CN110283454A - A kind of Low-smoke flame retardant cable material and preparation method thereof - Google Patents
A kind of Low-smoke flame retardant cable material and preparation method thereof Download PDFInfo
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- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
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Abstract
The present invention provides a kind of preparation method of Low-smoke flame retardant cable material, which comprises the steps of: step S1 mitoguazone and 1,1'- dinaphthalene -2,2'- dioctyl phthalate polycondensation, step S22- (chloromethyl) -4,4,5,5- tetramethyl -1,3,2- dioxaborolanes are grafted condensation polymer, step S3 ionization, the molding of step S4 CABLE MATERIALS.The present invention also provides the Low-smoke flame retardant cable materials being prepared according to the preparation method of the Low-smoke flame retardant cable material.The advantages of Low-smoke flame retardant cable material provided by the invention has mechanical performance and process industrial art performance good, and softness and weatherability are good, long service life and environmentally protective, low smoke and non-toxic, excellent in flame retardance.
Description
Technical field
The present invention relates to CABLE MATERIALS technical fields more particularly to a kind of Low-smoke flame retardant cable material and preparation method thereof.
Background technique
The world today, power supply field are flourished, and the indispensable a part of development of world economy is had become.And
Power cable spreads all trades and professions as the carrier of power supply, has the function of power Transmission and information conveyance, in people
It plays an important role in life and production.Since the insulating polymeric material that wire and cable uses belongs to combustible material,
Internal cause (cable self-heating, short circuit etc.) is often had in transmission power process and external cause (fire etc.) causes cable fire, it is right
Lives and properties damage.It is what the trend requires that developing, which has the CABLE MATERIALS of flame retardant property,.
Traditional fire-resistant cable material realized by the way of adding the fire retardants such as magnesium hydroxide into polymeric substrate, this kind of electricity
Although cable material can reach good flame retardant property, since the matrix resin of most of CABLE MATERIALSs is nonpolar polyolefin
Class macromolecule, it is poor with the compatibility of polar magnesium hydroxide based flame retardant, often reduce the mechanical property and processing of material
Performance, in CABLE MATERIALS long-term use process, the fire retardant of these additions easily exosmoses from polymeric matrix, to influence material
Stability, and then shorten the materials'use service life, Yi Yinqi safety accident.In the prior art frequently with halogen containing polymers and
Halogen containing flame-retardant obtains good flame retardant property by being kneaded, but this kind of CABLE MATERIALS can generate in the case of fire it is a large amount of toxic
Flue gas, these poison gas can cause people to suffocate.Therefore, low cigarette, low toxicity are designed and prepared, while but also with excellent flame retardancy
The hot spot of current fire-resistant cable material research can be become with the CABLE MATERIALS of insulation performance.
Authorization Notice No. is that the Chinese invention patent of CN102977611B discloses a kind of computer LSOH anti-flaming
CABLE MATERIALS is made from the following raw materials in parts by weight: 20-30 parts of polypropylene, 60-80 parts of methyl vinyl silicone rubber, EVA resin
10-20 parts, 8-10 parts of aluminium hydroxide, 0.5-1.0 parts of butyl stearate, 1-3 parts of zinc stearate, 8-12 parts of epoxidized soybean oil, oxygen
Change zinc 4-6 parts, 0.5-1.0 parts of molybdenum trioxide, 30-50 parts of gas-phase silica, modified clay 10-13 parts, antioxidant H 0.5-1.0
Part, W0.1-0.3 parts of antioxidant A, 0.5-1.5 parts of accelerant NOBS, 0.2-0.5 parts of vulcanizing agent DCBP, ammonium polyphosphate 8-10
Part, 12-15 parts of antimony oxide, 6-8 parts of hydration zinc borate.This CABLE MATERIALS not only has excellent flame retardancy and not flame-retarding power, combustion
Smoke amount is few when burning, does not generate toxic gas, and weatherability, wearability and insulating properties are good, but its complicated component, processing stream
Dynamic property is bad, and stability is bad, easily since consistency problem causes the materials'use service life short between each ingredient.
