CN106905618A - A kind of preparation method and applications of anti-flammability environment-friendlyinsulation insulation material - Google Patents
A kind of preparation method and applications of anti-flammability environment-friendlyinsulation insulation material Download PDFInfo
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- 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
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Abstract
The invention discloses a kind of preparation method and applications of anti-flammability environment-friendlyinsulation insulation material, the technique is by by semi-hydrated gypsum, perlite, bentonite carries out ball milling, granulation, then with the common banburying of epoxy resin, it is subsequently adding tetrahydrofuran vacuum stirring, add polyamide wax micropowder and by EP rubbers, methylhydroxypropylcellulose sodium, phenyl glycidyl ether, through dehydration, heating, vacuum reaction thing obtained by vacuum reaction, through plasticating, charging, ultrasound, it is evaporated under reduced pressure, Screw Extrusion, reaction under high pressure, deaeration solidifies, it is compressing, a series of special processes such as pelletizing are made finished product.The insulating materials being prepared from, it has excellent fire resistance and mechanical strength concurrently, with preferable application prospect.The application as insulating materials obtained in the preparation technology in power industry is also disclosed simultaneously.
Description
Technical field
The present invention relates to this technical field of insulating materials, a kind of preparation of anti-flammability environment-friendlyinsulation insulation material is related specifically to
Method and its application.
Background technology
As the application of cable in production and living is growing and popularization, measured the need for cable increases very in recent years
Hurry up.And along with scientific and technological progress, requirement to its material also more and more higher.It is generally soft to requiring to include on cable performance
It is soft, wear-resisting, low temperature resistant etc..And demand it is more be flame retardant cable.Flame retardant cable refers to that under regulation experimental condition, sample is fired
Burn, after experiment burning things which may cause a fire disaster is removed, flame is spread only in the range of restriction, residual flame in limiting time can self-extinguish electricity
Cable.Its basic characteristic is：It is possible to be burned and can not run in case of fire, but spreading for the intensity of a fire can be prevented.Generically
Say, if cable catches fire, burning can be limited in subrange, do not produce and spread, keep other various equipment, it is to avoid
Result in greater loss.Life security and property safety can be to a greater extent protected, so with more universal.
The sheathing material of conventional cable has poly chloroacetic acid, polyethylene, crosslinked polyethylene, ethylene propylene diene rubber etc..As
The sheathing material of communication cable, polyvinyl chloride disclosure satisfy that and be normally applied all characteristics for requiring cable, and because it possesses
Fireproofing function, polyvinyl chloride is widely used in the crust and optical fiber of electric wire.Yet with polyvinyl chloride in electrical apparatus insulation performance side
The limitation in face, its insulation that cannot be used for high-tension cable and high quality communications cable.Also, used in mine construction and mining
Cable sheath material for cable protective effect requirement it is higher, it is necessary to have excellent mechanical strength, such as wearability, stretching
Intensity, elongation at break etc., which limits the further application of polyvinyl chloride cable shell, to the cable application of special trade
Bring no small influence.
The content of the invention
In order to solve the above technical problems, the present invention provides a kind of preparation method of anti-flammability environment-friendlyinsulation insulation material and its answers
With the technique carries out ball milling, granulation by by semi-hydrated gypsum, perlite, bentonite, then with the common banburying of epoxy resin, so
Add tetrahydrofuran to be stirred under vacuum afterwards, add polyamide wax micropowder and by EP rubbers, methylhydroxypropylcellulose sodium, benzene
Base glycidol ether, through dehydration, heating, the vacuum reaction thing obtained by vacuum reaction, through plasticating, feeding, ultrasound, be evaporated under reduced pressure,
A series of special processes such as Screw Extrusion, reaction under high pressure, deaeration solidification, compressing, pelletizing are made finished product.What is be prepared from is exhausted
Edge material, it has excellent fire resistance and mechanical strength concurrently, with preferable application prospect.Also disclose by the preparation simultaneously
