CN106009401A - Waterproof flame-retardant cable material and preparation method thereof - Google Patents
Waterproof flame-retardant cable material and preparation method thereof Download PDFInfo
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
- H01B3/443—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from vinylhalogenides or other halogenoethylenic compounds
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
- H01B7/29—Protection against damage caused by extremes of temperature or by flame
- H01B7/295—Protection against damage caused by extremes of temperature or by flame using material resistant to flame
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- 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
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Abstract
The invention discloses a waterproof flame-retardant cable material. The waterproof flame-retardant cable material is prepared from, by weight, 0.1-0.2 part of 2,2-dibromo-3-nitrilopropionamide, 6-7 parts of guanidine sulfamate, 20-23 parts of carbon nanotubes, 0.3-0.4 part of dicyclohexyl-carbodiimid, 4-5 parts of phosphonitrilic chloride trimer, 0.2-0.4 part of sodium hydroxide, 1-2 parts of thiourea, 17-20 parts of nylon, 120-130 parts of polyvinyl chloride, 0.3-1 part of triterpenoid saponin, 3-5 parts of microcrystalline wax, 4-6 parts of di-iso-decylphthalate, 0.3-0.5 part of diazolidinyl urea, 1-2 parts of sodium hexametaphosphate and 2-4 parts of calcium phosphate. The cable material has high hydrophobicity and is smooth in surface, free of shrinkage cavities, strong in anti-seepage function and good in comprehensive performance.
Description
Technical field
The present invention relates to CABLE MATERIALS technical field, particularly relate to a kind of water proof fire retardant CABLE MATERIALS 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 water proof fire retardant CABLE MATERIALS and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of water proof fire retardant CABLE MATERIALS, it is made up of the raw material of following weight parts:
2,2-bis-bromo-3-nitrilo propionic acid amide. 0.1-0.2, 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, triterpene saponin 0.3-1, microcrystalline wax 3-5, diisooctyl phthalate 4-6, double imidazolidinyl urea 0.3-0.5, sodium hexameta phosphate 1-2, calcium phosphate 2-4.
A kind of preparation method of described water proof fire retardant CABLE MATERIALS, 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) above-mentioned pair of imidazolidinyl urea is joined in the DMF of its weight 17-20 times, stir, add the 36-40% of above-mentioned acidifying carbon nanotubes, rise high-temperature and be 60-70 DEG C, insulated and stirred 10-17 minute, adding triterpene saponin, stirring, to room temperature, obtains amide dispersion liquid；
(3) taking above-mentioned Guanidine Sulfamate 99, N, N'-Dicyclohexylcarbodiimide mixes, and joins the N of compound weight 70-80 times, in dinethylformamide, 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) above-mentioned calcium phosphate is joined in the oxolane of its weight 16-20 times, ultrasonic 2-3 minute, add thiourea, stir, obtain furan dispersion liquid；
(5) by remaining acidifying CNT, hexachlorocyclotriph,sphazene, sodium hydroxide mixing, join in the oxolane of compound weight 60-70 times, add above-mentioned furan dispersion liquid, 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 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) above-mentioned sodium hexameta phosphate is joined in the deionized water of its weight 170-200 times, rise high-temperature and be 60-65 DEG C, add above-mentioned acid guanidine grafting carbon nanotube, ring three phosphonitrile grafting carbon nanotube, ultrasonic 10-20 minute, filter, normal temperature drying will be precipitated, obtain composite carbon nanometer tube；
(8) by above-mentioned composite carbon nanometer tube, 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, 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；
(9) 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 CABLE MATERIALS.
nullThe invention have the advantage that the CABLE MATERIALS 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 CABLE MATERIALS of the present invention has good hydrophobicity, and surfacing is without shrinkage cavity, and leakage resistance is strong, good combination property.
Detailed description of the invention
A kind of water proof fire retardant CABLE MATERIALS, it is made up of the raw material of following weight parts:
2,2 dibromo nitrilo propionic acid amide .s 0.1, 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, triterpene saponin 0.3, microcrystalline wax 3, diisooctyl phthalate 4, double imidazolidinyl urea 0.3, sodium hexameta phosphate 1, calcium phosphate 2.
