CN110183761A - A kind of preparation method of flame retardant type cable material - Google Patents
A kind of preparation method of flame retardant type cable material Download PDFInfo
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- CN110183761A CN110183761A CN201910512579.2A CN201910512579A CN110183761A CN 110183761 A CN110183761 A CN 110183761A CN 201910512579 A CN201910512579 A CN 201910512579A CN 110183761 A CN110183761 A CN 110183761A
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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
- 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
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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
- H01B3/441—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 alkenes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/328—Phosphates of heavy metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Insulated Conductors (AREA)
- Fireproofing Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of preparation method of flame retardant type cable material, raw material forms by weight: parts by weight composition: 80-100 parts of flyash, 35-40 parts of phosphoric acid hydrogen zirconium, 15-20 parts of ethyl acrylate, 2-4 parts of silane, 1-2 parts of Aluminate, 0.1-0.5 parts of titanate esters, 100-130 parts of deionized water, 1-6 parts of dehydrated alcohol, 1-3 parts of linear paraffin benzene sulfonic acid sodium salt, 80-100 parts of polyethylene, 8-13 parts of crosslinking agent, 4-8 parts of antioxidant, 4-8 parts of polyethylene wax, 3-5 parts of zinc stearate.Cable material prepared by the present invention can significantly improve the flame retardant effect of CABLE MATERIALS using alkalization flyash and modified phosphate hydrogen zirconium after compound, and flyash is as a kind of industrial solid wastes, flame-retardant composition for CABLE MATERIALS is both economically and environmentally beneficial, has broad application prospects.
Description
Technical field
The present invention relates to a kind of preparation methods of flame retardant type cable material, belong to cable machinery field.
Background technique
Cross-linked polyolefin uses the development of many years as cable insulation material, but polyethylene belongs to combustible material,
The twisted polyethylene cable material product of produced in conventional processes does not all have flame retardant property.Tradition uses aluminium hydroxide as fire-retardant
Filler influences the processing performance and surface smoothness of cable since dosage is larger, in order to meet the demand for security of prevention fire,
Exploitation flame retardant type cable material is of great significance.Flyash is at low cost as a kind of waste material, has certain flame-retarding characteristic, but
Its flame retardant property is limited, is more for the purpose of filler, how about playing the bigger flame retardant property of flyash is highly desirable.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of flame retardant type cable material, the material prepared by this method
With excellent flame retardant effect.
A kind of preparation method of flame retardant type cable material, it is characterised in that method includes the following steps:
100 parts of flyash are placed in 300 r/min ball milling of planetary ball mill, 10 min by step 1, be subsequently added to 500 parts it is dense
It spends in the sodium hydroxide solution of 0.3mol/L, 80 DEG C of magnetic agitation 2h, filtration washing, 60 DEG C of oven dryings, obtains alkalization fine coal
Ash；
Step 2 takes 40 parts of phosphoric acid hydrogen zirconiums to be added in 200 parts of deionized water beakers, is placed in constant temperature water bath, at 40 DEG C and
Pre-dispersed 30min under 300rpm revolving speed；
10 parts of ethyl acrylate is slowly added dropwise in step 3, Xiang Shangshu dispersion liquid, continues to stir after being added dropwise, insulation reaction
60min；
Step 4, end of reaction filter to obtain wet gel layer, are transferred in vacuum oven, and dry 5h, grinding obtain at 80 DEG C
Modified phosphate hydrogen zirconium powder body；
3 parts of silane, 1.6 parts of Aluminates, 0.4 part of titanate coupling agent are poured into beaker by step 5, and 20 parts of deionized waters, 4 are added
Part dehydrated alcohol, 80 DEG C of hydrolysis 10min must compound coupling agent；
Step 6 continuously adds 100 parts of deionized waters, 1.5 parts of linear paraffin benzene sulfonic acid sodium salts and 80 parts into above-mentioned compounding coupling agent
Alkalize coal ash and 20 parts of modified phosphate hydrogen zirconium powder bodies, and suction filtration, washing after 15min are reacted at 80 DEG C, and 50 DEG C of 24 h of oven drying are obtained
To composite flame-proof powder；
Step 7 weighs 200 parts of polyethylene, 45 parts of composite flame-proof powders, 9 parts of crosslinking agents, 6 parts of antioxidants, 5 parts by weight
Polyethylene wax and 3 parts of zinc stearates put into high-speed mixer, are stirred 30min blowing；
Step 8 puts into above-mentioned mixture in screw extruder, and extruding pelletization, temperature is controlled at 140 DEG C, finally in injection molding machine
On standard batten is made, under room temperature place 72h after be tested for the property.