Therefore, the Low-smoke flame retardant cable material for developing a kind of excellent combination property accords with the demands of the market, and has extensive market
Value and application prospect.
Summary of the invention
The main purpose of the present invention is to provide a kind of Low-smoke flame retardant cable material, which overcomes tradition
A large amount of poison gas can be generated existing for halogen fire-resistant cable material in the case of fire, these poison gas can cause people to suffocate
Defect, also overcome by add halogen-free flame retardants cause CABLE MATERIALS processing flowability poor, the short technology of service life is asked
Topic has mechanical performance and process industrial art performance good, and softness and weatherability are good, long service life and environmentally protective, low cigarette
It is nontoxic, the advantages of excellent in flame retardance.
To achieve the above objectives, the present invention provides a kind of preparation method of Low-smoke flame retardant cable material, includes the following steps:
Step S1 mitoguazone and 1,1'- dinaphthalene -2,2'- dioctyl phthalate polycondensation: by mitoguazone, 1,1'- dinaphthalene -2,2'-
Dioctyl phthalate, n,N-diisopropylethylamine, 4-dimethylaminopyridine, which are dissolved in high boiling solvent, forms solution, then solution is added instead
It answers in kettle, with air in nitrogen or inert gas replacement kettle, 130-140 DEG C reaction 3-5 hours under normal pressure, then it is warming up to 240-
250 DEG C, carried out polycondensation reaction 15-20 hours at 300-500Pa, after be cooled to room temperature, be adjusted to normal pressure, be precipitated in water, will
After the polymer of precipitation ethanol washing 4-6 times, it is placed at 80-90 DEG C of vacuum oven and dries to constant weight, obtain condensation polymer；
Step S22- (chloromethyl) -4,4,5,5- tetramethyl -1,3,2- dioxaborolanes are grafted condensation polymer: will pass through
The condensation polymer that step S1 is prepared, which is dissolved in N-Methyl pyrrolidone, forms solution, then into solution be added basic catalyst and
2- (chloromethyl) -4,4,5,5- tetramethyls -1,3,2- dioxaborolanes are stirred to react 4-6 hours at 60-80 DEG C, after
It is precipitated in water, the polymer of precipitation is washed 3-5 times with methylene chloride, be placed at 80-90 DEG C of vacuum oven and dry extremely
Constant weight obtains intermediate product；
Step S3 ionization: the intermediate product being prepared by step S2 is dissolved in dimethyl sulfoxide, then is added thereto
Enter 4- (chloromethyl) phenyltrimethoxysila,e, be stirred to react at 40-60 DEG C 6-8 hours, after product is precipitated in water, then set
It is dried at 85-95 DEG C of vacuum oven to constant weight, the intermediate product ionized；
Step S4 CABLE MATERIALS molding: by intermediate product, the microcapsule red phosphorus, drip of the ionization being prepared by step S3
Blueness, carboxy nitrile rubber, carbon fiber, diatomaceous earth are added to extrusion molding in double screw extruder, obtain CABLE MATERIALS.
Further, mitoguazone described in step S1,1,1'- dinaphthalene -2,2'- dioctyl phthalate, n,N-diisopropylethylamine,
4-dimethylaminopyridine, high boiling solvent mass ratio be 1:1.86:(0.4-0.6): 0.3:(10-15).
Preferably, the high boiling solvent is selected from dimethyl sulfoxide, N-Methyl pyrrolidone, n,N-Dimethylformamide, N,
At least one of N- dimethyl acetamide；The inert gas is selected from one of helium, neon, argon gas.
Further, condensation polymer described in step S2, N-Methyl pyrrolidone, basic catalyst, 2- (chloromethyl) -4,4,
The mass ratio of 5,5- tetramethyl -1,3,2- dioxaborolanes is 1.5:(9-15): (0.4-0.8): 1.
Preferably, the basic catalyst is selected from least one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate.