A kind of preparation method of described water proof fire retardant CABLE MATERIALS, 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) above-mentioned pair of imidazolidinyl urea is joined in the DMF of its weight 17 times, stir, adding the 36% of above-mentioned acidifying carbon nanotubes, rising high-temperature is 60 DEG C, insulated and stirred 10 minutes, adding triterpene saponin, stirring, to room temperature, obtains amide dispersion liquid；
(3) taking above-mentioned Guanidine Sulfamate 99, N, N' Dicyclohexylcarbodiimide mixes, and joins the N of compound weight 70 times, in N-dimethylformamide, add above-mentioned amide dispersion liquid, ultrasonic 100 minutes, sending in reactor, be 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) above-mentioned calcium phosphate is joined in the oxolane of its weight 16 times, ultrasonic 2 minutes, add thiourea, stir, obtain furan dispersion liquid；
(5) by remaining acidifying CNT, hexachlorocyclotriph,sphazene, sodium hydroxide mixing, join in the oxolane of compound weight 60 times, add above-mentioned furan dispersion liquid, ultrasonic 100 minutes, sending in reactor, be passed through nitrogen, rising high-temperature is 68 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 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) being joined by above-mentioned sodium hexameta phosphate in the deionized water of its weight 170 times, rising high-temperature is 60 DEG C, adds above-mentioned acid guanidine grafting carbon nanotube, ring three phosphonitrile grafting carbon nanotube, ultrasonic 10 minutes, filters, will precipitate normal temperature drying, and obtain composite carbon nanometer tube；
(8) by above-mentioned composite carbon nanometer tube, the mixing of hydroxylating nylon liquid, preheating 4 minutes at 87 DEG C, rising high-temperature is 155 DEG C, insulated and stirred 3 minutes, filters, and is washed 2 times by precipitation oxolane, it is placed at 70 DEG C vacuum drying 30 minutes, obtains modified nylon CNT；
(9) 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 CABLE MATERIALS.
Performance test:
Hot strength: 19.4 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 (%)-7.9；
Extension at break rate of change (%)-8.0.
Claims (2)
1. a water proof fire retardant CABLE MATERIALS, it is characterised in that it is made up of the raw material of following weight parts:
2,2-bis-bromo-3-nitrilo propionic acid amide. 0.1-0.2, 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, triterpene saponin 0.3-1, microcrystalline wax 3-5, diisooctyl phthalate 4-6, double imidazolidinyl urea 0.3-0.5, sodium hexameta phosphate 1-2, calcium phosphate 2-4.
2. the preparation method of a water proof fire retardant CABLE MATERIALS 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) above-mentioned pair of imidazolidinyl urea is joined in the DMF of its weight 17-20 times, stir, add the 36-40% of above-mentioned acidifying carbon nanotubes, rise high-temperature and be 60-70 DEG C, insulated and stirred 10-17 minute, adding triterpene saponin, stirring, to room temperature, obtains amide dispersion liquid；
(3) taking above-mentioned Guanidine Sulfamate 99, N, N'-Dicyclohexylcarbodiimide mixes, and joins the N of compound weight 70-80 times, in dinethylformamide, 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) above-mentioned calcium phosphate is joined in the oxolane of its weight 16-20 times, ultrasonic 2-3 minute, add thiourea, stir, obtain furan dispersion liquid；
(5) by remaining acidifying CNT, hexachlorocyclotriph,sphazene, sodium hydroxide mixing, join in the oxolane of compound weight 60-70 times, add above-mentioned furan dispersion liquid, 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 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) above-mentioned sodium hexameta phosphate is joined in the deionized water of its weight 170-200 times, rise high-temperature and be 60-65 DEG C, add above-mentioned acid guanidine grafting carbon nanotube, ring three phosphonitrile grafting carbon nanotube, ultrasonic 10-20 minute, filter, normal temperature drying will be precipitated, obtain composite carbon nanometer tube；
(8) by above-mentioned composite carbon nanometer tube, 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, 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；
(9) 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 CABLE MATERIALS.
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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 |
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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 |
|---|
| 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》 * |
| 杨中文 编著: "《塑料用树脂与助剂》", 31 December 2009, 北京：印刷工业出版社 * |
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