CN116790094A - Flame-retardant waterproof bus duct and preparation method thereof - Google Patents
Flame-retardant waterproof bus duct and preparation method thereof Download PDFInfo
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- CN116790094A CN116790094A CN202310708779.1A CN202310708779A CN116790094A CN 116790094 A CN116790094 A CN 116790094A CN 202310708779 A CN202310708779 A CN 202310708779A CN 116790094 A CN116790094 A CN 116790094A
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- flame
- retardant
- zirconium carbide
- bus duct
- powder
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 104
- 239000003063 flame retardant Substances 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 229910026551 ZrC Inorganic materials 0.000 claims abstract description 62
- OTCHGXYCWNXDOA-UHFFFAOYSA-N [C].[Zr] Chemical compound [C].[Zr] OTCHGXYCWNXDOA-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000008139 complexing agent Substances 0.000 claims abstract description 34
- 239000003607 modifier Substances 0.000 claims abstract description 29
- 239000000945 filler Substances 0.000 claims abstract description 26
- 238000005266 casting Methods 0.000 claims abstract description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-N acetic acid Substances CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- ROHTVIURAJBDES-UHFFFAOYSA-N 2-n,2-n-bis(prop-2-enyl)-1,3,5-triazine-2,4,6-triamine Chemical compound NC1=NC(N)=NC(N(CC=C)CC=C)=N1 ROHTVIURAJBDES-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003822 epoxy resin Substances 0.000 claims abstract description 17
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 17
- 230000000379 polymerizing effect Effects 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 239000000843 powder Substances 0.000 claims description 44
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- 238000001035 drying Methods 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- 238000010438 heat treatment Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 24
- 239000000047 product Substances 0.000 claims description 22
- 239000007822 coupling agent Substances 0.000 claims description 21
- 238000005406 washing Methods 0.000 claims description 21
- 238000005485 electric heating Methods 0.000 claims description 20
- 239000011256 inorganic filler Substances 0.000 claims description 20
- 229910003475 inorganic filler Inorganic materials 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 15
- 230000004913 activation Effects 0.000 claims description 14
- 239000000463 material Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical group N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 238000010992 reflux Methods 0.000 claims description 9
- YUAXLYYGNPOOKU-UHFFFAOYSA-N OP(=O)=CC(=O)O Chemical compound OP(=O)=CC(=O)O YUAXLYYGNPOOKU-UHFFFAOYSA-N 0.000 claims description 8
- YBRVSVVVWCFQMG-UHFFFAOYSA-N 4,4'-diaminodiphenylmethane Chemical compound C1=CC(N)=CC=C1CC1=CC=C(N)C=C1 YBRVSVVVWCFQMG-UHFFFAOYSA-N 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 5
- 230000000996 additive effect Effects 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 239000010445 mica Substances 0.000 claims description 5
- 229910052618 mica group Inorganic materials 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000006772 olefination reaction Methods 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 239000012265 solid product Substances 0.000 claims description 5
- 239000003999 initiator Substances 0.000 claims description 4
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 4
- 229910052622 kaolinite Inorganic materials 0.000 claims description 4
- 229910052611 pyroxene Inorganic materials 0.000 claims description 4
- 239000010453 quartz Substances 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims description 3
- 229910021532 Calcite Inorganic materials 0.000 claims description 3
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims description 3
- 229940018564 m-phenylenediamine Drugs 0.000 claims description 3
- 125000003118 aryl group Chemical group 0.000 claims description 2
- 238000013329 compounding Methods 0.000 claims description 2
- 239000004845 glycidylamine epoxy resin Substances 0.000 claims description 2
- 229920000768 polyamine Polymers 0.000 claims description 2
- 229920005989 resin Polymers 0.000 abstract description 5
- 239000011347 resin Substances 0.000 abstract description 5
- 238000004132 cross linking Methods 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 4
- 230000000536 complexating effect Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 18
- -1 glycidol amine Chemical class 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 7
- 230000005540 biological transmission Effects 0.000 description 4
- 239000004020 conductor Substances 0.000 description 4
- 235000019441 ethanol Nutrition 0.000 description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 4
- 239000008213 purified water Substances 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000009970 fire resistant effect Effects 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 125000002897 diene group Chemical group 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- ABLZXFCXXLZCGV-UHFFFAOYSA-N phosphonic acid group Chemical group P(O)(O)=O ABLZXFCXXLZCGV-UHFFFAOYSA-N 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003918 triazines Chemical class 0.000 description 1
Classifications
-