Application of the anti-flammability environment-friendlyinsulation insulation material in power industry obtained in technique.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of preparation method of anti-flammability environment-friendlyinsulation insulation material, comprises the following steps：
(1) by 15 parts of semi-hydrated gypsum, 12 parts of perlite, 8 parts of mixing of bentonite, it is milled in addition planetary ball mill machine
Uniformly, it is that 80% glycerin solution is mixed to add 500mL concentration, is subsequently added in comminutor and is granulated, and is made grain
Footpath is 0.6-0.8 μm of particle；
(2) by 10 parts of EP rubbers, 6 parts of methylhydroxypropylcellulose sodium, 5 parts of stirring in 150rpm of phenyl glycidyl ether
Vacuum dehydration under the conditions of mixing, is subsequently added 5 parts of salethyl, and 120 DEG C are heated under nitrogen atmosphere, is heated up after reaction 3-5h
To 150 DEG C, after maintaining 2-3h, 0.01-0.03MPa is evacuated to, maintains 27min, obtain vacuum reaction thing；
(3) by the particle obtained by step (1) and 10 parts of addition banburies of epoxy resin, it is well mixed, is 110- in temperature
Banburying 10-15min at 120 DEG C, obtains banburying product；
(4) by the banburying product obtained by step (3) and tetrahydrofuran 20 parts mix, inserting vacuum mixer carries out vacuum
Stirring 10min, then stands 15min, obtains initial mixture；
(5) two roll plastic mixing mill is risen into high-temperature to 180-200 DEG C, by the initial mixture and polyamide wax of step (4)
7 parts of micro mist adds double roller intermediate melt to plasticate, and the vacuum reaction thing obtained by step (2) is added after it is well mixed, and adjustment is double
Roller spacing, roll milling, it is thin it is logical be repeatedly well mixed the two, must plasticate product；
(6) product of plasticating of step (5) mixes with 6 parts of polycarbonate resin, 50 parts of deionized water, is heated to 90-100
DEG C, 3 parts of accelerator 2-ethyl-4-methylimidazole is added after stirring reaction 1-2h, then ultrasonic disperse 15-20min is decompressed to
0.03MPa, steams low-boiling point material, obtains initial reaction product；
(7) initial reaction product of step (6) is added into double screw extruder, intermediate reaction product is obtained after melting extrusion
Thing, wherein double-screw extruder screw draw ratio are 20:1；
(8) intermediate reaction product that obtains step (7) is added in autoclave, add 2 parts of dicyclopentadiene with
And appropriate deionized water, 3 parts of styrene is added after 25min is stirred in a nitrogen atmosphere, reactor pressure is lifted into 15MPa,
2 parts of liquor potassic permanganate is added dropwise to after mixture is warming up into 150 DEG C, reaction under high pressure 35-45min obtains final reacting product；
(9) by the final reacting product addition reaction vessel of step (8), processed through deaeration after being uniformly mixed, with
After be heated to 85-95 DEG C solidification 3-4h, after being finally warming up to 160-180 DEG C with the speed of 7 DEG C/min again, isothermal curing 1.5-
2h, naturally cools to and mixed material is transferred in vulcanizing press in compressing, pelletizing at 180 DEG C after room temperature, obtains into
Product.
Preferably, the particle diameter of particle is 0.7 μm in the step (1).
Preferably, double screw extruder extrusion temperature is in the step (7)：One 150-160 DEG C of area's temperature, two area's temperature
It it is 170-180 DEG C, three area's temperature are 210-220 DEG C, four area's temperature are 230-250 DEG C.
Preferably, the concentration of liquor potassic permanganate is preferably 2.5% in the step (8).
The answering in power industry present invention also offers the anti-flammability environment-friendlyinsulation insulation material obtained by above-mentioned preparation technology
With.
Compared with prior art, its advantage is the present invention：
(1) anti-flammability environment-friendlyinsulation insulation material preparation technology of the invention is carried out by by semi-hydrated gypsum, perlite, bentonite
Ball milling, granulation, then with the common banburying of epoxy resin, are subsequently adding tetrahydrofuran vacuum stirring, add polyamide wax micropowder
And by EP rubbers, methylhydroxypropylcellulose sodium, phenyl glycidyl ether, through true obtained by dehydration, heating, vacuum reaction
Empty reactant, through plasticating, feeding, ultrasound, reduction vaporization, Screw Extrusion, reaction under high pressure, deaeration solidification, compressing, pelletizing etc.
A series of special processes are made finished product.The insulating materials being prepared from, it has excellent fire resistance and mechanical strength concurrently, has
Preferable application prospect.
(2) anti-flammability environment-friendlyinsulation insulation material raw material of the invention is cheap, process is simple, is suitable to heavy industrialization utilization,
It is practical.
Specific embodiment
The technical scheme invented is described in detail with reference to specific embodiment.
