CN108794853A - A kind of preparation method of flame retardant flexible heat-shrinkable T bush - Google Patents
A kind of preparation method of flame retardant flexible heat-shrinkable T bush Download PDFInfo
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- CN108794853A CN108794853A CN201810478851.5A CN201810478851A CN108794853A CN 108794853 A CN108794853 A CN 108794853A CN 201810478851 A CN201810478851 A CN 201810478851A CN 108794853 A CN108794853 A CN 108794853A
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- shrinkable
- heat
- bush
- flame retardant
- temperature
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 28
- 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 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 235000014676 Phragmites communis Nutrition 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 29
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical class [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 claims abstract description 24
- 229920001971 elastomer Polymers 0.000 claims abstract description 22
- 150000001875 compounds Chemical class 0.000 claims abstract description 19
- 239000000835 fiber Substances 0.000 claims abstract description 15
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 14
- 229920001903 high density polyethylene Polymers 0.000 claims abstract description 14
- 239000004700 high-density polyethylene Substances 0.000 claims abstract description 14
- 238000002844 melting Methods 0.000 claims abstract description 14
- 230000008018 melting Effects 0.000 claims abstract description 14
- 229920000573 polyethylene Polymers 0.000 claims abstract description 13
- 229910001051 Magnalium Inorganic materials 0.000 claims abstract description 12
- 239000004698 Polyethylene Substances 0.000 claims abstract description 12
- -1 polyethylene Polymers 0.000 claims abstract description 12
- 238000010074 rubber mixing Methods 0.000 claims abstract description 10
- 238000010348 incorporation Methods 0.000 claims abstract description 8
- 239000008188 pellet Substances 0.000 claims abstract description 8
- 238000012545 processing Methods 0.000 claims abstract description 8
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims abstract description 7
- 239000005038 ethylene vinyl acetate Substances 0.000 claims abstract description 5
- 239000000725 suspension Substances 0.000 claims description 22
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 14
- 238000003828 vacuum filtration Methods 0.000 claims description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 239000000706 filtrate Substances 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 12
- 239000006185 dispersion Substances 0.000 claims description 9
- 230000005855 radiation Effects 0.000 claims description 8
- QCMYYKRYFNMIEC-UHFFFAOYSA-N COP(O)=O Chemical class COP(O)=O QCMYYKRYFNMIEC-UHFFFAOYSA-N 0.000 claims description 7
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 7
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 6
- 239000005977 Ethylene Substances 0.000 claims description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 6
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000000748 compression moulding Methods 0.000 claims description 6
- 238000005286 illumination Methods 0.000 claims description 6
- 239000011591 potassium Substances 0.000 claims description 6
- 229910052700 potassium Inorganic materials 0.000 claims description 6
- 239000011265 semifinished product Substances 0.000 claims description 6
- 229920002379 silicone rubber Polymers 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000003760 magnetic stirring Methods 0.000 claims description 5
- 238000004073 vulcanization Methods 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 239000000454 talc Substances 0.000 claims description 2
- 229910052623 talc Inorganic materials 0.000 claims description 2
- 239000003643 water by type Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 1
- 229910001701 hydrotalcite Inorganic materials 0.000 abstract description 7
- 229960001545 hydrotalcite Drugs 0.000 abstract description 7
- 229920002522 Wood fibre Polymers 0.000 abstract description 4
- 239000011229 interlayer Substances 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract description 4
- 150000001450 anions Chemical class 0.000 abstract description 2
- 238000002485 combustion reaction Methods 0.000 abstract description 2
- 238000006114 decarboxylation reaction Methods 0.000 abstract description 2
- 238000002955 isolation Methods 0.000 abstract description 2
- 229920005610 lignin Polymers 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 11
- 238000000034 method Methods 0.000 description 9