- 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
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34928—Salts
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/10—Metal compounds
- C08K3/14—Carbides
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- 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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- 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
-
- 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
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)
- Fireproofing Substances (AREA)
Abstract
The invention relates to a flame-retardant waterproof bus duct and a preparation method thereof, wherein the bus duct comprises casting rubber, and the casting rubber comprises the following components in parts by weight: 50-70 parts of epoxy resin, 20-30 parts of fireproof filler, 14-28 parts of flame-retardant complexing agent and 25-35 parts of curing agent; the flame-retardant complexing agent is prepared by combining 2-hydroxy-phosphoric acid-acetic acid and 2, 4-diamino-6-diallylamino-1, 3, 5-triazine to obtain a flame-retardant modifier, and polymerizing the flame-retardant modifier and olefinized zirconium carbide. The flame retardant complexing agent prepared by the invention is obtained by carrying out a crosslinking complexing reaction on a flame retardant modifier obtained by the reaction of 2-hydroxy phosphoric acid acetic acid and 2, 4-diamino-6-diallylamino-1, 3, 5-triazine and olefinized zirconium carbide. The flame-retardant complexing agent prepared by the invention has excellent flame-retardant effect and can enhance other performance performances of the resin.
Description
Technical Field
The invention relates to the field of bus ducts, in particular to a flame-retardant waterproof bus duct and a preparation method thereof.
Background
The bus duct is a novel conductor formed by taking copper or aluminum as a conductor, supporting the conductor by non-olefinic insulation, and then filling the conductor into a metal groove. The bus duct is commonly used in power equipment, the bus duct consists of a bus wrapped with a fire-resistant mica tape and a bracket made of fire-resistant insulating materials, a plurality of grooves are formed in the bracket, the bus is arranged in the grooves and fixed, the bus duct is correspondingly adapted according to different environments,
bus ducts have increasingly replaced wires and cables in the field of low-voltage indoor power transmission mains engineering. With the advent of modern industrial facilities and equipment, the power consumption of various industries is rapidly increased, and particularly, the occurrence of numerous high-rise buildings and large-scale factory workshops, the conventional cable serving as a power transmission wire cannot meet the requirements in a high-current transmission system, and the parallel connection use of multiple cables brings a plurality of inconveniences to field installation construction connection. The plug-in bus duct is a novel distribution wire, compared with the traditional cable, the plug-in bus duct fully shows its superiority in the process of heavy current transmission, and meanwhile, due to the adoption of the novel technology and the novel process, the contact resistance and the temperature rise of the connection part of the two ends of the bus duct and the plug-in position of the wire distributing port are greatly reduced, and a high-quality insulating material is used in the bus duct, so that the safety and the reliability of the bus duct are improved, and the whole system is more perfect.
The cast bus duct on the market at present is formed by casting high-performance insulating resin and inorganic mineral substances, the bus duct is directly cast and sealed, and the cast bus duct has certain waterproof, fireproof, explosion-proof and other functions, but along with the improvement of the requirements of the bus duct, the waterproof property and the flame retardance of the bus duct on the market at present cannot meet the requirements.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a flame-retardant waterproof bus duct and a preparation method thereof.
The aim of the invention is realized by adopting the following technical scheme:
in a first aspect, the invention provides a flame-retardant waterproof bus duct, which comprises a casting rubber, wherein the casting rubber comprises the following components in parts by weight:
50-70 parts of epoxy resin, 20-30 parts of fireproof filler, 14-28 parts of flame-retardant complexing agent and 25-35 parts of curing agent.
Preferably, the epoxy resin is glycidylamine epoxy resin, and the model comprises AG-80 or AFG-90.
Preferably, the fireproof filler is a product of inorganic filler subjected to activation treatment of a coupling agent KH 570; the inorganic filler comprises one or more of quartz powder, mica powder, pyroxene powder, calcite powder, kaolinite powder and talcum powder; the particle size of the inorganic filler is 10-20 μm.
Preferably, the preparation process of the fireproof filler comprises the following steps:
placing inorganic filler into 50% ethanol water solution by mass fraction, dispersing uniformly by ultrasonic, dripping coupling agent KH570, heating to reflux and stirring for 8-12h, centrifuging to obtain solid particles, washing with purified water for three times, and drying in an oven at 80-100deg.C to obtain filler.