Embodiment 1
(1) by 15 parts of semi-hydrated gypsum, 12 parts of perlite, 8 parts of mixing of bentonite, it is milled in addition planetary ball mill machine
Uniformly, it is that 80% glycerin solution is mixed to add 500mL concentration, is subsequently added in comminutor and is granulated, and is made grain
Footpath is 0.7 μm of particle；
(2) by 10 parts of EP rubbers, 6 parts of methylhydroxypropylcellulose sodium, 5 parts of stirring in 150rpm of phenyl glycidyl ether
Vacuum dehydration under the conditions of mixing, is subsequently added 5 parts of salethyl, and 120 DEG C are heated under nitrogen atmosphere, is warming up to after reaction 3h
150 DEG C, after maintaining 2h, 0.01MPa is evacuated to, maintains 27min, obtain vacuum reaction thing；
(3) by the particle obtained by step (1) and 10 parts of addition banburies of epoxy resin, it is well mixed, is 110 DEG C in temperature
Lower banburying 10min, obtains banburying product；
(4) by the banburying product obtained by step (3) and tetrahydrofuran 20 parts mix, inserting vacuum mixer carries out vacuum
Stirring 10min, then stands 15min, obtains initial mixture；
(5) two roll plastic mixing mill is risen into high-temperature to 180 DEG C, by the initial mixture and polyamide wax micropowder 7 of step (4)
Part adds double roller intermediate melt to plasticate, and is added after it is well mixed between the vacuum reaction thing obtained by step (2), adjustment double roller
Away from, roll milling, it is thin it is logical be repeatedly well mixed the two, must plasticate product；
(6) product of plasticating of step (5) mixes with 6 parts of polycarbonate resin, 50 parts of deionized water, is heated to 90 DEG C, stirs
3 parts of accelerator 2-ethyl-4-methylimidazole is added after mixing reaction 1h, then ultrasonic disperse 15min is decompressed to 0.03MPa, steams
Low-boiling point material, obtains initial reaction product；
(7) initial reaction product of step (6) is added into double screw extruder, intermediate reaction product is obtained after melting extrusion
Thing, wherein double-screw extruder screw draw ratio are 20:1, double screw extruder extrusion temperature is：One 150 DEG C of area's temperature, 2nd area
Temperature is 170 DEG C, and three area's temperature are 210 DEG C, and four area's temperature are 230 DEG C；
(8) intermediate reaction product that obtains step (7) is added in autoclave, add 2 parts of dicyclopentadiene with
And appropriate deionized water, 3 parts of styrene is added after 25min is stirred in a nitrogen atmosphere, reactor pressure is lifted into 15MPa,
2 parts of the liquor potassic permanganate that dropwise addition concentration after 150 DEG C is 2.5% is warming up to by mixture, reaction under high pressure 35min is obtained most
End reaction product；
(9) by the final reacting product addition reaction vessel of step (8), processed through deaeration after being uniformly mixed, with
After be heated to 85 DEG C solidification 3h, after being finally warming up to 160 DEG C with the speed of 7 DEG C/min again, isothermal curing 1.5h is naturally cooled to
Mixed material is transferred in vulcanizing press in compressing, pelletizing at 180 DEG C after room temperature, obtains finished product.
The performance test results of obtained anti-flammability environment-friendlyinsulation insulation material are as shown in table 1.