- 238000009413 insulation Methods 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000009830 intercalation Methods 0.000 description 3
- 230000002687 intercalation Effects 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- BFMKFCLXZSUVPI-UHFFFAOYSA-N ethyl but-3-enoate Chemical compound CCOC(=O)CC=C BFMKFCLXZSUVPI-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- IIVCYFSRDZBYCV-UHFFFAOYSA-N C(CCCCCCCCCCC)[P] Chemical compound C(CCCCCCCCCCC)[P] IIVCYFSRDZBYCV-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229940030225 antihemorrhagics Drugs 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000000025 haemostatic effect Effects 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000011490 mineral wool Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229920000431 shape-memory polymer Polymers 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- GAJQCIFYLSXSEZ-UHFFFAOYSA-N tridecyl dihydrogen phosphate Chemical class CCCCCCCCCCCCCOP(O)(O)=O GAJQCIFYLSXSEZ-UHFFFAOYSA-N 0.000 description 1
- 210000005239 tubule Anatomy 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
- B29C59/16—Surface shaping of articles, e.g. embossing; Apparatus therefor by wave energy or particle radiation, e.g. infrared heating
- B29C59/165—Surface shaping of articles, e.g. embossing; Apparatus therefor by wave energy or particle radiation, e.g. infrared heating of profiled articles, e.g. hollow or tubular articles
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- 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
- C08L2203/18—Applications used for pipes
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Toxicology (AREA)
- Physics & Mathematics (AREA)
- Oral & Maxillofacial Surgery (AREA)
- Thermal Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
Abstract
The present invention relates to tubing preparing technical fields, and in particular to a kind of preparation method of flame retardant flexible heat-shrinkable T bush.The present invention is by reed powder, organically-modified hydrotalcite, ethyl acetate is mixed to get lifeless thing fiber, high density polyethylene (HDPE) masterbatch pellet is put into melting in rubber mixing machine, mix lifeless thing fiber, obtain rubber compound, rubber compound is transferred to mixer, incorporation ethylene-vinyl acetate copolymer obtains flame retardant flexible heat-shrinkable T bush through processing, lignin is adsorbed in fiber surface and hole, enhance the interface binding power between wood fibre and polyethylene, to make heat-shrinkable T bush become softness rich in toughness, heat-shrinkable T bush is in combustion, make magnalium hydrotalcite that can lose interlayer hydrone and interlayer anion, also occur that decarboxylation reaction, play the role of protecting polymer and air-isolation, to improve heat-shrinkable T bush flame retardant property, it has a extensive future.
Description
Technical field
The present invention relates to tubing preparing technical fields, and in particular to a kind of preparation method of flame retardant flexible heat-shrinkable T bush.
Background technology
Heat-shrinkable T bush also known as thermal contraction protection sleeve pipe, insulation protection is provided for electric wire, cable or wire end.Due to heat
Heat-Shrinkable Tubings have many advantages, such as that high-temperature shrinkage, soft fire-retardant, insulation corrosion protection, the insulation for being widely used in various harness, solder joint, inductance are protected
Shield and metal tube, the antirust of stick, corrosion protection etc..It, on the one hand can be to electronic component as the exterior insulation clad of these elements
It is effectively protected, and on the one hand can indicate the information of electronic component on the surface of heat-shrink tube in order to identify.
The common method for preparing material contracting with heat has radiation cross-linking process, peroxide crosslinking method, silane cross-linking method, copolymerization method
Deng.Material contracting with heat is frequently utilized for automobile industry（Pyrocondensation tubule, double-wall pipe, environmentally friendly heat-shrink tube）, power industry（High-tension cable is attached
Part, mesolow cable accessory, pyrocondensation insulation bus-bar casing tube）, medical equipment（Haemostatic clamp, orthopaedics fix material）, packaging material（Heat
Contracting packing film, pyrocondensation trade mark）, pipeline transportation（Thermal shrinkable sleeve, pyrocondensation repaire belt, pyrocondensation covering piece）, military industry（Reducing socket
Set, radar cable protective sleeve）In.