Preferably, the mass ratio of the inorganic filler, the coupling agent KH570 and the aqueous ethanol solution is 1:0.15:10.
Preferably, the flame retardant complexing agent is prepared by combining 2-hydroxyphosphoryl acetic acid and 2, 4-diamino-6-diallylamino-1, 3, 5-triazine to obtain a flame retardant modifier, and then polymerizing the flame retardant modifier with the olefinized zirconium carbide.
Preferably, the curing agent is an aromatic polyamine curing agent and comprises any one or more of 4,4 '-diaminodiphenyl methane, 4' -diaminodiphenyl sulfone and m-phenylenediamine.
Preferably, the preparation method of the flame retardant additive comprises the following steps:
s1, preparation of a flame retardant modifier:
mixing 2-hydroxy phosphoric acid base acetic acid and absolute ethyl alcohol in a reaction bottle, building the reaction bottle on an electric heating sleeve provided with a stirrer, heating the electric heating sleeve to 45-55 ℃, stirring until the electric heating sleeve is completely dissolved, gradually adding 2, 4-diamino-6-diallylamino-1, 3, 5-triazine in half an hour, heating the electric heating sleeve to 70-80 ℃, carrying out heat preservation reflux reaction for 4-6 hours, and sequentially carrying out centrifugal separation, washing and drying to obtain the flame retardant modifier;
s2, olefination treatment of zirconium carbide:
dispersing zirconium carbide powder in a sodium hydroxide solution, stirring for 4-8 hours at 45-55 ℃, separating out the powder, washing to be neutral by using clear water, and drying to obtain a zirconium carbide activated product;
dispersing the zirconium carbide activation product in deionized water, dropwise adding a coupling agent KH-570, heating to 35-45 ℃, stirring and dispersing for 10-20 hours, separating out powder, washing with clear water for three times, and drying to obtain olefinized zirconium carbide;
s3, preparing a flame-retardant complexing agent:
dispersing olefine zirconium carbide and flame retardant modifier in N, N-dimethyl formamide successively, adding small amount of azo initiator, heating to 50-70 deg.c, maintaining for 5-10 hr while stirring, filtering to obtain solid product, washing with absolute alcohol for three times, and drying to obtain flame retardant compounding agent.
Preferably, in the S1, the mass ratio of the 2-hydroxyphosphoryl acetic acid, the 2, 4-diamino-6-diallylamino-1, 3, 5-triazine and the absolute ethyl alcohol is 1.56-3.12:2.06-4.12:100-200.
Preferably, in the step S2, the grain diameter of the zirconium carbide powder is 30-50 μm, and the mass fraction of the sodium hydroxide solution is 10% -20%; the mass ratio of the zirconium carbide powder to the sodium hydroxide solution is 1:20-40.
Preferably, in the S2, the mass ratio of the zirconium carbide activation product, the coupling agent KH-570 and the deionized water is 1:0.1-0.3:20-40.
Preferably, in the S3, the mass ratio of the olefinized zirconium carbide, the flame retardant modifier and the N, N-dimethylformamide is 1:0.2-0.6:30-50.
Preferably, in the step S3, the azo initiator is azobisisobutyronitrile, and the addition amount is 1% -2% of the mass of the olefinized zirconium carbide.
In a second aspect, the invention provides a method for preparing a flame-retardant waterproof bus duct, which comprises the following steps:
step 1, preventing bus copper bars from being fixed in corresponding positions in a pre-prepared mold;
step 2, uniformly mixing the epoxy resin, the fireproof filler and the flame-retardant complexing agent in the casting rubber material component, uniformly mixing with the curing agent, and then injecting into the die in the step 2;
and step 3, placing the cast mould into a baking oven at 130-150 ℃ for drying treatment for 3-5 hours, and removing the mould after cooling to normal temperature to obtain the refractory bus duct.
The beneficial effects of the invention are as follows:
1. the invention prepares a flame-retardant waterproof bus duct, mainly aiming at improving the pouring rubber material in the bus duct, in order to enhance the performance of the pouring rubber material, the invention firstly adopts glycidol amine epoxy resin with multi-functionality, high epoxy equivalent, high crosslinking density and good heat resistance; secondly, the invention carries out activation treatment on the fireproof filler, wherein the coupling agent KH570 is used for the activation treatment, and the combination property between the activated fireproof filler and the resin is better; and then the invention also prepares the flame-retardant complexing agent, and compared with the flame retardant on the market, the flame-retardant complexing agent has better flame-retardant effect and can enhance the fire resistance and strength of the resin.