Further, intermediate product described in step S3, dimethyl sulfoxide, 4- (chloromethyl) phenyltrimethoxysila,e matter
Amount is than being 1.78:(9-15): 1.
Further, intermediate product, microcapsule red phosphorus, pitch, carboxy nitrile rubber, the carbon of ionization described in step S4
Fiber, diatomaceous earth mass ratio be 1:0.03:0.05:(0.4-0.6): 0.1:(0.1-0.15).
Preferably, the technique of the extrusion molding is as follows: extrusion temperature, the first 185-195 DEG C of area, the second area 195-205
DEG C, 205-210 DEG C of third area, the 4th 210-215 DEG C of area, the 5th 220-230 DEG C of area, die head temperature be 230-240 DEG C, extruder
Driving screw revolving speed 160-180r/min, feed revolving speed 190-210r/min.
Further, a kind of Low-smoke flame retardant cable material is made of the preparation method of above-mentioned Low-smoke flame retardant cable material.
Due to the application of the above technical scheme, the invention has the following advantages:
(1) Low-smoke flame retardant cable material disclosed by the invention, preparation method is simple, not high to device dependence, raw material
It is easy to get, it is cheap, it is suitble to large-scale production.
(2) it is existing in generation fire to overcome the halogen fire-resistant cable material of tradition for Low-smoke flame retardant cable material disclosed by the invention
A large amount of poison gas can be generated when calamity, the defect that these poison gas can cause people to suffocate is also overcomed by adding Halogen
Fire retardant causes CABLE MATERIALS processing flowability poor, the short technical problem of service life, has mechanical performance and processing technology
Can be good, the advantages of softness and weatherability are good, long service life and environmentally protective, low smoke and non-toxic, excellent in flame retardance.
(3) Low-smoke flame retardant cable material disclosed by the invention, substrate is rich in the structure of nitrogen and phenyl ring using main chain, so that material
Excellent combination property, especially anti-flammability are even more the raising of substantially degree, are grafted by the substance of boracic structure, then ionize and draw
Enter siloxane structure, the compatibility for improving it with other compositions can be conducive to；Ion occurs with carboxy nitrile rubber after ionization
Exchange, vapored away in the form of hydrogen chloride by be allowed chloride ion, finally obtains Low-smoke flame retardant cable material, more environmentally protective；Each ingredient
Synergistic effect is so that material excellent combination property.
Specific embodiment
It is described below for disclosing the present invention so that those skilled in the art can be realized the present invention.It is excellent in being described below
Embodiment is selected to be only used as illustrating, it may occur to persons skilled in the art that other obvious modifications.
Raw material described in the embodiment of the present invention is purchased from Mo Bei (Shanghai) Biotechnology Co., Ltd.
Embodiment 1
A kind of preparation method of Low-smoke flame retardant cable material, includes the following steps:
Step S1 mitoguazone and 1,1'- dinaphthalene -2,2'- dioctyl phthalate polycondensation: by dinaphthalene -2 mitoguazone 1kg, 1,1'-,
2'- dioctyl phthalate 1.86kg, N, N- diisopropylethylamine 0.4kg, 4-dimethylaminopyridine 0.3kg are dissolved in shape in dimethyl sulfoxide 10kg
It is added in reaction kettle at solution, then by solution, with air in nitrogen displacement kettle, lower 130 DEG C of normal pressure are reacted 3 hours, then are warming up to
240 DEG C, carried out polycondensation reaction 15 hours at 300Pa, after be cooled to room temperature, be adjusted to normal pressure, be precipitated in water, by the poly- of precipitation
It closes object and is dried to constant weight with after ethanol washing 4 times, being placed at 80 DEG C of vacuum oven, obtain condensation polymer；
Step S22- (chloromethyl) -4,4,5,5- tetramethyl -1,3,2- dioxaborolanes are grafted condensation polymer: will pass through