Embodiment 2
(1) by 15 parts of semi-hydrated gypsum, 12 parts of perlite, 8 parts of mixing of bentonite, it is milled in addition planetary ball mill machine
Uniformly, it is that 80% glycerin solution is mixed to add 500mL concentration, is subsequently added in comminutor and is granulated, and is made grain
Footpath is 0.7 μm of particle；
(2) by 10 parts of EP rubbers, 6 parts of methylhydroxypropylcellulose sodium, 5 parts of stirring in 150rpm of phenyl glycidyl ether
Vacuum dehydration under the conditions of mixing, is subsequently added 5 parts of salethyl, and 120 DEG C are heated under nitrogen atmosphere, is warming up to after reaction 4h
150 DEG C, after maintaining 2.5h, 0.02MPa is evacuated to, maintains 27min, obtain vacuum reaction thing；
(3) by the particle obtained by step (1) and 10 parts of addition banburies of epoxy resin, it is well mixed, is 115 DEG C in temperature
Lower banburying 13min, obtains banburying product；
(4) by the banburying product obtained by step (3) and tetrahydrofuran 20 parts mix, inserting vacuum mixer carries out vacuum
Stirring 10min, then stands 15min, obtains initial mixture；
(5) two roll plastic mixing mill is risen into high-temperature to 190 DEG C, by the initial mixture and polyamide wax micropowder 7 of step (4)
Part adds double roller intermediate melt to plasticate, and is added after it is well mixed between the vacuum reaction thing obtained by step (2), adjustment double roller
Away from, roll milling, it is thin it is logical be repeatedly well mixed the two, must plasticate product；
(6) product of plasticating of step (5) mixes with 6 parts of polycarbonate resin, 50 parts of deionized water, is heated to 95 DEG C, stirs
3 parts of accelerator 2-ethyl-4-methylimidazole is added after mixing reaction 1.5h, then ultrasonic disperse 18min is decompressed to 0.03MPa, steamed
Go out low-boiling point material, obtain initial reaction product；
(7) initial reaction product of step (6) is added into double screw extruder, intermediate reaction product is obtained after melting extrusion
Thing, wherein double-screw extruder screw draw ratio are 20:1, double screw extruder extrusion temperature is：One 155 DEG C of area's temperature, 2nd area
Temperature is 175 DEG C, and three area's temperature are 215 DEG C, and four area's temperature are 240 DEG C；
(8) intermediate reaction product that obtains step (7) is added in autoclave, add 2 parts of dicyclopentadiene with
And appropriate deionized water, 3 parts of styrene is added after 25min is stirred in a nitrogen atmosphere, reactor pressure is lifted into 15MPa,
2 parts of the liquor potassic permanganate that dropwise addition concentration after 150 DEG C is 2.5% is warming up to by mixture, reaction under high pressure 40min is obtained most
End reaction product；
(9) by the final reacting product addition reaction vessel of step (8), processed through deaeration after being uniformly mixed, with
After be heated to 90 DEG C solidification 3.5h, after being finally warming up to 170 DEG C with the speed of 7 DEG C/min again, isothermal curing 2h is naturally cooled to
Mixed material is transferred in vulcanizing press in compressing, pelletizing at 180 DEG C after room temperature, obtains finished product.
The performance test results of obtained anti-flammability environment-friendlyinsulation insulation material are as shown in table 1.
Embodiment 3
(1) by 15 parts of semi-hydrated gypsum, 12 parts of perlite, 8 parts of mixing of bentonite, it is milled in addition planetary ball mill machine
Uniformly, it is that 80% glycerin solution is mixed to add 500mL concentration, is subsequently added in comminutor and is granulated, and is made grain
Footpath is 0.7 μm of particle；
(2) by 10 parts of EP rubbers, 6 parts of methylhydroxypropylcellulose sodium, 5 parts of stirring in 150rpm of phenyl glycidyl ether
Vacuum dehydration under the conditions of mixing, is subsequently added 5 parts of salethyl, and 120 DEG C are heated under nitrogen atmosphere, is warming up to after reaction 5h
150 DEG C, after maintaining 3h, 0.03MPa is evacuated to, maintains 27min, obtain vacuum reaction thing；
(3) by the particle obtained by step (1) and 10 parts of addition banburies of epoxy resin, it is well mixed, is 120 DEG C in temperature
Lower banburying 15min, obtains banburying product；
(4) by the banburying product obtained by step (3) and tetrahydrofuran 20 parts mix, inserting vacuum mixer carries out vacuum
Stirring 10min, then stands 15min, obtains initial mixture；
(5) two roll plastic mixing mill is risen into high-temperature to 200 DEG C, by the initial mixture and polyamide wax micropowder 7 of step (4)
Part adds double roller intermediate melt to plasticate, and is added after it is well mixed between the vacuum reaction thing obtained by step (2), adjustment double roller
Away from, roll milling, it is thin it is logical be repeatedly well mixed the two, must plasticate product；
(6) product of plasticating of step (5) mixes with 6 parts of polycarbonate resin, 50 parts of deionized water, is heated to 100 DEG C, stirs
3 parts of accelerator 2-ethyl-4-methylimidazole is added after mixing reaction 2h, then ultrasonic disperse 20min is decompressed to 0.03MPa, steams
Low-boiling point material, obtains initial reaction product；
(7) initial reaction product of step (6) is added into double screw extruder, intermediate reaction product is obtained after melting extrusion
Thing, wherein double-screw extruder screw draw ratio are 20:1, double screw extruder extrusion temperature is：One 160 DEG C of area's temperature, 2nd area
Temperature is 180 DEG C, and three area's temperature are 220 DEG C, and four area's temperature are 250 DEG C；
(8) intermediate reaction product that obtains step (7) is added in autoclave, add 2 parts of dicyclopentadiene with
And appropriate deionized water, 3 parts of styrene is added after 25min is stirred in a nitrogen atmosphere, reactor pressure is lifted into 15MPa,
2 parts of the liquor potassic permanganate that dropwise addition concentration after 150 DEG C is 2.5% is warming up to by mixture, reaction under high pressure 45min is obtained most
End reaction product；
(9) by the final reacting product addition reaction vessel of step (8), processed through deaeration after being uniformly mixed, with
After be heated to 95 DEG C solidification 4h, after being finally warming up to 180 DEG C with the speed of 7 DEG C/min again, isothermal curing 2h naturally cools to room
Mixed material is transferred in vulcanizing press in compressing, pelletizing at 180 DEG C after temperature, obtains finished product.