2. The flame retardant complexing agent prepared by the invention is obtained by carrying out a crosslinking complexing reaction on a flame retardant modifier obtained by the reaction of 2-hydroxy phosphoric acid acetic acid and 2, 4-diamino-6-diallylamino-1, 3, 5-triazine and olefinized zirconium carbide. The flame-retardant complexing agent prepared by the invention has excellent flame-retardant effect and can enhance other performance performances of the resin.
3. In the preparation process of the flame retardant modifier, reactants are 2-hydroxyphosphoric acid acetic acid containing reactive carboxyl and phosphonic acid groups and triazine compounds 2, 4-diamino-6-diallylamino-1, 3, 5-triazine containing diamino and diene groups, and the two reactants can be independently used as flame retardant materials. After the composite treatment of the invention, the two are combined into salt through carboxyl and amino, and then double bond groups on the product and double bond groups of olefinized zirconium carbide are utilized to carry out polymerization crosslinking, so that a reticular polymer which is coated on the surface of the zirconium carbide and contains a large amount of N and P elements is obtained.
Detailed Description
The technical scheme of the invention is described below through specific examples. It is to be understood that the mention of one or more method steps of the present invention does not exclude the presence of other method steps before and after the combination step or that other method steps may be interposed between these explicitly mentioned steps; it should also be understood that these examples are illustrative of the present invention and are not intended to limit the scope of the present invention. Moreover, unless otherwise indicated, the numbering of the method steps is merely a convenient tool for identifying the method steps and is not intended to limit the order of arrangement of the method steps or to limit the scope of the invention in which the invention may be practiced, as such changes or modifications in their relative relationships may be regarded as within the scope of the invention without substantial modification to the technical matter.
In order to better understand the above technical solution, exemplary embodiments of the present invention are described in more detail below. While exemplary embodiments of the invention are shown, it should be understood that the invention may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The invention is further described with reference to the following examples.
Example 1
The flame-retardant waterproof bus duct comprises casting rubber, wherein the casting rubber comprises the following components in parts by weight:
60 parts of glycidol amine epoxy resin AG-80, 25 parts of fireproof filler, 21 parts of flame retardant complexing agent and 30 parts of curing agent 4,4' -diaminodiphenyl methane.
The preparation process of the fireproof filler comprises the following steps:
placing inorganic filler in ethanol water solution with the mass fraction of 50%, uniformly dispersing by ultrasonic, dripping a coupling agent KH570, heating to reflux, stirring for 10 hours, centrifuging to obtain solid particles, flushing with purified water for three times, and drying in a 90 ℃ oven to obtain the filler; wherein the mass ratio of the inorganic filler to the coupling agent KH570 to the ethanol aqueous solution is 1:0.15:10; the inorganic filler comprises quartz powder, mica powder, pyroxene powder, calcite powder, kaolinite powder and talcum powder mixed according to the mass ratio of 0.8:0.6:1.2:1.5:1.3:1; the particle size of the inorganic filler is 10-20 μm.
The preparation method of the flame retardant additive comprises the following steps:
s1, preparation of a flame retardant modifier:
mixing 2-hydroxy phosphoric acid base acetic acid and absolute ethyl alcohol in a reaction bottle, building the reaction bottle on an electric heating sleeve provided with a stirrer, heating the electric heating sleeve to 50 ℃, stirring until the electric heating sleeve is completely dissolved, gradually adding 2, 4-diamino-6-diallylamino-1, 3, 5-triazine in half an hour, heating the electric heating sleeve to 75 ℃, carrying out heat preservation and reflux reaction for 5 hours, and sequentially carrying out centrifugal separation, washing and drying to obtain the flame retardant modifier;
wherein the mass ratio of the 2-hydroxyphosphoryl acetic acid to the 2, 4-diamino-6-diallylamino-1, 3, 5-triazine to the absolute ethyl alcohol is 2.34:3.09:200.
S2, olefination treatment of zirconium carbide:
dispersing zirconium carbide powder in a sodium hydroxide solution, stirring for 6 hours at 50 ℃, separating out the powder, washing to be neutral by using clear water, and drying to obtain a zirconium carbide activated product;
wherein the grain diameter of the zirconium carbide powder is 30-50 mu m, and the mass fraction of the sodium hydroxide solution is 15%; the mass ratio of the zirconium carbide powder to the sodium hydroxide solution is 1:30.
