CN106046608A - Environment-friendly flame-retardant cable material and preparation method thereof - Google Patents
Environment-friendly flame-retardant cable material and preparation method thereof Download PDFInfo
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- CN106046608A CN106046608A CN201610521795.XA CN201610521795A CN106046608A CN 106046608 A CN106046608 A CN 106046608A CN 201610521795 A CN201610521795 A CN 201610521795A CN 106046608 A CN106046608 A CN 106046608A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses an evironment-friendly flame-retardant cable material which is composed of, by weight, 3-5 parts of ethylhexyl methacrylate, 0.7-1 part of zinc acetylacetone, 6-7 parts of guanidine sulfamate, 0.3-0.4 part of N, N'-dicyclohexyl carbimide, 4-5 parts of hexachlorocyclotriphosphazene, 0.2-0.4 part of sodium hydroxide, 1-2 parts of thiourea, 0.7-1 part of lauryl dimethyl amine oxide, 17-20 parts of nylon, 120-130 parts of polyvinyl chloride, 1-2 parts of barium stearate, 2-3 parts of beewax, 0.6-1 part of anhydrous calcium chloride, 20-30 parts of carbon nanotube and 0.6-1 part of 1, 2-dimethyleimidazole. The cable material is high in safety and environment friendliness and free of toxic and harmful volatile matters.
Description
Technical field
The present invention relates to CABLE MATERIALS technical field, particularly relate to a kind of Environment-friendlyflame-retardant flame-retardant cable material and preparation method thereof.
Background technology
Nanotechnology is in the eighties rise in last century, and is widely used in multiple fields.Research finds,
Polymer adds after nanoparticle, can the performance of significantly lift-off material.Such as when add in polymer a small amount of graphite skilful,
During the nanoparticle such as CNT, molybdenum bisuphide, the mechanical strength of material will be obviously improved IWI.Research finds, only adds pole
A small amount of nano material just can be greatly reduced the HRR of material combustion, the most also can the mechanics of lift-off composite strong
Degree.The nano flame retardant system that research is relatively more at present mainly has several: (1) inorganic nano-particle, such as nanometer ammoxidation town, nanometer
Ammoxidation lead and nano silicon etc..This based flame retardant is relatively low due to himself flame retarding efficiency, fire retardant mechanism also with other
Nanoparticle is different, needs bigger addition when reality is applied, therefore can not be classified as flame retardant nano-materials completely.And fill out
The filling of material also can produce impact to the mechanical property of material self.(2) laminated inorganic matter, as nanoclay, brucite, can
Expanded graphite etc..(3) pipe carbon and acicular nanoparticles, such as CNT, halloysite nanotubes and meerschaum etc..In 21 century
In the tenth day of lunar month year, a large amount of report galapectite in recent years and meerschaum about polymer/carbon nano-tube flame-retardant system is had to be increasingly becoming
The focus nano flame retardant technology of research occurs two during the last ten years, although gradually grows up and achieves a series of achievement in research,
But the polymeric material of nanorize combustion to extensively application, still has very long road to walk from research；
About the application in the polymer of nano flame retardant technology, some problem following is currently mainly had to need to solve: 1. nanometer resistance
Combustion additive significant advantage is that in trying for taper calorimetric, HRR reduces for a lot nanoparticles, only
Need to add few amount and just the HRR of material combustion can be greatly reduced by W.But for traditional fire-retardant trial work section,
As oxygen index (OI) and vertical combustion test effect significantly, negative effect the most also can be played.Therefore, need to consider nanoparticle
Son is modified or reaches the effect of cooperative flame retardant by compounding use with conventional flame retardant.The most in recent years, to nanoparticle
Modified research gets more and more, the particularly intercalation modifying to nanoclay.But the intercalation of existing frequently-used nanoclay changes