The performance test results of obtained anti-flammability environment-friendlyinsulation insulation material are as shown in table 1.
Comparative example 1
(1) by 15 parts of semi-hydrated gypsum, 12 parts of perlite, 8 parts of mixing of bentonite, it is milled in addition planetary ball mill machine
Uniformly, it is that 80% glycerin solution is mixed to add 500mL concentration, is subsequently added in comminutor and is granulated, and is made grain
Footpath is 0.7 μm of particle；
(2) by 15 parts of EP rubbers, 4 parts of methylhydroxypropylcellulose sodium, 5 parts of stirring in 150rpm of phenyl glycidyl ether
Vacuum dehydration under the conditions of mixing, is subsequently added 5 parts of salethyl, and 120 DEG C are heated under nitrogen atmosphere, is warming up to after reaction 3h
150 DEG C, after maintaining 2h, 0.01MPa is evacuated to, maintains 27min, obtain vacuum reaction thing；
(3) by the particle obtained by step (1) and 15 parts of addition banburies of epoxy resin, it is well mixed, is 110 DEG C in temperature
Lower banburying 10min, obtains banburying product；
(4) by the banburying product obtained by step (3) and tetrahydrofuran 15 parts mix, inserting vacuum mixer carries out vacuum
Stirring 10min, then stands 15min, obtains initial mixture；
(5) two roll plastic mixing mill is risen into high-temperature to 180 DEG C, by the initial mixture and polyamide wax micropowder 7 of step (4)
Part adds double roller intermediate melt to plasticate, and is added after it is well mixed between the vacuum reaction thing obtained by step (2), adjustment double roller
Away from, roll milling, it is thin it is logical be repeatedly well mixed the two, must plasticate product；
(6) product of plasticating of step (5) mixes with 6 parts of polycarbonate resin, 50 parts of deionized water, is heated to 90 DEG C, stirs
3 parts of accelerator 2-ethyl-4-methylimidazole is added after mixing reaction 1h, then ultrasonic disperse 15min is decompressed to 0.03MPa, steams
Low-boiling point material, obtains initial reaction product；
(7) initial reaction product of step (6) is added into double screw extruder, intermediate reaction product is obtained after melting extrusion
Thing, wherein double-screw extruder screw draw ratio are 20:1, double screw extruder extrusion temperature is：One 150 DEG C of area's temperature, 2nd area
Temperature is 170 DEG C, and three area's temperature are 210 DEG C, and four area's temperature are 230 DEG C；
(8) intermediate reaction product that obtains step (7) is added in autoclave, add 2 parts of dicyclopentadiene with
And appropriate deionized water, 3 parts of styrene is added after 25min is stirred in a nitrogen atmosphere, reactor pressure is lifted into 15MPa,
2 parts of the liquor potassic permanganate that dropwise addition concentration after 150 DEG C is 2.5% is warming up to by mixture, reaction under high pressure 35min is obtained most
End reaction product；
(9) by the final reacting product addition reaction vessel of step (8), processed through deaeration after being uniformly mixed, with
After be heated to 85 DEG C solidification 3h, after being finally warming up to 160 DEG C with the speed of 7 DEG C/min again, isothermal curing 1.5h is naturally cooled to
Mixed material is transferred in vulcanizing press in compressing, pelletizing at 180 DEG C after room temperature, obtains finished product.
