CN106009383A - Nylon plastic flame-retardant optical cable material and preparation method thereof - Google Patents
Nylon plastic flame-retardant optical cable material and preparation method thereof Download PDFInfo
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- CN106009383A CN106009383A CN201610457195.1A CN201610457195A CN106009383A CN 106009383 A CN106009383 A CN 106009383A CN 201610457195 A CN201610457195 A CN 201610457195A CN 106009383 A CN106009383 A CN 106009383A
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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
- 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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Abstract
The invention discloses a nylon plastic flame-retardant optical cable material. The material is prepared from raw materials in parts by weight as follows: 1-2 parts of calcium sulfoaluminate, 0.8-1 part of pentaerythritol, 6-7 parts of guanidine sulfamic acid, 20-23 parts of carbon nanotubes, 0.3-0.4 parts of N,N'-dicyclohexylcarbodiimide, 4-5 parts of phosphonitrilic chloride trimer, 0.2-0.4 parts of sodium hydroxide, 1-2 parts of thiourea, 17-20 parts of nylon, 120-130 parts of polyvinyl chloride, 0.7-1 part of ammonium hexafluorozirconate, 0.1-0.2 parts of triethanolamine borate, 0.8-1 part of 2-thiol benzimidazole, 2-4 parts of talc, 3-5 parts of dimethyl succinate and 0.4-1 part of tin octyl mercaptan. According to the material, nylon and polyvinyl chloride are blended, so that the dispersity of filler particles in a polymer is effectively improved, agglomeration is reduced, and the stability of a finished product is improved.
Description
Technical field
The present invention relates to mass technical field, particularly relate to a kind of nylon plastic(s) fire-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, adds after nanoparticle in the polymer, can the performance of significantly lift-off material.Such as when adding the nanoparticles such as a small amount of graphite skilful, CNT, molybdenum bisuphide in polymer, the mechanical strength of material will be obviously improved IWI.Research finds, only adds minimal amount of nano material and the HRR of material combustion just can be greatly reduced, the most also can the mechanical strength of lift-off composite.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, and fire retardant mechanism also with other nanoparticle difference, needs bigger addition, therefore can not be classified as flame retardant nano-materials completely when reality is applied.And the filling of filler also can produce impact to the mechanical property of material self.(2) laminated inorganic matter, such as nanoclay, brucite, expansible graphite etc..(3) pipe carbon and acicular nanoparticles, such as CNT, halloysite nanotubes and meerschaum etc..The tenth day of lunar month year in 21 century, the focus nano flame retardant technology having a large amount of report galapectite in recent years about polymer/carbon nano-tube flame-retardant system and meerschaum to be increasingly becoming research occurs two during the last ten years, although gradually growing up and achieve 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. nano fire-retarding additive significant advantage is that in trying for taper calorimetric, HRR reduces for a lot of nanoparticles, it is only necessary to add few amount and just the HRR of material combustion can be greatly reduced by W.But effect is tested significantly for traditional fire-retardant trial work section, such as oxygen index (OI) and vertical combustion, the most also can play negative effect.Therefore, need to consider nanoparticle to be modified or reaches the effect of cooperative flame retardant by compounding use with conventional flame retardant.The most in recent years, nanometer particle-modified research is got more and more, the particularly intercalation modifying to nanoclay.But the intercalation modifying agent of existing frequently-used nanoclay is the burning base amine salt of long-chain mostly, lacks and be specifically designed to flame-retardant modified intercalator or surface modifier.And most modifying agent itself does not have anti-flammability, some self the most flammable；Heat stability is the most poor, and initial decomposition degree is low, and difficulty is applicable to engineering plastics etc. and irons and melt the polymer that temperature is higher.Therefore, it is a direction of future studies for having nanometer particle-modified dose of anti-flammability and heat stability concurrently.3. having clear and definite fire retardant mechanism from the fire retardant such as halogen flame, phosphor nitrogen combustion inhibitor different, present stage lacks the explanation of system to the mechanism of nano flame retardant.Current approved mechanism mainly has the obstruct mechanism of the radical-scavenging mechanism of nanoclay, solid phase；Synergistic catalytic mechanism with expanding fire retardant；The network structure of CNT intercepts the impact etc. in mechanism and combustion process on system rheological characteristic.Therefore, the elaboration for nanoparticle fire retardant mechanism during polymer combustion will be the direction of future studies, and CNT lacks polar functional group due to surface simultaneously, and the compatibility with polymeric matrix is poor；The structure of high length-diameter ratio can cause the winding in the course of processing, gathering, thus is difficult to well disperse.Additionally, CNT only has obvious effect to reduction HRR, but can not effectively put forward oxygen index (OI) and the vertical combustion grade of material.In order to improve the CNT compatibility in the polymer and dispersibility, can use coupling agent, surfactant or polymer etc. that CNT is carried out surface to change, but class method of modifying often difficulty puies forward its fire resistance, some even can destroy 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 nylon plastic(s) fire-retardant cable material and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of nylon plastic(s) fire-retardant cable material, it is made up of the raw material of following weight parts:
Calcium sulphoaluminate 1-2, tetramethylolmethane 0.8-1, Guanidine Sulfamate 99 6-7, CNT 20-23, N, N'-Dicyclohexylcarbodiimide 0.3-0.4, hexachlorocyclotriph,sphazene 4-5, sodium hydroxide 0.2-0.4, thiourea 1-2, nylon 17-20, polrvinyl chloride 120-130, ammonium fluozirconate 0.7-1, triethanolamine borate 0.1-0.2,2-mercapto benzimidazole 0.8-1, Pulvis Talci 2-4, dimethyl succinate 3-5, octyl mercaptan stannum 0.4-1.