The condensation polymer 1.5kg that step S1 is prepared, which is dissolved in N-Methyl pyrrolidone 9kg, forms solution, then hydrogen-oxygen is added into solution
Change sodium 0.4kg and 2- (chloromethyl) -4,4,5,5- tetramethyls -1,3,2- dioxaborolanes 1kg is stirred to react at 60 DEG C
4 hours, after be precipitated in water, the polymer of precipitation is washed 3 times with methylene chloride, is placed at 80 DEG C of vacuum oven dry
To constant weight, intermediate product is obtained；
Step S3 ionization: the intermediate product 1.78kg being prepared by step S2 is dissolved in dimethyl sulfoxide 9kg, then
Thereto be added 4- (chloromethyl) phenyltrimethoxysila,e 1kg, be stirred to react at 40 DEG C 6 hours, after in water be precipitated produce
Object, then be placed at 85 DEG C of vacuum oven and dry to constant weight, the intermediate product ionized；
Step S4 CABLE MATERIALS molding: by intermediate product 1kg, the microcapsule red phosphorus of the ionization being prepared by step S3
0.03kg, pitch 0.05kg, carboxy nitrile rubber 0.4kg, carbon fiber 0.1kg, diatomaceous earth 0.1kg are added to double screw extruder
Middle extrusion molding, obtains CABLE MATERIALS；The technique of the extrusion molding is as follows: extrusion temperature, the first 185 DEG C of area, the second area 195
DEG C, 205 DEG C of third area, 210 DEG C of the 4th area, 220 DEG C of the 5th area, die head temperature be 230 DEG C, extruder driving screw revolving speed 160r/
Min, feed revolving speed 190r/min.
A kind of Low-smoke flame retardant cable material is made of the preparation method of above-mentioned Low-smoke flame retardant cable material.
Embodiment 2
A kind of preparation method of Low-smoke flame retardant cable material, includes the following steps:
Step S1 mitoguazone and 1,1'- dinaphthalene -2,2'- dioctyl phthalate polycondensation: by dinaphthalene -2 mitoguazone 1kg, 1,1'-,
2'- dioctyl phthalate 1.86kg, N, N- diisopropylethylamine 0.45kg, 4-dimethylaminopyridine 0.3kg are dissolved in N-Methyl pyrrolidone
Solution is formed in 11kg, then solution is added in reaction kettle, and with air in helium replacement kettle, the lower 132 DEG C of reactions 3.5 of normal pressure are small
When, then be warming up to 243 DEG C, carried out polycondensation reaction 16 hours at 350Pa, after be cooled to room temperature, be adjusted to normal pressure, analyse in water
Out, the polymer of precipitation is dried to constant weight with after ethanol washing 4 times, being placed at 83 DEG C of vacuum oven, obtains condensation polymer；
Step S22- (chloromethyl) -4,4,5,5- tetramethyl -1,3,2- dioxaborolanes are grafted condensation polymer: will pass through
The condensation polymer 1.5kg that step S1 is prepared, which is dissolved in N-Methyl pyrrolidone 10kg, forms solution, then hydrogen is added into solution
Potassium oxide 0.5kg and 2- (chloromethyl) -4,4,5,5- tetramethyls -1,3,2- dioxaborolanes 1kg are stirred anti-at 65 DEG C
Answer 4.5 hours, after be precipitated in water, the polymer of precipitation is washed 4 times with methylene chloride, is placed at 83 DEG C of vacuum oven
Drying obtains intermediate product to constant weight；
Step S3 ionization: the intermediate product 1.78kg being prepared by step S2 is dissolved in dimethyl sulfoxide 11kg,
Again thereto be added 4- (chloromethyl) phenyltrimethoxysila,e 1kg, be stirred to react at 45 DEG C 6.5 hours, after analyse in water
Product out, then be placed at 87 DEG C of vacuum oven and dry to constant weight, the intermediate product ionized；
Step S4 CABLE MATERIALS molding: by intermediate product 1kg, the microcapsule red phosphorus of the ionization being prepared by step S3
0.03kg, pitch 0.05kg, carboxy nitrile rubber 0.45kg, carbon fiber 0.1kg, diatomaceous earth 0.11kg are added to twin-screw extrusion
Extrusion molding in machine, obtains CABLE MATERIALS；The technique of the extrusion molding is as follows: extrusion temperature, the first 188 DEG C of area, the second area 197
DEG C, 207 DEG C of third area, 212 DEG C of the 4th area, 223 DEG C of the 5th area, die head temperature 232, extruder driving screw revolving speed 165r/
Min, feed revolving speed 193r/min.
