CN107586408A - A kind of fire protection flame retarding polythene material and preparation method thereof - Google Patents
A kind of fire protection flame retarding polythene material and preparation method thereof Download PDFInfo
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Abstract
The invention is related to a kind of fire protection flame retarding polythene material, including following raw material components：Polyethylene, retardation PES hot melt adhesive coats ferric sulfate, polyacrylate coats iron chloride, porous di-iron trioxide, the own ester cladding iron ammonium sulfate of polyacrylic acid, the different certain herbaceous plants with big flowers ester of pentaerythritol diphosphite two, barium stearate, retardation PES hot melt adhesive coats ferric sulfate by ferric sulfate, retardation PES hot melt adhesive, polyvinyl alcohol and cupric oxide reaction are made, polyacrylate coats iron chloride by iron chloride, acrylic acid, Isooctyl acrylate monomer, butyl acrylate and benzoin methyl ether reaction are made, porous di-iron trioxide is by iron powder, zinc powder, zinc oxide and zinc oxalate reaction are made, the own ester of polyacrylic acid coats iron ammonium sulfate by iron ammonium sulfate, Hexyl 2-propenoate, methyl acrylate and benzoin methyl ether reaction are made.The invention has excellent fire resistance and fire protecting performance.
Description
Technical field
The invention is related to a kind of fire protection flame retarding polythene material and preparation method thereof.
Background technology
Polythene material is a kind of plastic material, is suitable for thermoplastic molding and is processed into various plastic products, has processing
The advantage such as good moldability, transparent, inexpensive, chemical inertness, nontoxic, good airproof performance, is widely used in packaging for foodstuff, Medical treatment device
The fields such as tool, handicraft, electric wire, cable, chemical pipeline.
At present, polythene material needs further lifting in fire resistance and fire protecting performance.The invention using polyethylene,
Retardation PES hot melt adhesive cladding ferric sulfate, polyacrylate cladding iron chloride, porous di-iron trioxide, the own ester cladding sulfuric acid of polyacrylic acid
Ferrous ammonium is prepared for fire protection flame retarding polythene material, by extruding, being molded, being molded, the technique such as being blow molded and be prepared into various plastics systems
Product, fire protection flame retarding polythene material prepared by this method have excellent fire resistance and fire protecting performance.
The content of the invention
The purpose of the invention is to provide a kind of preparation method of fire protection flame retarding polythene material, and this method is anti-by changing
Raw material and technology mode are answered, the material of preparation has excellent fire resistance and fire protecting performance.
To achieve these goals, the technical scheme of the invention is as follows.
A kind of fire protection flame retarding polythene material and preparation method thereof, specifically includes following steps：(1), by iron ammonium sulfate,
Hexyl 2-propenoate, methyl acrylate and benzoin methyl ether are 50 according to quality parts ratio：35~53：10~26：0.5~1 adds
Into reactor, mixing speed is 65~78r/min, 20min is reacted under the conditions of 25~37 DEG C of maintenance system temperature, through 2000W
1~7s of lamp and high pressure mercury, obtain the own ester cladding iron ammonium sulfate of polyacrylic acid；(2), by iron powder, zinc powder, zinc oxide and oxalic acid
Zinc is according to quality parts ratio 50：35~43：80~97：31~44 are added in ball mill, and drum speed is 30~45r/min,
30min is reacted under the conditions of 35~46 DEG C of maintenance system temperature, product is through 200 DEG C of roasting 2h, and 300 DEG C of roasting 2h, 400 DEG C are calcined
2h, 500 DEG C of roasting 3h, product wash 45min through the 1000mL 10mol/L NaOH aqueous solution, filtering, 500mL water washings 3 times,
500mL ethanol washs 3 times, in 53 DEG C, -0.07MPa vacuum drying 14min, obtains porous di-iron trioxide；(3), by chlorination
Iron, acrylic acid, Isooctyl acrylate monomer, butyl acrylate and benzoin methyl ether are according to quality parts ratio 50：6~12：26~35：13
~27：0.3~1 is added in reactor, and mixing speed is 85~100r/min, under the conditions of 28~36 DEG C of maintenance system temperature
25min is reacted, through 3000W 1~5s of lamp and high pressure mercury, that is, obtains polyacrylate cladding iron chloride；(4), by ferric sulfate,
Retardation PES hot melt adhesive, polyvinyl alcohol and cupric oxide are according to quality parts ratio 70：18~26：2~7：5~9 are added to high-speed mixer
In, mixing velocity 500r/min, 2~6min is reacted under the conditions of 160 DEG C of maintenance system temperature, that is, obtain retardation PES hot melt adhesive cladding
Ferric sulfate；(5), by polyethylene, retardation PES hot melt adhesive coat ferric sulfate, polyacrylate coat iron chloride, porous di-iron trioxide,
The own ester cladding iron ammonium sulfate of polyacrylic acid, the different certain herbaceous plants with big flowers ester of pentaerythritol diphosphite two, barium stearate are according to quality parts ratio
60：38~46：31~39：33~45：23~31：3~6：2~7 are added in high-speed mixer, with high-speed mixer in temperature
170 DEG C of 2~8min of hybrid reaction, with extruder in 173~180 DEG C of extruding pelletizations of temperature, that is, obtain fire protection flame retarding polyethylene material
Material.