A kind of preparation method of described nylon plastic(s) fire-retardant cable material, it is made up of the raw material of following weight parts:
(1) above-mentioned CNT is joined in the mixed acid solution of its weight 80-100 times, described nitration mixture is made up of the sulphuric acid of the 96-98% that mass ratio is 3-4:1 and the hydrochloric acid solution of 87-90%, at 50-60 DEG C ultrasonic 17-20 minute, filter, precipitation is washed 2-3 time, it is vacuum dried 30-40 minute at 70-76 DEG C, obtains acidifying CNT；
(2) take above-mentioned 2-mercapto benzimidazole, join in the DMF of its weight 27-30 times, stir, add Pulvis Talci, ultrasonic 3-5 minute, obtain amide dispersion liquid；
(3) 47-50% of above-mentioned acidifying carbon nanotubes is taken, with Guanidine Sulfamate 99, N, N'-Dicyclohexylcarbodiimide mixes, join the N of compound weight 70-80 times, in dinethylformamide, stir, add above-mentioned amide dispersion 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 the baking oven of 70-80 DEG C and is dried to constant weight, obtain sulfonic acid guanidine grafting carbon nanotube；
(4) by above-mentioned octyl mercaptan stannum, thiourea mixing, join in the oxolane of compound weight 10-13 times, stir, obtain tetrahydrofuran solution；
(5) by remaining acidifying CNT, hexachlorocyclotriph,sphazene, sodium hydroxide mixing, join in the oxolane of compound weight 60-70 times, ultrasonic 100-110 minute, send in reactor, it is passed through nitrogen, rises high-temperature and be 68-70 DEG C, add above-mentioned tetrahydrofuran solution, 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 nanotube；
(6) 10-16% of above-mentioned nylon weight is taken, add in its weight 20-27 times, 17-20% formalin, stirring mixing 20-30 minute, dropping concentration is the hydrochloric acid of 3-6mol/l, and regulation pH is 2-3, it is passed through nitrogen, it is heated to boiling, keeps boiling 57-60 minute, discharging, it is cooled to room temperature, obtains hydroxylating nylon liquid；
(7) by above-mentioned sulfonic acid guanidine grafting carbon nanotube, ring three phosphonitrile grafting carbon nanotube, the mixing of hydroxylating nylon liquid, preheat 4-6 minute at 87-90 DEG C, rise high-temperature and be 155-160 DEG C, insulated and stirred 3-4 minute, adds above-mentioned calcium sulphoaluminate, ammonium fluozirconate, stirs, filter, precipitation oxolane is washed 2-3 time, is vacuum dried 30-40 minute at being placed in 70-80 DEG C, 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 extrude, cool down, sieve, obtain described mass.