Property agent be the burning base amine salt of long-chain mostly, lack and be specifically designed to flame-retardant modified intercalator or surface modifier.And it is most of
Modifying agent itself not there is anti-flammability, some self the most flammable；Heat stability is the most poor, and temperature of initial decomposition is low, difficult suitable
Iron for engineering plastics etc. and melt the polymer that temperature is higher.Therefore, change for having the nanoparticle of anti-flammability and heat stability concurrently
Property agent is a direction of future studies.3. with the fire retardant such as halogen flame, phosphor nitrogen combustion inhibitor, there is clear and definite fire retardant mechanism
Difference, the present stage explanation to the mechanism shortage system of nano flame retardant.Current approved mechanism mainly has oneself of nanoclay
The obstruct mechanism of mechanism, solid phase is caught by base；Synergistic catalytic mechanism with expanding fire retardant；The network structure of CNT intercepts
Impact etc. on system rheological characteristic in mechanism and combustion process.Therefore, for nanoparticle resistance during polymer combustion
The elaboration of combustion engine reason will be the direction of future studies, and CNT lacks polar functional group, with polymer base due to surface simultaneously
The compatibility of body is poor；The structure of high length-diameter ratio can cause the winding in the course of processing, gathering, thus is difficult to well divide
Dissipate.Additionally, CNT only to reduce HRR have obvious effect, but can not effectively carry material oxygen index (OI) and
Vertical combustion grade.In order to improve the CNT compatibility in the polymer and dispersibility, coupling agent, surface activity can be used
Agent or polymer etc. carry out surface to CNT and change, but class method of modifying often difficulty puies forward its fire resistance, and some is very
To destroying original anti-flammability；.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that a kind of Environment-friendlyflame-retardant flame-retardant cable material and preparation side thereof
Method.
The present invention is achieved by the following technical solutions:
A kind of Environment-friendlyflame-retardant flame-retardant cable material, it is made up of the raw material of following weight parts:
2-Propenoic acid, 2-methyl-, isooctyl ester 3-5, zinc acetylacetonate 0.7-1, Guanidine Sulfamate 99 6-7, N, N'-Dicyclohexylcarbodiimide
0.3-0.4, hexachlorocyclotriph,sphazene 4-5, sodium hydroxide 0.2-0.4, thiourea 1-2, lauryl dimethyl amine oxide 0.7-1, nylon
17-20, polrvinyl chloride 120-130, barium stearate 1-2, Cera Flava 2-3, anhydrous calcium chloride 0.6-1, CNT 20-23,1,2-
Methylimidazole 0.6-1.
A kind of preparation method of described Environment-friendlyflame-retardant flame-retardant cable material, it is made up of the raw material of following weight parts:
(1) being joined by above-mentioned CNT in the mixed acid solution of its weight 80-100 times, described nitration mixture is to be by mass ratio
The hydrochloric acid solution composition of the sulphuric acid of the 96-98% of 3-4:1 and 87-90%, at 50-60 DEG C ultrasonic 17-20 minute, filters, will be heavy
Form sediment and wash 2-3 time, be vacuum dried 30-40 minute at 70-76 DEG C, obtain acidifying CNT；
(2) being joined by above-mentioned zinc acetylacetonate in the DMF of its weight 27-30 times, liter high-temperature is 50-
60 DEG C, add above-mentioned barium stearate, the 30-40% of above-mentioned acidifying carbon nanotubes, insulated and stirred 17-20 minute, obtain amide pre-
Mixed liquid；
(3) by above-mentioned Guanidine Sulfamate 99, N, N'-Dicyclohexylcarbodiimide mixes, and joins the N of compound weight 70-80 times,
In dinethylformamide, mix with above-mentioned amide premixed liquid, ultrasonic 100-120 minute, send in reactor, be passed through nitrogen,
Rise high-temperature and be 120-127 DEG C, insulation reaction 35-40 hour, discharging, by product sucking filtration, with washing with acetone 3-4 time, it is placed in 70-
The baking oven of 80 DEG C is dried to constant weight, obtains sulfonic acid guanidine grafting carbon nanotube；
(4) by remaining acidifying CNT, hexachlorocyclotriph,sphazene, sodium hydroxide mixing, compound weight 60-70 times is joined