The utility model has the advantages that flame retardant type cable material prepared by the present invention, using alkalization flyash and modified phosphate hydrogen zirconium powder body
Compound to obtain fire-retardant powder, composite flame-retardant agent is based on, and supplemented by phosphoric acid hydrogen zirconium, price is more cheap.Phosphoric acid hydrogen zirconium passes through nanometer
Grade ethyl acrylate modification post-tensioning has arrived the interlamellar spacing of laminate, can effectively be embedded in alkalization flyash, pass through phosphoric acid hydrogen zirconium layer
Hydroxyl inside and outside plate and alkalization fine coal gray surface form stable hydrogen bond structure, compared to single flyash and phosphoric acid hydrogen zirconium,
Fire-retardant powder heat resistance after compound significantly improves, and in cable fuel combustion process, fire-retardant powder can be in polythene material table
Face quickly forms layer of charcoal and molten state substance, completely cuts off air, hinders heat transmitting, significantly improves the flame retardant effect of CABLE MATERIALS.In addition,
The hydroxyl condensation of silicone hydroxyl, aluminium hydroxyl, titanium hydroxyl and composite powder surface on compounding coupling agent, forms coupling agent clad,
Hot transmitting and the diffusion of oxygen have been obstructed, has effectively delayed and prevents the thermal degradation of polymer, it is suppressed that volatile combustible group
The generation divided.Flyash is as a kind of industrial solid wastes, and the flame-retardant composition for CABLE MATERIALS reduces the dosage of fire retardant, both
It is economical and environmentally friendly, it has broad application prospects.
Specific embodiment
Embodiment 1
A kind of preparation method of flame retardant type cable material, it is characterised in that method includes the following steps:
100 parts of flyash are placed in 300 r/min ball milling of planetary ball mill, 10 min by step 1, be subsequently added to 500 parts it is dense
It spends in the sodium hydroxide solution of 0.3mol/L, 80 DEG C of magnetic agitation 2h, filtration washing, 60 DEG C of oven dryings, obtains alkalization fine coal
Ash；
Step 2 takes 40 parts of phosphoric acid hydrogen zirconiums to be added in 200 parts of deionized water beakers, is placed in constant temperature water bath, at 40 DEG C and
Pre-dispersed 30min under 300rpm revolving speed；
10 parts of ethyl acrylate is slowly added dropwise in step 3, Xiang Shangshu dispersion liquid, continues to stir after being added dropwise, insulation reaction
60min；
Step 4, end of reaction filter to obtain wet gel layer, are transferred in vacuum oven, and dry 5h, grinding obtain at 80 DEG C
Modified phosphate hydrogen zirconium powder body；
3 parts of silane, 1.6 parts of Aluminates, 0.4 part of titanate coupling agent are poured into beaker by step 5, and 20 parts of deionized waters, 4 are added
Part dehydrated alcohol, 80 DEG C of hydrolysis 10min must compound coupling agent；
Step 6 continuously adds 100 parts of deionized waters, 1.5 parts of linear paraffin benzene sulfonic acid sodium salts and 80 parts into above-mentioned compounding coupling agent
Alkalize coal ash and 20 parts of modified phosphate hydrogen zirconium powder bodies, and suction filtration, washing after 15min are reacted at 80 DEG C, and 50 DEG C of 24 h of oven drying are obtained
To composite flame-proof powder；
Step 7 weighs 200 parts of polyethylene, 45 parts of composite flame-proof powders, 9 parts of crosslinking agents, 6 parts of antioxidants, 5 parts by weight
Polyethylene wax and 3 parts of zinc stearates put into high-speed mixer, are stirred 30min blowing；
Step 8 puts into above-mentioned mixture in screw extruder, and extruding pelletization, temperature is controlled at 140 DEG C, finally in injection molding machine
On standard batten is made.15.6 MPa of tensile strength, testing standard GB/T 1040.3-2006, elongation at break test mark
550% GB/T 1040.3-2006 of standard, limit oxygen index 39.1%.
Flyash used in the present invention is Industrial Solid Waste-flyash, and average grain diameter is 2.5 microns, and quality group becomes:
The Al2O3 of 32.4 %, 8.2% CaO, 4.3% Fe2O3,2.3% MgO, surplus SiO2.