nullThe invention have the advantage that the mass of the present invention has good fire-retardant fireproof performance，The present invention first uses Guanidine Sulfamate 99、The pre-nylon blending of CNT that chlorine ring three phosphonitrile is grafted respectively，Nylon after hydroxylating discharging can have the good compatibility with the CNT after grafting，Improve this composite dispersibility in finished cable material the most further，The fire retardant mechanism of this composite is: when nylon in combustion，CNT is at polymer melt surface aggregation，And form cancellated layer of charcoal，These netted carbon-coatings are fine and close and almost without hole，It is effectively prevented outside heat and the entrance of oxygen when burning，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，Guanidine Sulfamate 99 self decomposes can produce ammonia，Ammonia can react again the degraded promoting nylon with nylon，Both are common produces substantial amounts of ammonia、The non-flammable compressive gas such as steam and carbon dioxide，Oxygen in dilute combustion district and fuel gas，Play the effect that gas phase is fire-retardant；Chlorine ring three phosphonitrile of grafting plays the effect of similar patch, the mesh of the netted layer of charcoal that filling carbon nano-pipe is formed, can form Cl-, and catch the free radical that burning produces in chlorine atom combustion process the most therein, thus terminate the chain reaction of combustion process, improve the fire resistance of finished-product material.The present invention uses nylon with polychloroethylene blended, effectively raises filler grain dispersibility in the polymer, reduces reunion, improves the stability of finished product.
Detailed description of the invention
A kind of nylon plastic(s) fire-retardant cable material, it is made up of the raw material of following weight parts:
Calcium sulphoaluminate 1, tetramethylolmethane 0.8, Guanidine Sulfamate 99 6, CNT 20, N, N' Dicyclohexylcarbodiimide 0.3, hexachlorocyclotriph,sphazene 4, sodium hydroxide 0.2, thiourea 1, nylon 17, polrvinyl chloride 120, ammonium fluozirconate 0.7, triethanolamine borate 0.1,2 mercapto benzimidazole 0.8, Pulvis Talci 2, dimethyl succinate 3, octyl mercaptan stannum 0.4.
A kind of preparation method of described nylon plastic(s) fire-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 made up of the sulphuric acid of 96% that mass ratio is 3:1 and the hydrochloric acid solution of 87%, at 50 DEG C ultrasonic 17 minutes, filter, precipitation is washed 2 times, is vacuum dried 30 minutes at 70 DEG C, obtains acidifying CNT；
(2) take above-mentioned 2 mercapto benzimidazoles, join in the DMF of its weight 27 times, stir, add Pulvis Talci, ultrasonic 3 minutes, obtain amide dispersion liquid；
(3) taking the 47% of above-mentioned acidifying carbon nanotubes, with Guanidine Sulfamate 99, N, N' Dicyclohexylcarbodiimide mixes, join in the DMF of compound weight 70 times, stir, add above-mentioned amide dispersion liquid, ultrasonic 100 minutes, send in reactor, being passed through nitrogen, rising high-temperature 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 constant weight, obtain sulfonic acid guanidine grafting carbon nanotube；
(4) by above-mentioned octyl mercaptan stannum, thiourea mixing, join in the oxolane of compound weight 10 times, stir, obtain tetrahydrofuran solution；
(5) by remaining acidifying CNT, hexachlorocyclotriph,sphazene, sodium hydroxide mixing, join in the oxolane of compound weight 60 times, ultrasonic 100 minutes, send in reactor, being passed through nitrogen, rising high-temperature is 68 DEG C, adds above-mentioned tetrahydrofuran solution, 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 constant weight, obtain ring three phosphonitrile grafting carbon nanotube；
(6) take the 10% of above-mentioned nylon weight, add in its weight 20 times, the formalin of 17%, stirring mixing 20 minutes, dropping concentration is the hydrochloric acid of 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；
(7) by above-mentioned sulfonic acid guanidine grafting carbon nanotube, ring three phosphonitrile grafting carbon nanotube, the mixing of hydroxylating nylon liquid, preheat 4 minutes at 87 DEG C, rising high-temperature is 155 DEG C, insulated and stirred 3 minutes, adds above-mentioned calcium sulphoaluminate, ammonium fluozirconate, stirs, filter, precipitation oxolane is washed 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 extrude, cool down, sieve, obtain described mass.
Performance test:
Hot strength: 19.9 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 (%)-7.1；
Extension at break rate of change (%)-8.1.