Oxolane in, ultrasonic 100-110 minute, send in reactor, be passed through nitrogen, rise high-temperature and be 68-70 DEG C, insulation reaction
35-40 hour, discharging, by product sucking filtration, with washing with acetone 3-4 time, it is placed in the baking oven of 70-80 DEG C and is dried to constant weight, obtain ring
Three phosphonitrile grafting carbon nanotubes；
(5) take the 10-16% of above-mentioned nylon weight, add in its weight 20-27 times, 17-20% formalin, stirring mixing
20-30 minute, dropping concentration was the hydrochloric acid of 3-6mol/l, and regulation pH is 2-3, is passed through nitrogen, is heated to boiling, keeps boiling
57-60 minute, discharging, it is cooled to room temperature, obtains hydroxylating nylon liquid；
(6) by above-mentioned 1,2-methylimidazole joins in the dehydrated alcohol of its weight 6-8 times, rises high-temperature and is 80-86 DEG C, adds
Entering Cera Flava, insulated and stirred 10-15 minute, add lauryl dimethyl amine oxide, stirring, to room temperature, obtains alcohol emulsion；
(7) by above-mentioned sulfonic acid guanidine grafting carbon nanotube, ring three phosphonitrile grafting carbon nanotube, the mixing of hydroxylating nylon liquid, at 87-90
Preheat 4-6 minute at DEG C, rise high-temperature and be 155-160 DEG C, insulated and stirred 3-4 minute, add above-mentioned alcohol emulsion, 100-200 turns/
Divide stirring 3-4 minute, filter, precipitation oxolane is washed 2-3 time, is vacuum dried 30-40 minute at being placed in 70-80 DEG C,
Obtain modified nylon CNT；
(8) above-mentioned modified nylon CNT is mixed with remaining each raw material, stir, dry, put into screw extruder and melt
Melt extrusion, cool down, sieve, obtain described CABLE MATERIALS.
The invention have the advantage that the CABLE MATERIALS of the present invention has good fire-retardant fireproof performance, the present invention first uses amino sulphur
The pre-nylon blending of CNT that acid guanidine, chlorine ring three phosphonitrile are grafted respectively, the nylon after hydroxylating discharging can be with grafting
After CNT have the good compatibility, improve this composite dispersibility in finished cable material the most further, this is multiple
The fire retardant mechanism of condensation material is: when nylon in combustion, CNT is at polymer melt surface aggregation, and is formed netted
The layer of charcoal of structure, these netted carbon-coatings are fine and close and almost without hole, are effectively prevented outside heat and oxygen when burning
Entering, such that it is able to effectively reduce HRR and mass loss rate, and the Guanidine Sulfamate 99 being grafted can be coated on
Carbon nano tube surface, its catabolite contributes to CNT and forms the finest and close network structure layer of charcoal, and Guanidine Sulfamate 99 is certainly
Status solution can produce ammonia, and ammonia can react again the degraded promoting nylon with nylon, and both jointly produce substantial amounts of ammonia gas and water and steam
The non-flammable compressive gas such as gas and carbon dioxide, the oxygen in dilute combustion district and fuel gas, play the effect that gas phase is fire-retardant；Grafting
Chlorine ring three phosphonitrile plays the effect of similar patch, and the mesh of the netted layer of charcoal that filling carbon nano-pipe is formed, chlorine the most therein is former
Sub-combustion process can be formed Cl-, and catch the free radical that burning produces, thus terminate the chain reaction of combustion process, carry
The fire resistance of high finished-product material.The CABLE MATERIALS Safety and Environmental Protection of the present invention is good, without poisonous noxious volatile material.
Detailed description of the invention
A kind of Environment-friendlyflame-retardant flame-retardant cable material, it is made up of the raw material of following weight parts:
2-Propenoic acid, 2-methyl-, isooctyl ester 3, zinc acetylacetonate 0.7, Guanidine Sulfamate 99 6, N, N' Dicyclohexylcarbodiimide 0.3, chlordene
Ring three phosphonitrile 4, sodium hydroxide 0.2, thiourea 1, lauryl dimethyl amine oxide 0.7, nylon 17, polrvinyl chloride 120, barium stearate
1, Cera Flava 2, anhydrous calcium chloride 0.6, CNT 20,1,2 methylimidazole 0.6.