Dispersing the zirconium carbide activation product in deionized water, dropwise adding a coupling agent KH-570, heating to 40 ℃, stirring and dispersing for 15 hours, separating out powder, washing with clear water for three times, and drying to obtain olefinized zirconium carbide;
wherein the mass ratio of the zirconium carbide activation product, the coupling agent KH-570 and the deionized water is 1:0.2:30.
S3, preparing a flame-retardant complexing agent:
dispersing olefinized zirconium carbide and a flame retardant modifier in N, N-dimethylformamide in turn, adding a small amount of azodiisobutyronitrile, heating to 60 ℃, preserving heat for 8 hours, continuously stirring during the period, filtering out a solid product after the reaction is finished, washing for three times by using absolute ethyl alcohol, and drying to obtain a flame retardant complexing agent;
wherein the mass ratio of the olefinized zirconium carbide to the flame retardant modifier to the N, N-dimethylformamide is 1:0.4:40; the addition amount of the azodiisobutyronitrile is 2 percent of the mass of the olefin zirconium carbide.
The preparation method of the flame-retardant waterproof bus duct comprises the following steps:
step 1, preventing bus copper bars from being fixed in corresponding positions in a pre-prepared mold;
step 2, uniformly mixing the epoxy resin, the fireproof filler and the flame-retardant complexing agent in the casting rubber material component, uniformly mixing with the curing agent, and then injecting into the die in the step 2;
and 3, drying the cast die in an oven at 140 ℃ for 4 hours, and removing the die after cooling to normal temperature to obtain the refractory bus duct.
Example 2
The flame-retardant waterproof bus duct comprises casting rubber, wherein the casting rubber comprises the following components in parts by weight:
50 parts of glycidol amine epoxy resin AFG-90, 20 parts of fireproof filler, 14 parts of flame retardant complexing agent and 25 parts of curing agent 4,4' -diaminodiphenyl sulfone.
The preparation process of the fireproof filler comprises the following steps:
placing inorganic filler in ethanol water solution with the mass fraction of 50%, uniformly dispersing by ultrasonic, dripping a coupling agent KH570, heating to reflux, stirring for 8 hours, centrifuging to obtain solid particles, flushing with purified water for three times, and drying in an oven at 80 ℃ to obtain the filler; wherein the mass ratio of the inorganic filler to the coupling agent KH570 to the ethanol aqueous solution is 1:0.15:10; the inorganic filler comprises quartz powder, mica powder and pyroxene powder which are mixed according to the mass ratio of 1:1.2:1.6; the particle size of the inorganic filler is 10-20 μm.
The preparation method of the flame retardant additive comprises the following steps:
s1, preparation of a flame retardant modifier:
mixing 2-hydroxy phosphoric acid base acetic acid and absolute ethyl alcohol in a reaction bottle, building the reaction bottle on an electric heating sleeve provided with a stirrer, heating the electric heating sleeve to 45 ℃, stirring until the electric heating sleeve is completely dissolved, gradually adding 2, 4-diamino-6-diallylamino-1, 3, 5-triazine in half an hour, heating the electric heating sleeve to 70 ℃, carrying out heat preservation and reflux reaction for 4 hours, and sequentially carrying out centrifugal separation, washing and drying to obtain the flame retardant modifier;
wherein the mass ratio of the 2-hydroxy-phosphoric acid base acetic acid to the 2, 4-diamino-6-diallylamino-1, 3, 5-triazine to the absolute ethyl alcohol is 1.56:2.06:100.
S2, olefination treatment of zirconium carbide:
dispersing zirconium carbide powder in a sodium hydroxide solution, stirring for 4 hours at 45 ℃, separating out the powder, washing to be neutral by using clear water, and drying to obtain a zirconium carbide activated product;
wherein the grain diameter of the zirconium carbide powder is 30-50 mu m, and the mass fraction of the sodium hydroxide solution is 10%; the mass ratio of the zirconium carbide powder to the sodium hydroxide solution is 1:20.
Dispersing the zirconium carbide activation product in deionized water, dropwise adding a coupling agent KH-570, heating to 35 ℃, stirring and dispersing for 10 hours, separating out powder, washing with clear water for three times, and drying to obtain olefinized zirconium carbide;
wherein the mass ratio of the zirconium carbide activation product, the coupling agent KH-570 and the deionized water is 1:0.1:20.