Claims (2)
1. a nylon plastic(s) fire-retardant cable material, it is characterised in that it is made up of the raw material of following weight parts:
Calcium sulphoaluminate 1-2, tetramethylolmethane 0.8-1, Guanidine Sulfamate 99 6-7, CNT 20-23, N, N'-Dicyclohexylcarbodiimide 0.3-0.4, hexachlorocyclotriph,sphazene 4-5, sodium hydroxide 0.2-0.4, thiourea 1-2, nylon 17-20, polrvinyl chloride 120-130, ammonium fluozirconate 0.7-1, triethanolamine borate 0.1-0.2,2-mercapto benzimidazole 0.8-1, Pulvis Talci 2-4, dimethyl succinate 3-5, octyl mercaptan stannum 0.4-1.
2. the preparation method of a nylon plastic(s) fire-retardant cable material as claimed in claim 1, it is characterised in that it is made up of the raw material of following weight parts:
(1) above-mentioned CNT is joined in the mixed acid solution of its weight 80-100 times, described nitration mixture is made up of the sulphuric acid of the 96-98% that mass ratio is 3-4:1 and the hydrochloric acid solution of 87-90%, at 50-60 DEG C ultrasonic 17-20 minute, filter, precipitation is washed 2-3 time, it is vacuum dried 30-40 minute at 70-76 DEG C, obtains acidifying CNT；
(2) take above-mentioned 2-mercapto benzimidazole, join in the DMF of its weight 27-30 times, stir, add Pulvis Talci, ultrasonic 3-5 minute, obtain amide dispersion liquid；
(3) 47-50% of above-mentioned acidifying carbon nanotubes is taken, with Guanidine Sulfamate 99, N, N'-Dicyclohexylcarbodiimide mixes, join the N of compound weight 70-80 times, in dinethylformamide, stir, add above-mentioned amide dispersion 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 the baking oven of 70-80 DEG C and is dried to constant weight, obtain sulfonic acid guanidine grafting carbon nanotube；
(4) by above-mentioned octyl mercaptan stannum, thiourea mixing, join in the oxolane of compound weight 10-13 times, stir, obtain tetrahydrofuran solution；
(5) by remaining acidifying CNT, hexachlorocyclotriph,sphazene, sodium hydroxide mixing, join in the oxolane of compound weight 60-70 times, ultrasonic 100-110 minute, send in reactor, it is passed through nitrogen, rises high-temperature and be 68-70 DEG C, add above-mentioned tetrahydrofuran solution, 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 nanotube；
(6) 10-16% of above-mentioned nylon weight is taken, add in its weight 20-27 times, 17-20% formalin, stirring mixing 20-30 minute, dropping concentration is the hydrochloric acid of 3-6mol/l, and regulation pH is 2-3, it is passed through nitrogen, it is heated to boiling, keeps boiling 57-60 minute, discharging, it is cooled to room temperature, obtains hydroxylating nylon liquid；
(7) by above-mentioned sulfonic acid guanidine grafting carbon nanotube, ring three phosphonitrile grafting carbon nanotube, the mixing of hydroxylating nylon liquid, preheat 4-6 minute at 87-90 DEG C, rise high-temperature and be 155-160 DEG C, insulated and stirred 3-4 minute, adds above-mentioned calcium sulphoaluminate, ammonium fluozirconate, stirs, filter, precipitation oxolane is washed 2-3 time, is vacuum dried 30-40 minute at being placed in 70-80 DEG C, 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 extrude, cool down, sieve, obtain described mass.
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| Application Number | Priority Date | Filing Date | Title |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108545717A (en) * | 2018-05-21 | 2018-09-18 | 广东工业大学 | A kind of method and modified carbon nano-tube of surface modification of carbon nanotube |
| WO2019210588A1 (en) * | 2018-05-04 | 2019-11-07 | 江苏弘盛新材料股份有限公司 | Light fire-retardant pa engineering plastic filler and preparation method therefor |
| WO2023060560A1 (en) * | 2021-10-14 | 2023-04-20 | 武汉工程大学 | P-n-b flame-retardant pbs plastic and preparation method therefor |
-
2016
- 2016-06-22 CN CN201610457195.1A patent/CN106009383A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019210588A1 (en) * | 2018-05-04 | 2019-11-07 | 江苏弘盛新材料股份有限公司 | Light fire-retardant pa engineering plastic filler and preparation method therefor |
| CN108545717A (en) * | 2018-05-21 | 2018-09-18 | 广东工业大学 | A kind of method and modified carbon nano-tube of surface modification of carbon nanotube |
| WO2023060560A1 (en) * | 2021-10-14 | 2023-04-20 | 武汉工程大学 | P-n-b flame-retardant pbs plastic and preparation method therefor |
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Application publication date: 20161012 |