The performance test results of obtained anti-flammability environment-friendlyinsulation insulation material are as shown in table 1.
Comparative example 2
(1) by 15 parts of semi-hydrated gypsum, 12 parts of perlite, 8 parts of mixing of bentonite, it is milled in addition planetary ball mill machine
Uniformly, it is that 80% glycerin solution is mixed to add 500mL concentration, is subsequently added in comminutor and is granulated, and is made grain
Footpath is 0.7 μm of particle；
(2) by 10 parts of EP rubbers, 6 parts of methylhydroxypropylcellulose sodium, 5 parts of stirring in 150rpm of phenyl glycidyl ether
Vacuum dehydration under the conditions of mixing, is subsequently added 5 parts of salethyl, and 150 DEG C are heated under nitrogen atmosphere, is warming up to after reaction 4h
180 DEG C, after maintaining 2.5h, 0.02MPa is evacuated to, maintains 27min, obtain vacuum reaction thing；
(3) by the particle obtained by step (1) and 10 parts of addition banburies of epoxy resin, it is well mixed, is 115 DEG C in temperature
Lower banburying 13min, obtains banburying product；
(4) by the banburying product obtained by step (3) and tetrahydrofuran 20 parts mix, inserting vacuum mixer carries out vacuum
Stirring 10min, then stands 15min, obtains initial mixture；
(5) two roll plastic mixing mill is risen into high-temperature to 190 DEG C, by the initial mixture and polyamide wax micropowder 7 of step (4)
Part adds double roller intermediate melt to plasticate, and is added after it is well mixed between the vacuum reaction thing obtained by step (2), adjustment double roller
Away from, roll milling, it is thin it is logical be repeatedly well mixed the two, must plasticate product；
(6) product of plasticating of step (5) mixes with 6 parts of polycarbonate resin, 50 parts of deionized water, is heated to 95 DEG C, stirs
3 parts of accelerator 2-ethyl-4-methylimidazole is added after mixing reaction 1.5h, then ultrasonic disperse 18min is decompressed to 0.03MPa, steamed
Go out low-boiling point material, obtain initial reaction product；
(7) initial reaction product of step (6) is added into double screw extruder, intermediate reaction product is obtained after melting extrusion
Thing, wherein double-screw extruder screw draw ratio are 20:1, double screw extruder extrusion temperature is：One 155 DEG C of area's temperature, 2nd area
Temperature is 175 DEG C, and three area's temperature are 215 DEG C, and four area's temperature are 240 DEG C；
(8) intermediate reaction product that obtains step (7) is added in autoclave, add 2 parts of dicyclopentadiene with
And appropriate deionized water, 3 parts of styrene is added after 25min is stirred in a nitrogen atmosphere, reactor pressure is lifted into 12MPa,
2 parts of the liquor potassic permanganate that dropwise addition concentration after 150 DEG C is 2.5% is warming up to by mixture, reaction under high pressure 40min is obtained most
End reaction product；
(9) by the final reacting product addition reaction vessel of step (8), processed through deaeration after being uniformly mixed, with
After be heated to 90 DEG C solidification 3.5h, after being finally warming up to 170 DEG C with the speed of 7 DEG C/min again, isothermal curing 2h is naturally cooled to
Mixed material is transferred in vulcanizing press in compressing, pelletizing at 180 DEG C after room temperature, obtains finished product.
The performance test results of obtained anti-flammability environment-friendlyinsulation insulation material are as shown in table 1.
