 80 ° C respectively, dried Lithium chloride (anhydrous), nylon 6 and epoxy resin E51 are mixed, be added to extruding pelletization in twin screw extruder again, heating and temperature control, at 180-240 ° of C, obtains modification of nylon 6 particle;
(4) particle of step (3), Magnesium Stearate and Tenox PG are added to the mixed 3-10 minute of heat in high-speed mixer, heating and temperature control, at 70-80 ° of C, obtains hot batch mixing;
(5) particle of step (4) is added in cold mixer, add material and all the other surplus materialss that step (1) obtains when temperature is reduced to room temperature, after being uniformly mixed 5-10 minute, transfer to that Heating temperature is 220-250 ° of C, screw speed is carry out melting mixing granulation in the twin screw extruder of 180-300 rev/min.
Advantage of the present invention is: the present invention adopts ethylene/vinyl alcohol copolymer to activate and is coated on reinforcement surface, add the consistency between reinforcement and nylon 6, avoid the reduction of the mechanical property of nylon 6 own, the ANTIMONY TRIOXIDE SB 203 99.8 PCT of adding can reduce the usage quantity of fire retardant, the flame retardant rating of strongthener, the expansion mica added can improve intensity and the flame retardant effect of goods, and mobility when can improve materials processing, reduce the infringement to instrument.
specific embodiments
Below by specific examples, the present invention is described in detail.
A fire-retardant nylon matrix material for good stability, is made up of the raw material of following weight part (kilogram): antimonous oxide 11, Tenox PG 0.4, phosphorous acid ester triphenylmethyl methacrylate 0.7, expansion mica 5, Magnesium Stearate 0.6, nylon 69 7, lithium chloride 3, epoxy resin E516, EVA emulsion 15, ethyl acetate 80, Viscotrol C 2, ethylene/vinyl alcohol copolymer powder 6, distilled water 30;
The fire-retardant nylon matrix material of a kind of good stability of the present invention, be made up of following concrete steps:
(1) mixing of ethyl acetate, distilled water and EVA emulsion is added in ultrasonic wave, ultrasonic disperse is even, add antimonous oxide and expansion mica again in 90W ultrasonic disperse 10 minutes, after end, mixture is heated to 90 ° of C and keeps 3 hours, stirring and refluxing in the process, then stops heating by product filtration, washing, dry for standby;
(2) mix after Viscotrol C thermal dehydration with ethylene/vinyl alcohol copolymer powder, under 190 ° of C, activation treatment is carried out 10 minutes to the product of step (1), be cooled to room temperature after terminating for subsequent use;
(3) by Lithium chloride (anhydrous) and nylon 6 under 120 ° of C and 80 ° C dry 8 hours respectively, dried Lithium chloride (anhydrous), nylon 6 and epoxy resin E51 are mixed, be added to extruding pelletization in twin screw extruder again, heating and temperature control, at 220 ° of C, obtains modification of nylon 6 particle;
(4) particle of step (3), Magnesium Stearate and Tenox PG are added to heat in high-speed mixer to mix 8 minutes, heating and temperature control, at 80 ° of C, obtains hot batch mixing;
(5) particle of step (4) is added in cold mixer, add material and all the other surplus materialss that step (1) obtains when temperature is reduced to room temperature, after being uniformly mixed 8 minutes, transfer to that Heating temperature is 240 ° of C, screw speed is carry out melting mixing granulation in the twin screw extruder of 250 revs/min.
In the present embodiment, the performance perameter of nylon composite materials is as follows:
Tensile strength (MPa): 84.9;
Flexural strength (MPa): 106.2;
Notched Izod impact strength (kJ/m2): 82.5;
Vicat softening temperature (° C): 73;
Flame retardant rating: V0 level.