A kind of Low-smoke flame retardant cable material is made of the preparation method of above-mentioned Low-smoke flame retardant cable material.
Embodiment 3
A kind of preparation method of Low-smoke flame retardant cable material, includes the following steps:
Step S1 mitoguazone and 1,1'- dinaphthalene -2,2'- dioctyl phthalate polycondensation: by dinaphthalene -2 mitoguazone 1kg, 1,1'-,
2'- dioctyl phthalate 1.86kg, N, N- diisopropylethylamine 0.5kg, 4-dimethylaminopyridine 0.3kg are dissolved in N,N-dimethylformamide
Solution is formed in 13kg, then solution is added in reaction kettle, with air in neon displacement kettle, lower 135 DEG C of normal pressure are reacted 4 hours,
Be warming up to 245 DEG C again, carried out polycondensation reaction 17 hours at 400Pa, after be cooled to room temperature, be adjusted to normal pressure, be precipitated in water, will
The polymer of precipitation is dried to constant weight with after ethanol washing 5 times, being placed at 85 DEG C of vacuum oven, and condensation polymer is obtained；
Step S22- (chloromethyl) -4,4,5,5- tetramethyl -1,3,2- dioxaborolanes are grafted condensation polymer: will pass through
The condensation polymer 1.5kg that step S1 is prepared, which is dissolved in N-Methyl pyrrolidone 12.5kg, forms solution, then is added into solution
Sodium carbonate 0.6kg and 2- (chloromethyl) -4,4,5,5- tetramethyls -1,3,2- dioxaborolanes 1kg are stirred anti-at 70 DEG C
Answer 5 hours, after be precipitated in water, the polymer of precipitation is washed 4 times with methylene chloride, be placed at 85 DEG C of vacuum oven do
It is dry to constant weight, obtain intermediate product；
Step S3 ionization: the intermediate product 1.78kg being prepared by step S2 is dissolved in dimethyl sulfoxide 13kg,
Again thereto be added 4- (chloromethyl) phenyltrimethoxysila,e 1kg, be stirred to react at 50 DEG C 7 hours, after be precipitated in water
Product, then be placed at 89 DEG C of vacuum oven and dry to constant weight, the intermediate product ionized；
Step S4 CABLE MATERIALS molding: by intermediate product 1kg, the microcapsule red phosphorus of the ionization being prepared by step S3
0.03kg, pitch 0.05kg, carboxy nitrile rubber 0.5kg, carbon fiber 0.1kg, diatomaceous earth 0.13kg are added to twin-screw extrusion
Extrusion molding in machine, obtains CABLE MATERIALS；The technique of the extrusion molding is as follows: extrusion temperature, the first 190 DEG C of area, the second area 200
DEG C, 208 DEG C of third area, 213 DEG C of the 4th area, 225 DEG C of the 5th area, die head temperature be 235 DEG C, extruder driving screw revolving speed 175r/
Min, feed revolving speed 200r/min.
A kind of Low-smoke flame retardant cable material is made of the preparation method of above-mentioned Low-smoke flame retardant cable material.