A kind of preparation method of described Environment-friendlyflame-retardant flame-retardant cable material, it is made up of the raw material of following weight parts:
(1) being joined by above-mentioned CNT in the mixed acid solution of its weight 80 times, described nitration mixture is 3:1 by mass ratio
The sulphuric acid of 96% and the hydrochloric acid solution composition of 87%, at 50 DEG C ultrasonic 17 minutes, filter, by precipitation washing 2 times, vacuum at 70 DEG C
It is dried 30 minutes, obtains acidifying CNT；
(2) being joined by above-mentioned zinc acetylacetonate in the DMF of its weight 27 times, rising high-temperature is 50 DEG C, adds
Enter above-mentioned barium stearate, the 30% of above-mentioned acidifying carbon nanotubes, insulated and stirred 17 minutes, obtain amide premixed liquid；
(3) by above-mentioned Guanidine Sulfamate 99, N, N' Dicyclohexylcarbodiimide mixes, and joins the N, N bis-of compound weight 70 times
In methylformamide, mix with above-mentioned amide premixed liquid, ultrasonic 100 minutes, send in reactor, be passed through nitrogen, rise high-temperature
It is 120 DEG C, insulation reaction 35 hours, discharging, by product sucking filtration, with washing with acetone 3 times, it is placed in the baking oven of 70 DEG C and is dried to perseverance
Weight, obtains sulfonic acid guanidine grafting carbon nanotube；
(4) by remaining acidifying CNT, hexachlorocyclotriph,sphazene, sodium hydroxide mixing, compound weight 60 times is joined
In oxolane, ultrasonic 100 minutes, sending in reactor, be passed through nitrogen, rising high-temperature is 68 DEG C, and insulation reaction 35 hours goes out
Material, by product sucking filtration, with washing with acetone 3 times, is placed in the baking oven of 70 DEG C and is dried to constant weight, obtain ring three phosphonitrile grafting carbon nanometer
Pipe；
(5) take the 10% of above-mentioned nylon weight, add in its weight 20 times, the formalin of 17%, stirring mixing 20 minutes, drip
Adding the hydrochloric acid that concentration is 3mol/l, regulation pH is 2, is passed through nitrogen, is heated to boiling, keeps boiling 57 minutes, discharging, is cooled to
Room temperature, obtains hydroxylating nylon liquid；
(6) being joined by above-mentioned 1,2 methylimidazoles in the dehydrated alcohol of its weight 6 times, rising high-temperature is 80 DEG C, adds honeybee
Wax, insulated and stirred 10 minutes, add lauryl dimethyl amine oxide, stirring, to room temperature, obtains alcohol emulsion；
(7) by above-mentioned sulfonic acid guanidine grafting carbon nanotube, ring three phosphonitrile grafting carbon nanotube, the mixing of hydroxylating nylon liquid, at 87 DEG C
Lower preheating 4 minutes, rising high-temperature is 155 DEG C, insulated and stirred 3 minutes, adds above-mentioned alcohol emulsion, and 100 revs/min are stirred 3 minutes, mistake
Filter, washs precipitation oxolane 2 times, is placed at 70 DEG C vacuum drying 30 minutes, obtains modified nylon CNT；
(8) above-mentioned modified nylon CNT is mixed with remaining each raw material, stir, dry, put into screw extruder and melt
Melt extrusion, cool down, sieve, obtain described CABLE MATERIALS.
Performance test:
Hot strength: 19.8 MPa；
Low temperature brittleness impact temperature (DEG C) :-30 DEG C are passed through；
Fire-retardant rank: V-0；
After 100 DEG C × 240h hot air aging: hot strength rate of change (%)-7.5；
Extension at break rate of change (%)-8.1.
Claims (2)
1. an Environment-friendlyflame-retardant flame-retardant cable material, it is characterised in that it is made up of the raw material of following weight parts:
2-Propenoic acid, 2-methyl-, isooctyl ester 3-5, zinc acetylacetonate 0.7-1, Guanidine Sulfamate 99 6-7, N, N'-Dicyclohexylcarbodiimide
0.3-0.4, hexachlorocyclotriph,sphazene 4-5, sodium hydroxide 0.2-0.4, thiourea 1-2, lauryl dimethyl amine oxide 0.7-1, nylon
17-20, polrvinyl chloride 120-130, barium stearate 1-2, Cera Flava 2-3, anhydrous calcium chloride 0.6-1, CNT 20-23,1,2-
Methylimidazole 0.6-1.