When electronic apparatus occasion uses heat-shrinkable T bush, heat-shrinkable T bush is sleeved on metal exemplar（Aluminium or copper or metal alloy）
Outer layer shields, and usually carries out heat shrink with large-scale oven heat or continuous tunnel furnace.However, using heat-shrinkable T bush in batch
When, when heat-shrinkable T bush is in high temperature process or is used in other hot environments, it is susceptible to mutual self-adhesion, or be in contact with it
Between metal material phenomena such as adhesion, influence product quality, can cause in this case it is secondary do over again, generate the waves such as artificial, material
Take, while production efficiency reduces, and brings competitive disadvantages to enterprise, influences enterprise development.In addition, there is also mechanical properties for heat-shrink tube
Inadequate defect, main reasons is that the chemical bond of shape-memory polymer is mainly covalent bond, bond energy is relatively low, and its structure
Type is complicated, is hardly formed consistent reply action, prodigious resultant force is can not form, simultaneously because the limitation of material, material contracting with heat are past
Toward not having fire-retardant performance, electrical insulation capability is poor（Discomfort is fit to do thinwalled insulation or higher voltage grade）And stress crack resistant
Poor performance.
It would therefore be highly desirable to invent the heat-shrinkable T bush that a kind of mechanical property is good, electrical insulating property is strong, temperature classification is high.
Invention content
Present invention mainly solves the technical issues of, for current heat-shrinkable T bush material based on plastics, due to the limit of material
System, material contracting with heat often do not have good flame retardant property, and heat-shrinkable T bush toughness is poor, in cable assembling process, is bending
The defect of stress cracking easily occurs for place, provides a kind of preparation method of flame retardant flexible heat-shrinkable T bush.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of flame retardant flexible heat-shrinkable T bush, it is characterised in that specifically preparation process is：
（1）600~700mL ethanol waters are added in three-necked flask, three-necked flask is transferred in water-bath, heating rises
30~35g magnalium hydrotalcites are added into three-necked flask for temperature, start magnetic stirring apparatus, are stirred 1~2h, and it is equal to obtain dispersion
Even hydrotacite suspension；
（2）70~80g onodoidecyl phosphonic acid methyl esters potassium is put into above-mentioned hydrotacite suspension, is stirred, with hydrochloric acid tune
Water-saving talc suspension pH, heat temperature raising are stirred to react, and obtain white slurries, and white slurries are placed in vacuum filtration machine and are taken out
After filter, white filter residue is washed with absolute ethyl alcohol and is placed in baking oven, has been dried to obtain by the isolated white filter residue of removal filtrate
Machine modified hydrotalcite；
（3）Reed is put into pulverizer and is crushed, sieving obtains reed powder, reed powder is placed in baking oven, heat temperature raising,
Dry, reed powder, organically-modified hydrotalcite, the ethyl acetate after drying are mixed, are placed in by the reed powder after being dried
High speed dispersor obtains dispersed paste with rotating speed 10~15min of high speed dispersion of 2000~2500r/min；
（4）Dispersed paste is placed in vacuum filtration machine and is filtered, the isolated lifeless thing fiber of filtrate is removed, takes 150~170g high
Density polyethylene masterbatch pellet is put into baking oven, heat temperature raising, after preheating, is put into the rubber mixing machine that set temperature is 160~200 DEG C
Middle melting, incorporation 60~65g lifeless things fiber, 40~50g silicon rubber, obtain rubber compound after polyethylene master batch completely melting；
（5）Rubber compound is transferred in mixer, 40~50g ethylene-vinyl acetate copolymers, mixing are mixed into rubber compound
After squeeze out into tubing die, tubing die is placed in compression molding agent and is vulcanized, demoulding obtains casing semi-finished product, then sets
The radiation treatment under ultraviolet source obtains flame retardant flexible heat-shrinkable T bush.