Comparative example 3
(1) by 15 parts of semi-hydrated gypsum, 12 parts of perlite, 8 parts of mixing of bentonite, it is milled in addition planetary ball mill machine
Uniformly, it is that 80% glycerin solution is mixed to add 500mL concentration, is subsequently added in comminutor and is granulated, and is made grain
Footpath is 0.7 μm of particle；
(2) by 10 parts of EP rubbers, 6 parts of methylhydroxypropylcellulose sodium, 5 parts of stirring in 150rpm of phenyl glycidyl ether
Vacuum dehydration under the conditions of mixing, is subsequently added 5 parts of salethyl, and 120 DEG C are heated under nitrogen atmosphere, is warming up to after reaction 5h
150 DEG C, after maintaining 3h, 0.03MPa is evacuated to, maintains 27min, obtain vacuum reaction thing；
(3) by the particle obtained by step (1) and 10 parts of addition banburies of epoxy resin, it is well mixed, is 120 DEG C in temperature
Lower banburying 15min, obtains banburying product；
(4) by the banburying product obtained by step (3) and tetrahydrofuran 20 parts mix, obtain initial mixture；
(5) two roll plastic mixing mill is risen into high-temperature to 200 DEG C, by the initial mixture and polyamide wax micropowder 7 of step (4)
Part adds double roller intermediate melt to plasticate, and is added after it is well mixed between the vacuum reaction thing obtained by step (2), adjustment double roller
Away from, roll milling, it is thin it is logical be repeatedly well mixed the two, must plasticate product；
(6) product of plasticating of step (5) mixes with 6 parts of polycarbonate resin, 50 parts of deionized water, is heated to 100 DEG C, stirs
3 parts of accelerator 2-ethyl-4-methylimidazole is added after mixing reaction 2h, then ultrasonic disperse 20min is decompressed to 0.03MPa, steams
Low-boiling point material, obtains initial reaction product；
(7) initial reaction product of step (6) is added into double screw extruder, intermediate reaction product is obtained after melting extrusion
Thing, wherein double-screw extruder screw draw ratio are 20:1, double screw extruder extrusion temperature is：One 160 DEG C of area's temperature, 2nd area
Temperature is 180 DEG C, and three area's temperature are 220 DEG C, and four area's temperature are 250 DEG C；
(8) intermediate reaction product that obtains step (7) is added in autoclave, add 2 parts of dicyclopentadiene with
And appropriate deionized water, 3 parts of styrene is added after 25min is stirred in a nitrogen atmosphere, reactor pressure is lifted into 15MPa,
2 parts of the liquor potassic permanganate that dropwise addition concentration after 150 DEG C is 2.5% is warming up to by mixture, reaction under high pressure 45min is obtained most
End reaction product；
(9) by the final reacting product addition reaction vessel of step (8), 95 DEG C of solidification 4h are heated to, finally again with 7
DEG C/after the speed of min is warming up to 180 DEG C, mixed material is transferred to compression molding by isothermal curing 2h after naturally cooling to room temperature
In compressing, pelletizing at 180 DEG C in machine, finished product is obtained.
The performance test results of obtained anti-flammability environment-friendlyinsulation insulation material are as shown in table 1.
The obtained anti-flammability environment-friendlyinsulation insulation material of embodiment 1-3 and comparative example 1-3 is carried out into flame retardant rating, extension at break
Rate this two performance tests, and rubbed 500 test wear rates with abrasion meter.
Table 1
Anti-flammability environment-friendlyinsulation insulation material preparation technology of the invention carries out ball by by semi-hydrated gypsum, perlite, bentonite
Mill, granulation, then with the common banburying of epoxy resin, be subsequently adding tetrahydrofuran vacuum stirring, add polyamide wax micropowder with
And by EP rubbers, methylhydroxypropylcellulose sodium, phenyl glycidyl ether, through the vacuum obtained by dehydration, heating, vacuum reaction
Reactant, through plasticating, feeding, ultrasound, reduction vaporization, Screw Extrusion, reaction under high pressure, deaeration solidification, compressing, pelletizing etc.
Serial special process is made finished product.The insulating materials being prepared from, it has excellent fire resistance and mechanical strength concurrently, with compared with
Good application prospect.Anti-flammability environment-friendlyinsulation insulation material raw material of the invention is cheap, process is simple, is suitable to heavy industrialization fortune
With practical.
Embodiments of the invention are the foregoing is only, the scope of the claims of the invention is not thereby limited, it is every to utilize this hair
Equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, is included within the scope of the present invention.