Claims (1)

1. the fire-retardant nylon matrix material of a good stability, it is characterized in that, be made up of the raw material of following weight part: antimonous oxide 8-13, Tenox PG 0.4-0.6, phosphorous acid ester triphenylmethyl methacrylate 0.5-1, expansion mica 4-7, Magnesium Stearate 0.5-1, nylon 69 0-100, lithium chloride 2.5-3.2, epoxy resin E513-9, EVA emulsion 10-15, ethyl acetate 60-80, Viscotrol C 1-3, ethylene/vinyl alcohol copolymer powder 4-7, distilled water 15-30;
According to claim 1, a fire-retardant nylon matrix material for good stability, is characterized in that, is made up of following concrete steps:
(1) mixing of ethyl acetate, distilled water and EVA emulsion is added in ultrasonic wave, ultrasonic disperse is even, add antimonous oxide and expansion mica again in 80-90W ultrasonic disperse 10-15 minute, after end, mixture is heated to 70-90 ° of C and keeps 2-3 hour, stirring and refluxing in the process, then stops heating by product filtration, washing, dry for standby;
(2) mix after Viscotrol C thermal dehydration with ethylene/vinyl alcohol copolymer powder, under 180-200 ° of C, activation treatment 10-15 minute is carried out to the product of step (1), be cooled to room temperature after terminating for subsequent use;
(3) by Lithium chloride (anhydrous) and nylon 6 dry 7-8 hour under 120 ° of C and 80 ° C respectively, dried Lithium chloride (anhydrous), nylon 6 and epoxy resin E51 are mixed, be added to extruding pelletization in twin screw extruder again, heating and temperature control, at 180-240 ° of C, obtains modification of nylon 6 particle;
(4) particle of step (3), Magnesium Stearate and Tenox PG are added to the mixed 3-10 minute of heat in high-speed mixer, heating and temperature control, at 70-80 ° of C, obtains hot batch mixing;
(5) particle of step (4) is added in cold mixer, add material and all the other surplus materialss that step (1) obtains when temperature is reduced to room temperature, after being uniformly mixed 5-10 minute, transfer to that Heating temperature is 220-250 ° of C, screw speed is carry out melting mixing granulation in the twin screw extruder of 180-300 rev/min.
CN201510191487.0A 2015-04-22 2015-04-22 Flame retardant nylon composite with high stability and preparation method of flame retardant nylon composite Pending CN104804422A (en)

Priority Applications (1)

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CN201510191487.0A CN104804422A (en) 2015-04-22 2015-04-22 Flame retardant nylon composite with high stability and preparation method of flame retardant nylon composite

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CN201510191487.0A CN104804422A (en) 2015-04-22 2015-04-22 Flame retardant nylon composite with high stability and preparation method of flame retardant nylon composite

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CN104804422A true CN104804422A (en) 2015-07-29

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102408705A (en) * 2011-09-22 2012-04-11 贵州凯科特材料有限公司 Nylon 6 with high performance and low melting-point and preparation method thereof
CN103589147A (en) * 2013-10-29 2014-02-19 安徽安缆模具有限公司 Impact-resistance nylon PA12 material for automobile connectors
CN103849142A (en) * 2012-11-30 2014-06-11 合肥杰事杰新材料股份有限公司 Lightweight flame retardant modified polyamide material and its preparation method
CN104004347A (en) * 2014-05-28 2014-08-27 广东银禧科技股份有限公司 PA6 (polyamide 6) composite material and preparation method thereof
CN104046004A (en) * 2014-05-19 2014-09-17 安徽安缆模具有限公司 Chemical-attack-resistant nylon composite for automobile water chamber and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102408705A (en) * 2011-09-22 2012-04-11 贵州凯科特材料有限公司 Nylon 6 with high performance and low melting-point and preparation method thereof
CN103849142A (en) * 2012-11-30 2014-06-11 合肥杰事杰新材料股份有限公司 Lightweight flame retardant modified polyamide material and its preparation method
CN103589147A (en) * 2013-10-29 2014-02-19 安徽安缆模具有限公司 Impact-resistance nylon PA12 material for automobile connectors
CN104046004A (en) * 2014-05-19 2014-09-17 安徽安缆模具有限公司 Chemical-attack-resistant nylon composite for automobile water chamber and preparation method thereof
CN104004347A (en) * 2014-05-28 2014-08-27 广东银禧科技股份有限公司 PA6 (polyamide 6) composite material and preparation method thereof

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Application publication date: 20150729

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