Step（1）The ethanol water mass fraction is 40%, and temperature is 70~80 DEG C after heat temperature raising.
Step（2）The mass fraction of the hydrochloric acid is 15%, adjusting hydrotacite suspension pH to 4~5, after heat temperature raising
Temperature is 80~90 DEG C, and it is 6~7h to be stirred to react the time, and baking oven set temperature is 90~100 DEG C, and drying time is 7~8h.
Step（3）The grinding time is 3~4h, and be sieved specification is 100 mesh, and temperature is 70~80 after heat temperature raising
DEG C, drying time is 10~12h, and the reed powder, organically-modified hydrotalcite, ethyl acetate mixing quality ratio after drying are 1 ︰, 3 ︰
10。
Step（4）Temperature is 120~130 DEG C after the baking oven heat temperature raising, and preheating time is 5~7min, rubber mixing machine
Set temperature is 160~200 DEG C.
Step（5）Ethylene mass content is 60~65% in the ethylene-vinyl acetate copolymer used, and control is close
The processing temperature of mill is 140~160 DEG C, and head rotating speed is 60~80r/min, and mixing time is 20~25min, control vulcanization
Temperature is 120~150 DEG C, and sulfide stress is 15~18MPa, and vulcanization time is 15~20min, and ultraviolet source intensity of illumination is
400~500Lx, radiation treatment time are 20~22h.
The beneficial effects of the invention are as follows：
（1）Magnalium hydrotalcite is mixed dispersion with ethanol water and obtains hydrotacite suspension by the present invention, with single dodecyl phosphorus
Sour methyl esters salt heats in acid condition with hydrotacite suspension reacts, through being filtered by vacuum, being dried to obtain organically-modified hydrotalcite,
Reed powder, organically-modified hydrotalcite, ethyl acetate are mixed, it, will through high speed dispersion, the isolated lifeless thing fiber of vacuum filtration
High density polyethylene (HDPE) masterbatch pellet is put into melting in rubber mixing machine, mixes lifeless thing fiber, obtains rubber compound, rubber compound is transferred to close
Mill mixes ethylene-vinyl acetate copolymer, and extruded, die-filling, vulcanization, radiation treatment obtain flame retardant flexible heat-shrinkable T bush,
Theoretical according to wooden powder's warm-pressing formation, lifeless thing fiber is mixed polyethylene melt by the present invention under the conditions of certain temperature, wooden
Element reaches glassy state, softens and generates flowing under high pressure, lignin has very strong adhesive force at this time, is adsorbed on fiber table
In face and hole, polyethylene is pressed closely, enhances the interface binding power between wood fibre and polyethylene, wood fibre is in casing
Radial direction can enhance the shock loading of polythene material, improve stress impact intensity, to make heat-shrinkable T bush become softness rich in tough
Property, it is not susceptible to stress cracking；
（2）Hydrotalcite grain size is smaller in the present invention, can reach nano-dispersion in the polymer, and resulting materials are really a kind of water
Talcum-Polyethylene Nanocomposites, after onodoidecyl phosphonic acid methyl esters salt is modified magnalium hydrotalcite, single dodecyl
Methyl orthophosphoric acid salt can substitute the carbanion between magnalium hydrotalcite intercalation, make the hydrophobic immersion oil of magnalium hydrotalcite intercalation, and make to insert
Interlamellar spacing increases, and is conducive to polyethylene macromolecular chain and is inserted into intercalation, forms compact composite material, thermal shrinkable sleeve of the invention
Pipe in combustion, makes magnalium hydrotalcite that can lose interlayer hydrone and interlayer anion, it also occur that decarboxylation reaction, this
A little processes will all absorb a large amount of heat while achieve the purpose that the concentration of dilution oxygen, promote polymer at charcoal, to
To the effect of protection polymer and air-isolation, the wood fibre of incorporation is under hot conditions can be charing expanded, forms carbon net,
Carbon yield rises, and exhaust smoke level declines, and to improve heat-shrinkable T bush flame retardant property, has a extensive future.