S3, preparing a flame-retardant complexing agent:
dispersing olefinized zirconium carbide and a flame retardant modifier in N, N-dimethylformamide in turn, adding a small amount of azodiisobutyronitrile, heating to 50 ℃, preserving heat for 5 hours, continuously stirring during the period, filtering out a solid product after the reaction is finished, washing for three times by using absolute ethyl alcohol, and drying to obtain a flame retardant complexing agent;
wherein the mass ratio of the olefinized zirconium carbide to the flame retardant modifier to the N, N-dimethylformamide is 1:0.2:30; the addition amount of the azodiisobutyronitrile is 1 percent of the mass of the olefin zirconium carbide.
The preparation method of the flame-retardant waterproof bus duct comprises the following steps:
step 1, preventing bus copper bars from being fixed in corresponding positions in a pre-prepared mold;
step 2, uniformly mixing the epoxy resin, the fireproof filler and the flame-retardant complexing agent in the casting rubber material component, uniformly mixing with the curing agent, and then injecting into the die in the step 2;
and 3, drying the cast die in an oven at 130 ℃ for 5 hours, cooling to normal temperature, and removing the die to obtain the refractory bus duct.
Example 3
The flame-retardant waterproof bus duct comprises casting rubber, wherein the casting rubber comprises the following components in parts by weight:
70 parts of glycidol amine epoxy resin AG-80, 30 parts of fireproof filler, 28 parts of flame retardant complexing agent and 35 parts of curing agent m-phenylenediamine.
The preparation process of the fireproof filler comprises the following steps:
placing inorganic filler in ethanol water solution with the mass fraction of 50%, uniformly dispersing by ultrasonic, dripping a coupling agent KH570, heating to reflux, stirring for 12h, centrifuging to obtain solid particles, flushing with purified water for three times, and drying in a 100 ℃ oven to obtain the filler; wherein the mass ratio of the inorganic filler to the coupling agent KH570 to the ethanol aqueous solution is 1:0.15:10; the inorganic filler is kaolinite powder; the particle size of the inorganic filler is 10-20 μm.
The preparation method of the flame retardant additive comprises the following steps:
s1, preparation of a flame retardant modifier:
mixing 2-hydroxy phosphoric acid base acetic acid and absolute ethyl alcohol in a reaction bottle, building the reaction bottle on an electric heating sleeve provided with a stirrer, heating the electric heating sleeve to 55 ℃, stirring until the electric heating sleeve is completely dissolved, gradually adding 2, 4-diamino-6-dien-propylamino-1, 3, 5-triazine in half an hour, heating the electric heating sleeve to 80 ℃, carrying out heat preservation and reflux reaction for 6 hours, and sequentially carrying out centrifugal separation, washing and drying to obtain the flame retardant modifier;
wherein the mass ratio of the 2-hydroxyphosphoryl acetic acid to the 2, 4-diamino-6-diallylamino-1, 3, 5-triazine to the absolute ethyl alcohol is 3.12:4.12:150.
S2, olefination treatment of zirconium carbide:
dispersing zirconium carbide powder in a sodium hydroxide solution, stirring for 8 hours at 55 ℃, separating out the powder, washing to be neutral by using clear water, and drying to obtain a zirconium carbide activated product;
wherein the grain diameter of the zirconium carbide powder is 30-50 mu m, and the mass fraction of the sodium hydroxide solution is 20%; the mass ratio of the zirconium carbide powder to the sodium hydroxide solution is 1:40.
Dispersing the zirconium carbide activation product in deionized water, dropwise adding a coupling agent KH-570, heating to 45 ℃, stirring and dispersing for 20 hours, separating out powder, washing with clear water for three times, and drying to obtain olefinized zirconium carbide;
wherein the mass ratio of the zirconium carbide activation product, the coupling agent KH-570 and the deionized water is 1:0.3:40.
S3, preparing a flame-retardant complexing agent:
dispersing olefinized zirconium carbide and a flame retardant modifier in N, N-dimethylformamide in turn, adding a small amount of azodiisobutyronitrile, heating to 70 ℃, preserving heat for 10 hours, continuously stirring during the period, filtering out a solid product after the reaction is finished, washing for three times by using absolute ethyl alcohol, and drying to obtain a flame retardant complexing agent;
wherein the mass ratio of the olefinized zirconium carbide to the flame retardant modifier to the N, N-dimethylformamide is 1:0.6:50; the addition amount of the azodiisobutyronitrile is 2 percent of the mass of the olefin zirconium carbide.