Claims (5)
1. a kind of preparation method of anti-flammability environment-friendlyinsulation insulation material, it is characterised in that comprise the following steps：
(1) by 15 parts of semi-hydrated gypsum, 12 parts of perlite, 8 parts of mixing of bentonite, it is milled in addition planetary ball mill machine
Even, it is that 80% glycerin solution is mixed to add 500mL concentration, is subsequently added in comminutor and is granulated, and is made particle diameter
It is 0.6-0.8 μm of particle；
(2) by 10 parts of EP rubbers, 6 parts of methylhydroxypropylcellulose sodium, 5 parts of stirring bars in 150rpm of phenyl glycidyl ether
Vacuum dehydration under part, is subsequently added 5 parts of salethyl, and 120 DEG C are heated under nitrogen atmosphere, is warming up to after reaction 3-5h
150 DEG C, after maintaining 2-3h, 0.01-0.03MPa is evacuated to, maintains 27min, obtain vacuum reaction thing；
(3) by the particle obtained by step (1) and 10 parts of addition banburies of epoxy resin, it is well mixed, is 110-120 DEG C in temperature
Lower banburying 10-15min, obtains banburying product；
(4) by the banburying product obtained by step (3) and tetrahydrofuran 20 parts mix, insert vacuum mixer and be stirred under vacuum
10min, then stands 15min, obtains initial mixture；
(5) two roll plastic mixing mill is risen into high-temperature to 180-200 DEG C, by the initial mixture and polyamide wax micropowder 7 of step (4)
Part adds double roller intermediate melt to plasticate, and is added after it is well mixed between the vacuum reaction thing obtained by step (2), adjustment double roller
Away from, roll milling, it is thin it is logical be repeatedly well mixed the two, must plasticate product；
(6) product of plasticating of step (5) mixes with 6 parts of polycarbonate resin, 50 parts of deionized water, is heated to 90-100 DEG C, stirs
3 parts of accelerator 2-ethyl-4-methylimidazole is added after mixing reaction 1-2h, then ultrasonic disperse 15-20min is decompressed to
0.03MPa, steams low-boiling point material, obtains initial reaction product；
(7) initial reaction product of step (6) is added into double screw extruder, intermediate reaction product is obtained after melting extrusion, its
Middle double-screw extruder screw draw ratio is 20:1；
(8) intermediate reaction product for obtaining step (7) is added in autoclave, is added 2 parts of dicyclopentadiene and is fitted
The deionized water of amount, 3 parts of styrene is added after 25min is stirred in a nitrogen atmosphere, and reactor pressure is lifted into 15MPa, extremely will
Mixture is added dropwise 2 parts of liquor potassic permanganate after being warming up to 150 DEG C, and reaction under high pressure 35-45min obtains final reacting product；
(9) by the final reacting product addition reaction vessel of step (8), processed through deaeration after being uniformly mixed, then added
Hot to 85-95 DEG C solidification 3-4h, after being finally warming up to 160-180 DEG C with the speed of 7 DEG C/min again, isothermal curing 1.5-2h, from
So it is cooled to after room temperature and mixed material is transferred in vulcanizing press in compressing, pelletizing at 180 DEG C, obtains finished product.
2. the preparation method of anti-flammability environment-friendlyinsulation insulation material according to claim 1, it is characterised in that the step (1)
The particle diameter of middle particle is 0.7 μm.
3. the preparation method of anti-flammability environment-friendlyinsulation insulation material according to claim 1, it is characterised in that the step (7)
Middle double screw extruder extrusion temperature is：One 150-160 DEG C of area's temperature, two area's temperature are 170-180 DEG C, and three area's temperature are 210-
220 DEG C, four area's temperature are 230-250 DEG C.
4. the preparation method of anti-flammability environment-friendlyinsulation insulation material according to claim 1, it is characterised in that the step (8)
The concentration of middle liquor potassic permanganate is preferably 2.5%.
5. the anti-flammability environment-friendlyinsulation insulation material that the preparation technology according to claim any one of 1-4 is obtained is in power industry
Using.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108395673A (en) * | 2018-03-14 | 2018-08-14 | 合肥尚强电气科技有限公司 | A kind of preparation method of insulating materials for power equipment |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101434728A (en) * | 2008-12-04 | 2009-05-20 | 黑龙江沃尔德电缆有限公司 | Ultraviolet light crosslinked EPT rubber cable insulation material and preparation thereof |
| CN105348739A (en) * | 2015-11-25 | 2016-02-24 | 国网河南唐河县供电公司 | Special insulating material for electrical equipment and preparation method for special insulating material |
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2017
- 2017-03-01 CN CN201710117010.7A patent/CN106905618A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101434728A (en) * | 2008-12-04 | 2009-05-20 | 黑龙江沃尔德电缆有限公司 | Ultraviolet light crosslinked EPT rubber cable insulation material and preparation thereof |
| CN105348739A (en) * | 2015-11-25 | 2016-02-24 | 国网河南唐河县供电公司 | Special insulating material for electrical equipment and preparation method for special insulating material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108395673A (en) * | 2018-03-14 | 2018-08-14 | 合肥尚强电气科技有限公司 | A kind of preparation method of insulating materials for power equipment |
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