Specific implementation mode
The ethanol water that 600~700mL mass fractions are 40% is added in three-necked flask, three-necked flask is shifted
Into water-bath, after being heated to 70~80 DEG C, 30~35g magnalium hydrotalcites are added into three-necked flask, starts magnetic force and stirs
Device is mixed, 1~2h is stirred with the rotating speed of 350~400r/min, obtains finely dispersed hydrotacite suspension；By 70~80g
Onodoidecyl phosphonic acid methyl esters potassium is put into above-mentioned hydrotacite suspension, is stirred 5~10min, is 15% with mass fraction
Hydrochloric acid adjusts hydrotacite suspension pH to 4~5, is heated to 80~90 DEG C, is stirred to react 6~7h, obtains white slurries, will
White slurries are placed in vacuum filtration machine after suction filtration, the isolated white filter residue of removal filtrate, by white filter residue absolute ethyl alcohol
Washing is placed in the baking oven that set temperature is 90~100 DEG C, and dry 7~8h obtains organically-modified hydrotalcite；Reed is put into
3~4h is crushed in pulverizer, sieves with 100 mesh sieve to obtain reed powder, reed powder is placed in baking oven, is heated to 70~80
DEG C, dry 10~12h, the reed powder after being dried, by the reed powder after drying, organically-modified hydrotalcite, acetic acid second
Ester is 1 ︰ 3 ︰ 10 mixing in mass ratio, is placed in high speed dispersor, with the rotating speed high speed dispersion 10 of 2000~2500r/min~
15min obtains dispersed paste；Dispersed paste is placed in vacuum filtration machine and is filtered, the isolated lifeless thing fiber of filtrate is removed, takes
150~170g high density polyethylene (HDPE) masterbatch pellets are put into baking oven, are heated to 120~130 DEG C, after preheating 5~7min, are put
Enter melting in the rubber mixing machine that set temperature is 160~200 DEG C, 60~65g of incorporation lifeless things are fine after polyethylene master batch completely melting
Dimension, 40~50g silicon rubber, obtain rubber compound；Rubber compound is transferred in mixer, 40~50g ethylene is mixed into rubber compound
The ethylene-vinyl acetate copolymer that mass content is 60~65%, the processing temperature for controlling mixer are 140~160 DEG C, machine
Head rotating speed is 60~80r/min, is squeezed out into tubing die after 20~25min of mixing, tubing die is placed on compression molding agent
On vulcanized, control curing temperature be 120~150 DEG C, sulfide stress be 15~18MPa, vulcanize 15~20min, demould
To casing semi-finished product, then it is placed in intensity of illumination 20~22h of radiation treatment under ultraviolet source with 400~500Lx, obtained fire-retardant soft
Property heat-shrinkable T bush.