The preparation method of fire protection flame retarding polythene material described in the invention, comprises the following steps：
(1) it is, 50 according to quality parts ratio by iron ammonium sulfate, Hexyl 2-propenoate, methyl acrylate and benzoin methyl ether：35~
53：10~26：0.5~1 is added in reactor, and mixing speed is 65~78r/min, 25~37 DEG C of bars of maintenance system temperature
20min is reacted under part, through 2000W 1~7s of lamp and high pressure mercury, obtains the own ester cladding iron ammonium sulfate of polyacrylic acid；Described
The purpose of iron ammonium sulfate is in order to improve the fire prevention of polyethylene and fire resistance.
(2), by iron powder, zinc powder, zinc oxide and zinc oxalate according to quality parts ratio 50：35~43：80~97：31~44 add
Enter into ball mill, drum speed is 30~45r/min, reacts 30min, product under the conditions of 35~46 DEG C of maintenance system temperature
Through 200 DEG C of roasting 2h, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 3h, product is through 1000mL 10mol/L NaOH water
Solution washs 45min, and filtering, 500mL water washings 3 times, 500mL ethanol wash 3 times, are dried in vacuo in 53 DEG C, -0.07MPa
14min, obtain porous di-iron trioxide；The purpose of described zinc powder, zinc oxide and zinc oxalate is in order to improve di-iron trioxide
Porosity.
(3), by iron chloride, acrylic acid, Isooctyl acrylate monomer, butyl acrylate and benzoin methyl ether according to quality parts ratio
50：6~12：26~35：13~27：0.3~1 is added in reactor, and mixing speed is 85~100r/min, maintenance system temperature
25min is reacted under the conditions of 28~36 DEG C of degree, through 3000W 1~5s of lamp and high pressure mercury, that is, obtains polyacrylate cladding chlorination
Iron；The purpose of described iron chloride is in order to improve the fire-retardant and fire protecting performance of polyethylene.
(4), by ferric sulfate, retardation PES hot melt adhesive, polyvinyl alcohol and cupric oxide according to quality parts ratio 70：18~26：2~7：5
~9 are added in high-speed mixer, mixing velocity 500r/min, and 2~6min is reacted under the conditions of 160 DEG C of maintenance system temperature,
Obtain retardation PES hot melt adhesive cladding ferric sulfate；The purpose of described ferric sulfate is in order to improve the fire-retardant and fire protecting performance of polyethylene.
(5), by polyethylene, retardation PES hot melt adhesive coat ferric sulfate, polyacrylate coat iron chloride, porous di-iron trioxide,
The own ester cladding iron ammonium sulfate of polyacrylic acid, the different certain herbaceous plants with big flowers ester of pentaerythritol diphosphite two, barium stearate are according to quality parts ratio
60：38~46：31~39：33~45：23~31：3~6：2~7 are added in high-speed mixer, with high-speed mixer in temperature
170 DEG C of 2~8min of hybrid reaction, with extruder in 173~180 DEG C of extruding pelletizations of temperature, that is, obtain fire protection flame retarding polyethylene material
Material.