Embodiment 4
A kind of preparation method of Low-smoke flame retardant cable material, includes the following steps:
Step S1 mitoguazone and 1,1'- dinaphthalene -2,2'- dioctyl phthalate polycondensation: by dinaphthalene -2 mitoguazone 1kg, 1,1'-,
2'- dioctyl phthalate 1.86kg, N, N- diisopropylethylamine 0.55kg, 4-dimethylaminopyridine 0.3kg are dissolved in high boiling solvent 14kg
Middle formation solution, then solution is added in reaction kettle, with air in argon gas displacement kettle, lower 138 DEG C of normal pressure are reacted 4.5 hours, then
Be warming up to 248 DEG C, carried out polycondensation reaction 19 hours at 480Pa, after be cooled to room temperature, be adjusted to normal pressure, be precipitated in water, will analyse
Polymer out is dried to constant weight with after ethanol washing 6 times, being placed at 88 DEG C of vacuum oven, and condensation polymer is obtained；It is described high boiling
Point solvent is dimethyl sulfoxide, N-Methyl pyrrolidone, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide 1:3 in mass ratio:
2:2 is mixed；
Step S22- (chloromethyl) -4,4,5,5- tetramethyl -1,3,2- dioxaborolanes are grafted condensation polymer: will pass through
The condensation polymer 1.5kg that step S1 is prepared, which is dissolved in N-Methyl pyrrolidone 14kg, forms solution, then alkali is added into solution
Property catalyst 0.7kg and 2- (chloromethyl) -4,4,5,5- tetramethyls -1,3,2- dioxaborolanes 1kg are stirred at 77 DEG C
Reaction 5.8 hours, after be precipitated in water, the polymer of precipitation is washed 5 times with methylene chloride, is placed on 88 DEG C of vacuum oven
Lower drying obtains intermediate product to constant weight；The basic catalyst is sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate by matter
Amount is mixed than 1:2:4:2；
Step S3 ionization: the intermediate product 1.78kg being prepared by step S2 is dissolved in dimethyl sulfoxide 14.5kg
In, then thereto be added 4- (chloromethyl) phenyltrimethoxysila,e 1kg, be stirred to react at 55 DEG C 7.8 hours, after in water
Product is precipitated, then is placed at 93 DEG C of vacuum oven and dries to constant weight, the intermediate product ionized；
Step S4 CABLE MATERIALS molding: by intermediate product 1kg, the microcapsule red phosphorus of the ionization being prepared by step S3
0.03kg, pitch 0.05kg, carboxy nitrile rubber 0.58kg, carbon fiber 0.1kg, diatomaceous earth 0.14kg are added to twin-screw extrusion
Extrusion molding in machine, obtains CABLE MATERIALS；The technique of the extrusion molding is as follows: extrusion temperature, the first 193 DEG C of area, the second area 203
DEG C, 209 DEG C of third area, 214 DEG C of the 4th area, 228 DEG C of the 5th area, die head temperature be 238 DEG C, extruder driving screw revolving speed 175r/
Min, feed revolving speed 205r/min.
A kind of Low-smoke flame retardant cable material is made of the preparation method of above-mentioned Low-smoke flame retardant cable material.