The ethanol water that 600mL mass fractions are 40% is added in three-necked flask, three-necked flask is transferred to water-bath
In pot, after being heated to 70 DEG C, 30g magnalium hydrotalcites are added into three-necked flask, start magnetic stirring apparatus, with 350r/min
Rotating speed be stirred 1h, obtain finely dispersed hydrotacite suspension；70g onodoidecyl phosphonic acid methyl esters potassium is put into above-mentioned
In hydrotacite suspension, it is stirred 5min, the hydrochloric acid for being 15% with mass fraction adjusts hydrotacite suspension pH to 4, and heating rises
Temperature is stirred to react 6h to 80 DEG C, obtains white slurries, white slurries is placed in vacuum filtration machine after filtering, removal filtrate point
From white filter residue is obtained, white filter residue is washed with absolute ethyl alcohol and is placed in the baking oven that set temperature is 90 DEG C, dry 7h is obtained
To organically-modified hydrotalcite；Reed is put into pulverizer and crushes 3h, sieves with 100 mesh sieve to obtain reed powder, reed powder is set
In baking oven, it is heated to 70 DEG C, dry 10h, the reed powder after being dried, by the reed powder, organic after drying
Modified hydrotalcite, ethyl acetate are 1 ︰, 3 ︰ 10 mixing in mass ratio, are placed in high speed dispersor, with the rotating speed high speed of 2000r/min
Disperse 10min, obtains dispersed paste；Dispersed paste is placed in vacuum filtration machine and is filtered, the isolated lifeless thing of removal filtrate is fine
Dimension, takes 150g high density polyethylene (HDPE) masterbatch pellets to be put into baking oven, is heated to 120 DEG C, after preheating 5min, is put into setting temperature
Degree is melting in 160 DEG C of rubber mixing machine, and incorporation 60g lifeless things fiber, 40g silicon rubber, obtain after polyethylene master batch completely melting
Rubber compound；Rubber compound is transferred in mixer, the ethyl vinyl acetate second that 40g Ethylene mass contents are 60% is mixed into rubber compound
Enoate copolymer, the processing temperature for controlling mixer are 140 DEG C, and head rotating speed is 60r/min, is squeezed out after mixing 20min to pipe
In formula mold, tubing die is placed in compression molding agent and is vulcanized, control curing temperature is 120 DEG C, and sulfide stress is
15MPa vulcanizes 15min, and demoulding obtains casing semi-finished product, then is placed in the intensity of illumination radiation treatment under ultraviolet source with 400Lx
20h obtains flame retardant flexible heat-shrinkable T bush.
The ethanol water that 650mL mass fractions are 40% is added in three-necked flask, three-necked flask is transferred to water-bath
In pot, after being heated to 75 DEG C, 33g magnalium hydrotalcites are added into three-necked flask, start magnetic stirring apparatus, with 375r/min
Rotating speed be stirred 1h, obtain finely dispersed hydrotacite suspension；75g onodoidecyl phosphonic acid methyl esters potassium is put into above-mentioned
In hydrotacite suspension, it is stirred 7min, the hydrochloric acid for being 15% with mass fraction adjusts hydrotacite suspension pH to 4, and heating rises
Temperature is stirred to react 6h to 85 DEG C, obtains white slurries, white slurries is placed in vacuum filtration machine after filtering, removal filtrate point
From white filter residue is obtained, white filter residue is washed with absolute ethyl alcohol and is placed in the baking oven that set temperature is 95 DEG C, dry 7h is obtained
To organically-modified hydrotalcite；Reed is put into pulverizer and crushes 3h, sieves with 100 mesh sieve to obtain reed powder, reed powder is set
In baking oven, it is heated to 75 DEG C, dry 11h, the reed powder after being dried, by the reed powder, organic after drying
Modified hydrotalcite, ethyl acetate are 1 ︰, 3 ︰ 10 mixing in mass ratio, are placed in high speed dispersor, with the rotating speed high speed of 2250r/min
Disperse 13min, obtains dispersed paste；Dispersed paste is placed in vacuum filtration machine and is filtered, the isolated lifeless thing of removal filtrate is fine
Dimension, takes 160g high density polyethylene (HDPE) masterbatch pellets to be put into baking oven, is heated to 125 DEG C, after preheating 6min, is put into setting temperature
Degree is melting in 180 DEG C of rubber mixing machine, and incorporation 63g lifeless things fiber, 45g silicon rubber, obtain after polyethylene master batch completely melting
Rubber compound；Rubber compound is transferred in mixer, the ethyl vinyl acetate second that 45g Ethylene mass contents are 63% is mixed into rubber compound
Enoate copolymer, the processing temperature for controlling mixer are 150 DEG C, and head rotating speed is 70r/min, is squeezed out after mixing 23min to pipe
In formula mold, tubing die is placed in compression molding agent and is vulcanized, control curing temperature is 135 DEG C, and sulfide stress is
17MPa vulcanizes 17min, and demoulding obtains casing semi-finished product, then is placed in the intensity of illumination radiation treatment under ultraviolet source with 450Lx
21h obtains flame retardant flexible heat-shrinkable T bush.