Embodiment 2
Step 5 weighs 200 parts of polyethylene, 35 parts of composite flame-proof powders, 9 parts of crosslinking agents, 6 parts of antioxidants, 5 parts by weight
Polyethylene wax and 3 parts of zinc stearates put into high-speed mixer, are stirred 30min blowing；Remaining preparation and embodiment 1 are identical.
Embodiment 3
Step 5 weighs 200 parts of polyethylene, 40 parts of composite flame-proof powders, 9 parts of crosslinking agents, 6 parts of antioxidants, 5 parts by weight
Polyethylene wax and 3 parts of zinc stearates put into high-speed mixer, are stirred 30min blowing；Remaining preparation and embodiment 1 are identical.
Reference examples 1
It is with 1 difference of embodiment: in the step 6 of cable material preparation, 40 parts of alkalization coal ash and 60 parts of modified phosphates is added
Hydrogen zirconium powder body, remaining step are identical with embodiment 1.
Reference examples 2
It is with 1 difference of embodiment: in the step 6 of cable material preparation, 50 parts of alkalization coal ash and 50 parts of modified phosphates is added
Hydrogen zirconium powder body, remaining step are identical with embodiment 1.
Reference examples 3
It is with 1 difference of embodiment: in the step 7 of cable material preparation, replaces composite flame-proof powder to add with equivalent flyash
Enter to high-speed mixer, extruding pelletization.
Reference examples 4
A kind of preparation method of flame retardant type cable material, it is characterised in that method includes the following steps:
100 parts of flyash are placed in 300 r/min ball milling of planetary ball mill, 10 min by step 1, be subsequently added to 500 parts it is dense
It spends in the sodium hydroxide solution of 0.3mol/L, 80 DEG C of magnetic agitation 2h, filtration washing, 60 DEG C of oven dryings, obtains alkalization fine coal
Ash；
3 parts of silane, 1.6 parts of Aluminates, 0.4 part of titanate coupling agent are poured into beaker by step 2, and 20 parts of deionized waters, 4 are added
Part dehydrated alcohol, 80 DEG C of hydrolysis 10min must compound coupling agent；
Step 3 continuously adds 100 parts of deionized waters, 1.5 parts of linear paraffin benzene sulfonic acid sodium salts and 80 parts into above-mentioned compounding coupling agent
Alkalize coal ash and 20 parts of ammonium dihydrogen phosphates, suction filtration, washing after 15min is reacted at 80 DEG C, 50 DEG C of 24 h of oven drying obtain compound
Fire-retardant powder；
Step 4 weighs 200 parts of polyethylene, 45 parts of composite flame-proof powders, 9 parts of crosslinking agents, 6 parts of antioxidants, 5 parts by weight
Polyethylene wax and 3 parts of zinc stearates put into high-speed mixer, are stirred 30min blowing；
Step 5 puts into above-mentioned mixture in screw extruder, and extruding pelletization, temperature is controlled at 140 DEG C, finally in injection molding machine
On standard batten is made.
It chooses the cable material that is prepared and carries out flame retardant property detection respectively, referring to GB/T2406.2-2009 standard,
It is tested on JF-3 type oxygen index (OI) tester.
Test result
| Limit oxygen index (%) | |
| Embodiment 1 | 39.1 |
| Embodiment 2 | 38.4 |
| Embodiment 3 | 39.3 |
| Reference examples 1 | 30.6 |
| Reference examples 2 | 31.5 |
| Reference examples 3 | 20.1 |
| Reference examples 4 | 26.7 |
The experimental results showed that cable material provided by the invention has excellent flame retardant effect, reference examples 1 and reference examples 2 are changed
Alkalize flyash and modified phosphate hydrogen zirconium powder body ratio, and total amount is unchanged, and limit oxygen index reduces, and illustrates modified phosphate hydrogen zirconium powder body
Usage ratio cannot be excessive, otherwise influence it is compound after material flame retardant property；Control 3 is made with the non-modified flyash of equivalent
For flame-retardant composition, flame retardant effect is unsatisfactory, illustrates by the modified resistance for improving high molecular polymer of composite flame-proof powder
Combustion property.
Comparative example substitutes modified phosphate hydrogen zirconium powder using ammonium dihydrogen phosphate, and effect can not show a candle to modified phosphate hydrogen zirconium powder.