Embodiment 5
A kind of preparation method of Low-smoke flame retardant cable material, includes the following steps:
Step S1 mitoguazone and 1,1'- dinaphthalene -2,2'- dioctyl phthalate polycondensation: by dinaphthalene -2 mitoguazone 1kg, 1,1'-,
2'- dioctyl phthalate 1.86kg, N, N- diisopropylethylamine 0.6kg, 4-dimethylaminopyridine 0.3kg are dissolved in DMAC N,N' dimethyl acetamide
Solution is formed in 15kg, then solution is added in reaction kettle, with air in nitrogen displacement kettle, lower 140 DEG C of normal pressure are reacted 5 hours,
Be warming up to 250 DEG C again, carried out polycondensation reaction 20 hours at 500Pa, after be cooled to room temperature, be adjusted to normal pressure, be precipitated in water, will
The polymer of precipitation is dried to constant weight with after ethanol washing 6 times, being placed at 90 DEG C of vacuum oven, and condensation polymer is obtained；
Step S22- (chloromethyl) -4,4,5,5- tetramethyl -1,3,2- dioxaborolanes are grafted condensation polymer: will pass through
The condensation polymer 1.5kg that step S1 is prepared, which is dissolved in N-Methyl pyrrolidone 15kg, forms solution, then carbon is added into solution
Sour potassium 0.8kg and 2- (chloromethyl) -4,4,5,5- tetramethyls -1,3,2- dioxaborolanes 1kg are stirred to react at 80 DEG C
6 hours, after be precipitated in water, the polymer of precipitation is washed 5 times with methylene chloride, is placed at 90 DEG C of vacuum oven dry
To constant weight, intermediate product is obtained；
Step S3 ionization: the intermediate product 1.78kg being prepared by step S2 is dissolved in dimethyl sulfoxide 15kg,
Again thereto be added 4- (chloromethyl) phenyltrimethoxysila,e 1kg, be stirred to react at 60 DEG C 8 hours, after be precipitated in water
Product, then be placed at 95 DEG C of vacuum oven and dry to constant weight, the intermediate product ionized；
Step S4 CABLE MATERIALS molding: by intermediate product 1kg, the microcapsule red phosphorus of the ionization being prepared by step S3
0.03kg, pitch 0.05kg, carboxy nitrile rubber 0.6kg, carbon fiber 0.1kg, diatomaceous earth 0.15kg are added to twin-screw extrusion
Extrusion molding in machine, obtains CABLE MATERIALS；The technique of the extrusion molding is as follows: extrusion temperature, the first 195 DEG C of area, the second area 205
DEG C, 210 DEG C of third area, 215 DEG C of the 4th area, 230 DEG C of the 5th area, die head temperature 240, extruder driving screw revolving speed 180r/
Min, feed revolving speed 210r/min.
A kind of Low-smoke flame retardant cable material is made of the preparation method of above-mentioned Low-smoke flame retardant cable material.
Comparative example 1
The present invention provides a kind of Low-smoke flame retardant cable material, and formula and preparation method are similar to Example 1, the difference is that not having
There is addition carboxy nitrile rubber.
Comparative example 2
The present invention provides a kind of Low-smoke flame retardant cable material, and formula and preparation method are similar to Example 1, the difference is that not having
There is addition diatomaceous earth.
Comparative example 3
The present invention provides a kind of Low-smoke flame retardant cable material, according to matching for Chinese invention patent CN108250765A embodiment 1
Side is made.
Above embodiments 1-5 and comparative example the 1-3 Low-smoke flame retardant cable material prepared are tested for the property, test method and
Test result is shown in Table 1.
1 CABLE MATERIALS the performance test results of table
As seen from Table 1, Low-smoke flame retardant cable material disclosed by the embodiments of the present invention, with low-smoke fireproof cable in the prior art
Material is compared, and has more excellent mechanical performance, anti-flammability and insulating properties, and smoke density is lower.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement is both fallen in the range of claimed invention.The present invention claims protection scope by appended claims and its
Equivalent defines.