The ethanol water that 700mL mass fractions are 40% is added in three-necked flask, three-necked flask is transferred to water-bath
In pot, after being heated to 80 DEG C, 35g magnalium hydrotalcites are added into three-necked flask, start magnetic stirring apparatus, with 400r/min
Rotating speed be stirred 2h, obtain finely dispersed hydrotacite suspension；80g onodoidecyl phosphonic acid methyl esters potassium is put into above-mentioned
In hydrotacite suspension, it is stirred 10min, the hydrochloric acid for being 15% with mass fraction adjusts hydrotacite suspension pH to 5, heating
90 DEG C are warming up to, 7h is stirred to react, obtains white slurries, white slurries is placed in vacuum filtration machine after filtering, removes filtrate
White filter residue is washed with absolute ethyl alcohol and is placed in the baking oven that set temperature is 100 DEG C by isolated white filter residue, dry
8h obtains organically-modified hydrotalcite；Reed is put into pulverizer and crushes 4h, sieves with 100 mesh sieve to obtain reed powder, by reed powder
End is placed in baking oven, is heated to 80 DEG C, dry 12h, the reed powder after being dried, by after drying reed powder,
Organically-modified hydrotalcite, ethyl acetate are 1 ︰, 3 ︰ 10 mixing in mass ratio, high speed dispersor are placed in, with the rotating speed of 2500r/min
High speed dispersion 15min, obtains dispersed paste；Dispersed paste is placed in vacuum filtration machine and is filtered, the isolated wood of filtrate is removed
Mineral wool takes 170g high density polyethylene (HDPE) masterbatch pellets to be put into baking oven, is heated to 130 DEG C, after preheating 7min, is put into and sets
Melting in the rubber mixing machine that constant temperature degree is 200 DEG C, incorporation 65g lifeless things fiber, 50g silicon rubber after polyethylene master batch completely melting,
Obtain rubber compound；Rubber compound is transferred in mixer, ethylene-vinegar that 50g Ethylene mass contents are 65% is mixed into rubber compound
Vinyl acetate copolymer, the processing temperature for controlling mixer are 160 DEG C, and head rotating speed is 80r/min, is squeezed out after mixing 25min
Into tubing die, tubing die is placed in compression molding agent and is vulcanized, control curing temperature is 150 DEG C, sulfide stress
For 18MPa, vulcanize 20min, demoulding obtains casing semi-finished product, then is placed under ultraviolet source at the intensity of illumination irradiation of 500Lx
22h is managed, flame retardant flexible heat-shrinkable T bush is obtained.
The heat-shrinkable T bush that comparative example is produced with company of Daliang City is as a comparison case to flame retardant flexible produced by the present invention warm
Heat-shrinkable T bush in Heat-Shrinkable Tubings and comparative example is detected, and testing result is as shown in table 1：
Mechanics Performance Testing
It is tested using mechanical property tester.
Flame retardant property measures
Oxygen index (OI) is according to GB/T2406-2009《Plastics limiting oxygen index determination burning behavior part 2：Room temperature is tested》Test.
1 performance measurement result of table
From the data in table 1, it can be seen that flame retardant flexible heat-shrinkable T bush function admirable produced by the present invention, has relaxation shrinkage height, elastic memory
Characteristic is good, environmentally friendly, moisture-proof, insulation performance is good, the features such as having a safety feature and is easy to process efficient, has important market price
Value and social value.