2. the preparation method of an Environment-friendlyflame-retardant flame-retardant cable material as claimed in claim 1, it is characterised in that it is by following weight
The raw material composition of part:
(1) being joined by above-mentioned CNT in the mixed acid solution of its weight 80-100 times, described nitration mixture is to be by mass ratio
The hydrochloric acid solution composition of the sulphuric acid of the 96-98% of 3-4:1 and 87-90%, at 50-60 DEG C ultrasonic 17-20 minute, filters, will be heavy
Form sediment and wash 2-3 time, be vacuum dried 30-40 minute at 70-76 DEG C, obtain acidifying CNT；
(2) being joined by above-mentioned zinc acetylacetonate in the DMF of its weight 27-30 times, liter high-temperature is 50-
60 DEG C, add above-mentioned barium stearate, the 30-40% of above-mentioned acidifying carbon nanotubes, insulated and stirred 17-20 minute, obtain amide pre-
Mixed liquid；
(3) by above-mentioned Guanidine Sulfamate 99, N, N'-Dicyclohexylcarbodiimide mixes, and joins the N of compound weight 70-80 times,
In dinethylformamide, mix with above-mentioned amide premixed liquid, ultrasonic 100-120 minute, send in reactor, be passed through nitrogen,
Rise high-temperature and be 120-127 DEG C, insulation reaction 35-40 hour, discharging, by product sucking filtration, with washing with acetone 3-4 time, it is placed in 70-
The baking oven of 80 DEG C is dried to constant weight, obtains sulfonic acid guanidine grafting carbon nanotube；
(4) by remaining acidifying CNT, hexachlorocyclotriph,sphazene, sodium hydroxide mixing, compound weight 60-70 times is joined
Oxolane in, ultrasonic 100-110 minute, send in reactor, be passed through nitrogen, rise high-temperature and be 68-70 DEG C, insulation reaction
35-40 hour, discharging, by product sucking filtration, with washing with acetone 3-4 time, it is placed in the baking oven of 70-80 DEG C and is dried to constant weight, obtain ring
Three phosphonitrile grafting carbon nanotubes；
(5) take the 10-16% of above-mentioned nylon weight, add in its weight 20-27 times, 17-20% formalin, stirring mixing
20-30 minute, dropping concentration was the hydrochloric acid of 3-6mol/l, and regulation pH is 2-3, is passed through nitrogen, is heated to boiling, keeps boiling
57-60 minute, discharging, it is cooled to room temperature, obtains hydroxylating nylon liquid；
(6) by above-mentioned 1,2-methylimidazole joins in the dehydrated alcohol of its weight 6-8 times, rises high-temperature and is 80-86 DEG C, adds
Entering Cera Flava, insulated and stirred 10-15 minute, add lauryl dimethyl amine oxide, stirring, to room temperature, obtains alcohol emulsion；
(7) by above-mentioned sulfonic acid guanidine grafting carbon nanotube, ring three phosphonitrile grafting carbon nanotube, the mixing of hydroxylating nylon liquid, at 87-90
Preheat 4-6 minute at DEG C, rise high-temperature and be 155-160 DEG C, insulated and stirred 3-4 minute, add above-mentioned alcohol emulsion, 100-200 turns/
Divide stirring 3-4 minute, filter, precipitation oxolane is washed 2-3 time, is vacuum dried 30-40 minute at being placed in 70-80 DEG C,
Obtain modified nylon CNT；
(8) above-mentioned modified nylon CNT is mixed with remaining each raw material, stir, dry, put into screw extruder and melt
Melt extrusion, cool down, sieve, obtain described CABLE MATERIALS.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108485270A (en) * | 2018-03-28 | 2018-09-04 | 天长市蓝天复合材料有限公司 | A kind of anti-flammability glass-fiber reinforced plastic grille and preparation method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104861397A (en) * | 2015-06-02 | 2015-08-26 | 珠海汉胜科技股份有限公司 | Polyvinyl chloride cable material and preparation method thereof |
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2016
- 2016-07-05 CN CN201610521795.XA patent/CN106046608A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104861397A (en) * | 2015-06-02 | 2015-08-26 | 珠海汉胜科技股份有限公司 | Polyvinyl chloride cable material and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| 孙军: ""新型无卤阻燃聚酰胺纤维、织物的研究"", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108485270A (en) * | 2018-03-28 | 2018-09-04 | 天长市蓝天复合材料有限公司 | A kind of anti-flammability glass-fiber reinforced plastic grille and preparation method |
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