The preparation method of the flame-retardant waterproof bus duct comprises the following steps:
step 1, preventing bus copper bars from being fixed in corresponding positions in a pre-prepared mold;
step 2, uniformly mixing the epoxy resin, the fireproof filler and the flame-retardant complexing agent in the casting rubber material component, uniformly mixing with the curing agent, and then injecting into the die in the step 2;
and step 3, placing the cast die into a baking oven at 150 ℃ for drying treatment for 3 hours, and removing the die after cooling to normal temperature to obtain the refractory bus duct.
Comparative example 1
A casting compound for a flame-retardant waterproof bus duct is different from that of example 1 in that a commercially available 2-hydroxyphosphoryl acetic acid is used as a flame-retardant complexing agent. The remaining ingredients and preparation method were the same as in example 1.
60 parts of glycidol amine epoxy resin AG-80, 25 parts of fireproof filler, 21 parts of flame retardant complexing agent and 30 parts of curing agent 4,4' -diaminodiphenyl methane.
Comparative example 2
A casting compound for a flame-retardant waterproof bus duct is different from example 1 in that 2, 4-diamino-6-diallylamino-1, 3, 5-triazine is used as a flame-retardant complexing agent. The remaining ingredients and preparation method were the same as in example 1.
60 parts of glycidol amine epoxy resin AG-80, 25 parts of fireproof filler, 21 parts of flame retardant complexing agent and 30 parts of curing agent 4,4' -diaminodiphenyl methane.
Comparative example 3
A casting compound for a flame-retardant waterproof bus duct is different from example 1 in that a compound of 2-hydroxyphosphoryl acetic acid and 2, 4-diamino-6-diallylamino-1, 3, 5-triazine is used as a flame-retardant complexing agent, and the mass ratio of 2-hydroxyphosphoryl acetic acid to 2, 4-diamino-6-diallylamino-1, 3, 5-triazine is 2.34:3.09. The remaining ingredients and preparation method were the same as in example 1.
60 parts of glycidol amine epoxy resin AG-80, 25 parts of fireproof filler, 21 parts of flame retardant complexing agent and 30 parts of curing agent 4,4' -diaminodiphenyl methane.
Experimental detection
For the performance test comparison of the casting compounds prepared in example 1 and comparative examples 1 to 3, the tests included strength, water resistance and fire resistance, tensile strength test standard GB/T1040.1, fire resistance test standard GB/T2406, fire resistance test standard GA/T537-2005 (sample treated at 1100 ℃, record fire resistance time without burning and with complete circuit, time on a per 10min basis), water impermeability test standard GB/T23445 (0.5 MPa,30 min).
The test results are shown in Table 1.
Table 1 comparison of the performance of the casting compounds
Example 1 | Comparative example 1 | Comparative example 2 | Comparative example 3 | |
Tensile Strength (MPa) | 88 | 75 | 73 | 75 |
Limiting Oxygen Index (LOI) | 37 | 31 | 34 | 33 |
Refractory time (min) | 200 | 170 | 180 | 180 |
Impermeability to water | Qualified product | Qualified product | Qualified product | Qualified product |
As can be seen from table 1, compared with the conventional flame retardant, the casting compound of example 1 has good waterproof property, high strength, good flame retardant effect and good fire resistance, and is suitable for bus ducts requiring waterproof and flame retardance and high strength requirements.
In the description of the present specification, a description referring to terms "one embodiment," "some embodiments," "examples," "specific examples," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms should not be understood as necessarily being directed to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Further, one skilled in the art can engage and combine the different embodiments or examples described in this specification.
While embodiments of the present invention have been shown and described above, it will be understood that the above embodiments are illustrative and not to be construed as limiting the invention, and that variations, modifications, alternatives and variations may be made to the above embodiments by one of ordinary skill in the art within the scope of the invention.
Claims (10)
1. The flame-retardant waterproof bus duct is characterized by comprising a casting rubber material, wherein the casting rubber material comprises the following components in parts by weight:
50-70 parts of epoxy resin, 20-30 parts of fireproof filler, 14-28 parts of flame-retardant complexing agent and 25-35 parts of curing agent;
the flame-retardant complexing agent is prepared by combining 2-hydroxy-phosphoric acid-acetic acid and 2, 4-diamino-6-diallylamino-1, 3, 5-triazine to obtain a flame-retardant modifier, and polymerizing the flame-retardant modifier and olefinized zirconium carbide.