Claims (6)
1. a kind of preparation method of flame retardant flexible heat-shrinkable T bush, it is characterised in that specifically preparation process is：
（1）600~700mL ethanol waters are added in three-necked flask, three-necked flask is transferred in water-bath, heating rises
30~35g magnalium hydrotalcites are added into three-necked flask for temperature, start magnetic stirring apparatus, are stirred 1~2h, and it is equal to obtain dispersion
Even hydrotacite suspension；
（2）70~80g onodoidecyl phosphonic acid methyl esters potassium is put into above-mentioned hydrotacite suspension, is stirred, with hydrochloric acid tune
Water-saving talc suspension pH, heat temperature raising are stirred to react, and obtain white slurries, and white slurries are placed in vacuum filtration machine and are taken out
After filter, white filter residue is washed with absolute ethyl alcohol and is placed in baking oven, has been dried to obtain by the isolated white filter residue of removal filtrate
Machine modified hydrotalcite；
（3）Reed is put into pulverizer and is crushed, sieving obtains reed powder, reed powder is placed in baking oven, heat temperature raising,
Dry, reed powder, organically-modified hydrotalcite, the ethyl acetate after drying are mixed, are placed in by the reed powder after being dried
High speed dispersor obtains dispersed paste with rotating speed 10~15min of high speed dispersion of 2000~2500r/min；
（4）Dispersed paste is placed in vacuum filtration machine and is filtered, the isolated lifeless thing fiber of filtrate is removed, takes 150~170g high
Density polyethylene masterbatch pellet is put into baking oven, heat temperature raising, after preheating, is put into the rubber mixing machine that set temperature is 160~200 DEG C
Middle melting, incorporation 60~65g lifeless things fiber, 40~50g silicon rubber, obtain rubber compound after polyethylene master batch completely melting；
（5）Rubber compound is transferred in mixer, 40~50g ethylene-vinyl acetate copolymers, mixing are mixed into rubber compound
After squeeze out into tubing die, tubing die is placed in compression molding agent and is vulcanized, demoulding obtains casing semi-finished product, then sets
The radiation treatment under ultraviolet source obtains flame retardant flexible heat-shrinkable T bush.
2. a kind of preparation method of flame retardant flexible heat-shrinkable T bush according to claim 1, it is characterised in that：Step（1）Institute
The ethanol water mass fraction stated is 40%, and temperature is 70~80 DEG C after heat temperature raising.
3. a kind of preparation method of flame retardant flexible heat-shrinkable T bush according to claim 1, it is characterised in that：Step（2）Institute
The mass fraction for the hydrochloric acid stated is 15%, adjusts hydrotacite suspension pH to 4~5, and temperature is 80~90 DEG C after heat temperature raising, is stirred
It is 6~7h to mix the reaction time, and baking oven set temperature is 90~100 DEG C, and drying time is 7~8h.
4. a kind of preparation method of flame retardant flexible heat-shrinkable T bush according to claim 1, it is characterised in that：Step（3）Institute
The grinding time stated is 3~4h, and be sieved specification is 100 mesh, and temperature is 70~80 DEG C after heat temperature raising, drying time for 10~
12h, reed powder, organically-modified hydrotalcite, ethyl acetate mixing quality ratio after drying are 1 ︰, 3 ︰ 10.
5. a kind of preparation method of flame retardant flexible heat-shrinkable T bush according to claim 1, it is characterised in that：Step（4）Institute
Temperature is 120~130 DEG C after the baking oven heat temperature raising stated, and preheating time is 5~7min, and rubber mixing machine set temperature is 160~200
℃。
6. a kind of preparation method of flame retardant flexible heat-shrinkable T bush according to claim 1, it is characterised in that：Step（5）Institute
Ethylene mass content is 60~65% in the ethylene-vinyl acetate copolymer used stated, and the processing temperature for controlling mixer is
140~160 DEG C, head rotating speed is 60~80r/min, and mixing time is 20~25min, and control curing temperature is 120~150
DEG C, sulfide stress is 15~18MPa, and vulcanization time is 15~20min, and ultraviolet source intensity of illumination is 400~500Lx, irradiation
Processing time is 20~22h.
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