Claims (9)
1. a kind of preparation method of Low-smoke flame retardant cable material, which comprises the steps of:
Step S1 mitoguazone and 1,1'- dinaphthalene -2,2'- dioctyl phthalate polycondensation: by mitoguazone, 1,1'- dinaphthalene -2,2'- diformazan
Acid, n,N-diisopropylethylamine, 4-dimethylaminopyridine, which are dissolved in high boiling solvent, forms solution, then reaction kettle is added in solution
In, with air in nitrogen or inert gas replacement kettle, 130-140 DEG C reaction 3-5 hours under normal pressure, then it is warming up to 240-250 DEG C,
Carried out polycondensation reaction 15-20 hours at 300-500Pa, after be cooled to room temperature, be adjusted to normal pressure, be precipitated in water, by precipitation
After polymer ethanol washing 4-6 times, it is placed at 80-90 DEG C of vacuum oven and dries to constant weight, obtain condensation polymer；
Step S22- (chloromethyl) -4,4,5,5- tetramethyl -1,3,2- dioxaborolanes are grafted condensation polymer: will pass through step
The condensation polymer that S1 is prepared, which is dissolved in N-Methyl pyrrolidone, forms solution, then basic catalyst and 2- are added into solution
(chloromethyl) -4,4,5,5- tetramethyls -1,3,2- dioxaborolanes are stirred to react 4-6 hours at 60-80 DEG C, after
It is precipitated in water, the polymer of precipitation is washed 3-5 times with methylene chloride, be placed at 80-90 DEG C of vacuum oven and dry to perseverance
Weight, obtains intermediate product；
Step S3 ionization: the intermediate product being prepared by step S2 is dissolved in dimethyl sulfoxide, then 4- is added thereto
(chloromethyl) phenyltrimethoxysila,e is stirred to react 6-8 hours at 40-60 DEG C, after product is precipitated in water, then be placed in true
It is dried at 85-95 DEG C of empty drying box to constant weight, the intermediate product ionized；
The molding of step S4 CABLE MATERIALS: by the intermediate product for the ionization being prepared by step S3, microcapsule red phosphorus, pitch,
Carboxy nitrile rubber, carbon fiber, diatomaceous earth are added to extrusion molding in double screw extruder, obtain CABLE MATERIALS.
2. a kind of preparation method of Low-smoke flame retardant cable material according to claim 1, which is characterized in that described in step S1
Mitoguazone, 1,1'- dinaphthalene -2,2'- dioctyl phthalate, N, N- diisopropylethylamine, 4-dimethylaminopyridine, the matter of high boiling solvent
Amount is than being 1:1.86:(0.4-0.6): 0.3:(10-15).
3. a kind of preparation method of Low-smoke flame retardant cable material according to claim 1, which is characterized in that the higher boiling is molten
Agent is selected from least one of dimethyl sulfoxide, N-Methyl pyrrolidone, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide；
The inert gas is selected from one of helium, neon, argon gas.
4. a kind of preparation method of Low-smoke flame retardant cable material according to claim 1, which is characterized in that described in step S2
Condensation polymer, N-Methyl pyrrolidone, basic catalyst, penta boron of 2- (chloromethyl) -4,4,5,5- tetramethyl -1,3,2- dioxane
The mass ratio of alkane is 1.5:(9-15): (0.4-0.8): 1.
5. a kind of preparation method of Low-smoke flame retardant cable material according to claim 1, which is characterized in that the base catalysis
Agent is selected from least one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate.
6. a kind of preparation method of Low-smoke flame retardant cable material according to claim 1, which is characterized in that described in step S3
Intermediate product, dimethyl sulfoxide, 4- (chloromethyl) phenyltrimethoxysila,e mass ratio be 1.78:(9-15): 1.
7. a kind of preparation method of Low-smoke flame retardant cable material according to claim 1, which is characterized in that described in step S4
The intermediate product of ionization, microcapsule red phosphorus, pitch, carboxy nitrile rubber, carbon fiber, diatomaceous earth mass ratio be 1:0.03:
0.05:(0.4-0.6):0.1:(0.1-0.15)。
8. a kind of preparation method of Low-smoke flame retardant cable material according to claim 1, which is characterized in that the extrusion molding
Technique it is as follows: extrusion temperature, the first 185-195 DEG C of area, 195-205 DEG C of the secondth area, 205-210 DEG C of third area, the 4th area
210-215 DEG C, the 5th 220-230 DEG C of area, die head temperature are 230-240 DEG C, and extruder driving screw revolving speed 160-180r/min adds
Expect revolving speed 190-210r/min.
9. a kind of low cigarette that the preparation method of Low-smoke flame retardant cable material according to claim 1-8 is prepared resistance
Fire CABLE MATERIALS.
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Cited By (1)
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| CN110746885A (en) * | 2019-11-27 | 2020-02-04 | 湖南辰砾新材料有限公司 | Sound-insulation weather-resistant waterproof coating and preparation method thereof |
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Application publication date: 20190927 |