2. The flame-retardant waterproof bus duct of claim 1, wherein the epoxy resin is a glycidylamine epoxy resin, and the type comprises AG-80 or AFG-90.
3. A flame retardant and waterproof bus duct according to claim 1, characterized in that the fireproof filler is a product of an inorganic filler subjected to an activation treatment of a coupling agent KH 570; the inorganic filler comprises one or more of quartz powder, mica powder, pyroxene powder, calcite powder, kaolinite powder and talcum powder; the particle size of the inorganic filler is 10-20 μm.
4. The flame-retardant waterproof bus duct of claim 1, wherein the curing agent is an aromatic polyamine curing agent comprising any one or a combination of more of 4,4 '-diaminodiphenylmethane, 4' -diaminodiphenylsulfone and m-phenylenediamine.
5. The flame-retardant waterproof bus duct of claim 1, wherein the flame-retardant additive is prepared by the following method:
s1, preparation of a flame retardant modifier:
mixing 2-hydroxy phosphoric acid base acetic acid and absolute ethyl alcohol in a reaction bottle, building the reaction bottle on an electric heating sleeve provided with a stirrer, heating the electric heating sleeve to 45-55 ℃, stirring until the electric heating sleeve is completely dissolved, gradually adding 2, 4-diamino-6-diallylamino-1, 3, 5-triazine in half an hour, heating the electric heating sleeve to 70-80 ℃, carrying out heat preservation reflux reaction for 4-6 hours, and sequentially carrying out centrifugal separation, washing and drying to obtain the flame retardant modifier;
s2, olefination treatment of zirconium carbide:
dispersing zirconium carbide powder in a sodium hydroxide solution, stirring for 4-8 hours at 45-55 ℃, separating out the powder, washing to be neutral by using clear water, and drying to obtain a zirconium carbide activated product;
dispersing the zirconium carbide activation product in deionized water, dropwise adding a coupling agent KH-570, heating to 35-45 ℃, stirring and dispersing for 10-20 hours, separating out powder, washing with clear water for three times, and drying to obtain olefinized zirconium carbide;
s3, preparing a flame-retardant complexing agent:
dispersing olefine zirconium carbide and flame retardant modifier in N, N-dimethyl formamide successively, adding small amount of azo initiator, heating to 50-70 deg.c, maintaining for 5-10 hr while stirring, filtering to obtain solid product, washing with absolute alcohol for three times, and drying to obtain flame retardant compounding agent.
6. The flame-retardant waterproof bus duct according to claim 5, wherein in the S1, the mass ratio of the 2-hydroxyphosphoryl acetic acid, the 2, 4-diamino-6-diallylamino-1, 3, 5-triazine and the absolute ethyl alcohol is 1.56-3.12:2.06-4.12:100-200.
7. The flame-retardant waterproof bus duct according to claim 5, wherein in the S2, the grain diameter of the zirconium carbide powder is 30-50 μm, and the mass fraction of the sodium hydroxide solution is 10% -20%; the mass ratio of the zirconium carbide powder to the sodium hydroxide solution is 1:20-40.
8. The flame-retardant waterproof bus duct according to claim 5, wherein in S2, the mass ratio of the zirconium carbide activation product, the coupling agent KH-570 and the deionized water is 1:0.1-0.3:20-40.
9. The flame-retardant waterproof bus duct according to claim 1, wherein in the S3, the mass ratio of the olefinized zirconium carbide, the flame-retardant modifier and the N, N-dimethylformamide is 1:0.2-0.6:30-50; in the step S3, the azo initiator is azodiisobutyronitrile, and the addition amount is 1-2% of the mass of the olefinized zirconium carbide.
10. A method for preparing the flame-retardant waterproof bus duct of claim 1, comprising the steps of:
step 1, preventing bus copper bars from being fixed in corresponding positions in a pre-prepared mold;
step 2, uniformly mixing the epoxy resin, the fireproof filler and the flame-retardant complexing agent in the casting rubber material component, uniformly mixing with the curing agent, and then injecting into the die in the step 2;
and step 3, placing the cast mould into a baking oven at 130-150 ℃ for drying treatment for 3-5 hours, and removing the mould after cooling to normal temperature to obtain the refractory bus duct.
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