Claims (8)
1. a kind of preparation method of flame retardant type cable material, which is characterized in that including following raw material:
By weight form: 80-100 parts of flyash, 35-40 parts of phosphoric acid hydrogen zirconium, 15-20 parts of ethyl acrylate, 2-4 parts of silane,
1-2 parts of Aluminate, 0.1-0.5 parts of titanate esters, 100-130 parts of deionized water, 1-6 parts of dehydrated alcohol, linear paraffin benzene sulfonic acid sodium salt
1-3 parts, 80-100 parts of polyethylene, 8-13 parts of crosslinking agent, 4-8 parts of antioxidant, 4-8 parts of polyethylene wax, 3-5 parts of zinc stearate.
2. a kind of preparation method of flame retardant type cable material according to claim 1, which is characterized in that including walking in detail below
It is rapid:
Flyash is placed in planetary ball mill 300-350 r/min ball milling 10-15 min by step 1, and it is molten to be subsequently added to highly basic
In liquid, 70-80 DEG C of magnetic agitation 1-2h, filtration washing, 60 DEG C of oven dryings, obtain alkalization flyash；
Phosphoric acid hydrogen zirconium is added in deionized water beaker step 2, is placed in constant temperature water bath, in 40-45 DEG C and 300-
Pre-dispersed 25-30min under 350rpm revolving speed；
Ethyl acrylate is slowly added dropwise in step 3, Xiang Shangshu dispersion liquid, continues to stir after being added dropwise, insulation reaction 50-
60min；
Step 4, end of reaction filter to obtain wet gel layer, are transferred in vacuum oven, and dry 4-5h, grinds at 70-80 DEG C
Mill obtains modified phosphate hydrogen zirconium powder body；
Silane, Aluminate, titanate coupling agent are poured into beaker by step 5, and deionized water, dehydrated alcohol, 80-85 DEG C of water is added
Solution 10-15min must compound coupling agent；
Step 6 continuously adds deionized water, linear paraffin benzene sulfonic acid sodium salt, alkalization coal ash and modification into above-mentioned compounding coupling agent
Phosphoric acid hydrogen zirconium powder body, react at 80-85 DEG C filter after 15-20min, washing, oven drying obtains composite flame-proof powder；
Step 7 weighs polyethylene, composite flame-proof powder, crosslinking agent, antioxidant, polyethylene wax and zinc stearate by weight
High-speed mixer is put into, 30-40min blowing is stirred；
Step 8 puts into above-mentioned mixture in double screw extruder, and extruding pelletization, temperature is controlled at 140-170 DEG C, is finally existed
Standard batten is made on injection molding machine, is tested for the property after placing 72h under room temperature.
3. a kind of preparation method of flame retardant type cable material according to claim 1, which is characterized in that strong in the step 1
Aqueous slkali is the sodium hydroxide solution or potassium hydroxide solution of concentration 0.3-0.5mol/L.
4. a kind of preparation method of flame retardant type cable material according to claim 1, which is characterized in that aluminium in the step 5
Acid esters is three benzyl ester of three isopropyl ester of aluminic acid or chloric acid.
5. a kind of preparation method of flame retardant type cable material according to claim 1, which is characterized in that titanium in the step 5
Acid esters is three isostearic acid isopropyl titanates.
6. a kind of preparation method of flame retardant type cable material according to claim 1, which is characterized in that straight in the step 6
Alkane benzene sulfonic acid sodium salt is neopelex or butyl sulfonic acid sodium.
7. a kind of preparation method of flame retardant type cable material according to claim 1, which is characterized in that resist in the step 7
Oxidant is a kind of in preferably 1010,1035 and 168 models.
8. a kind of preparation method of flame retardant type cable material according to claim 1, which is characterized in that handed in the step 7
Joining agent is preferably cumyl peroxide or peroxidating ethane.
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| CN201910512579.2A CN110183761A (en) | 2019-06-13 | 2019-06-13 | A kind of preparation method of flame retardant type cable material |
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| CN201910512579.2A CN110183761A (en) | 2019-06-13 | 2019-06-13 | A kind of preparation method of flame retardant type cable material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112321903A (en) * | 2020-12-03 | 2021-02-05 | 宿松晨辉塑料制品有限公司 | Biodegradable composite plastic production process |
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2019
- 2019-06-13 CN CN201910512579.2A patent/CN110183761A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112321903A (en) * | 2020-12-03 | 2021-02-05 | 宿松晨辉塑料制品有限公司 | Biodegradable composite plastic production process |
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