The beneficial effect of the invention is：
1st, iron ammonium sulfate is water-soluble material, and the own ester cladding of polyacrylic acid can improve the hydrophobicity of iron ammonium sulfate and hypotonic water
Performance, when polyethylene burns or caught fire, iron ammonium sulfate can consume the oxygen of polyethylene surface, meanwhile, iron ammonium sulfate point
Ammonia caused by solution can form layer of inert in polyethylene surface, slow down the burn rate and ignition rate of polyethylene, so as to,
The own ester cladding iron ammonium sulfate of polyacrylic acid can improve the fire-retardant and fire protecting performance of polyethylene；
2nd, iron powder can be well dispersed in zinc powder, zinc oxide and zinc oxalate by ball-milling reaction by zinc powder, zinc oxide and zinc oxalate,
Being handled by high-temperature roasting, obtain the mixture of zinc oxide and di-iron trioxide, zinc oxide can be dissolved in strong base solution, from
And porous di-iron trioxide is prepared, porous di-iron trioxide can improve the fire-retardant of polyethylene and fire prevention by porous heat-insulating effect
Performance；
3rd, iron chloride is water-soluble material, and polyacrylate coats the hydrophobicity and low water permeability energy that can improve iron chloride, poly-
Ethylene combustion or when catching fire, iron chloride can generate poly-ferric chloride in the case of heated in polyethylene surface, prevent polyethylene table
The burning in face, so as to which polyacrylate cladding iron chloride improves the fire-retardant and fire protecting performance of polyethylene；
4th, ferric sulfate is water-soluble material, and retardation PES hot melt adhesive coats the hydrophobicity and low water permeability energy that can improve ferric sulfate, in poly- second
When alkene burns or caught fire, ferric sulfate can generate bodied ferric sulfate in the case of heated in polyethylene surface, prevent polyethylene surface
Burning, so as to which, retardation PES hot melt adhesive cladding ferric sulfate improves the fire-retardant and fire protecting performance of polyethylene；
5th, in polyethylene, retardation PES hot melt adhesive cladding ferric sulfate, polyacrylate cladding iron chloride, porous di-iron trioxide, polypropylene
Under the synergy of the own ester cladding iron ammonium sulfate of acid, assign polyethylene excellent fire-retardant and fire protecting performance.
Embodiment
The embodiment of the invention is described with reference to embodiment, to be better understood from the invention.
Embodiment 1
A kind of fire protection flame retarding polythene material, its preparation method comprise the following steps：
(1) 50 parts of iron ammonium sulfates, 38 parts of Hexyl 2-propenoates, 17 parts of methyl acrylates and 0.5 part of benzoin methyl ether, is weighed to add
Into reactor, mixing speed 70r/min, 20min is reacted under the conditions of 27 DEG C of maintenance system temperature, through 2000W high-pressure sodium lamps
Illumination 2s, obtain the own ester cladding iron ammonium sulfate of polyacrylic acid；
(2), weigh 50 parts of iron powders, 38 parts of zinc powders, 85 parts of zinc oxide and 35 parts of zinc oxalates to be added in ball mill, drum speed is
35r/min, reacts 30min under the conditions of 36 DEG C of maintenance system temperature, and product is through 200 DEG C of roasting 2h, 300 DEG C of roasting 2h, 400 DEG C
2h, 500 DEG C of roasting 3h are calcined, product washs 45min, filtering, 500mL water washings 3 through the 1000mL 10mol/L NaOH aqueous solution
Secondary, 500mL ethanol washs 3 times, in 53 DEG C, -0.07MPa vacuum drying 14min, obtains porous di-iron trioxide；
(3) 50 parts of iron chloride, 8 parts of acrylic acid, 29 parts of Isooctyl acrylate monomers, 18 parts of butyl acrylates and 0.4 part of styrax, are weighed
Methyl ether is added in reactor, mixing speed 90r/min, 25min is reacted under the conditions of 30 DEG C of maintenance system temperature, through 3000W
Lamp and high pressure mercury 2s, that is, obtain polyacrylate cladding iron chloride；
(4) 70 parts of ferric sulfate, 20 parts of retardation PES hot melt adhesives, 4 parts of polyvinyl alcohol and 6 parts of cupric oxide, are weighed and are added to high-speed mixer
In, mixing velocity 500r/min, 3min is reacted under the conditions of 160 DEG C of maintenance system temperature, that is, obtain retardation PES hot melt adhesive cladding sulphur
Sour iron；
(5) 60 parts of polyethylene, are weighed, 41 parts of retardation PES hot melt adhesives coat ferric sulfate, 36 parts of polyacrylate coat iron chloride, 40 parts
The own ester cladding iron ammonium sulfate of porous di-iron trioxide, 26 parts of polyacrylic acid, the different certain herbaceous plants with big flowers ester of 4 parts of pentaerythritol diphosphites two, 5
Part barium stearate is added in high-speed mixer, with high-speed mixer in 170 DEG C of hybrid reaction 3min of temperature, with extruder in temperature
176 DEG C of extruding pelletizations are spent, that is, obtain fire protection flame retarding polythene material.
Embodiment 2
A kind of fire protection flame retarding polythene material, its preparation method comprise the following steps：
(1) 50 parts of iron ammonium sulfates, 35 parts of Hexyl 2-propenoates, 10 parts of methyl acrylates and 0.5 part of benzoin methyl ether, is weighed to add
Into reactor, mixing speed 65r/min, 20min is reacted under the conditions of 25 DEG C of maintenance system temperature, through 2000W high-pressure sodium lamps
Illumination 7s, obtain the own ester cladding iron ammonium sulfate of polyacrylic acid；
(2), weigh 50 parts of iron powders, 35 parts of zinc powders, 80 parts of zinc oxide and 31 parts of zinc oxalates to be added in ball mill, drum speed is
30r/min, reacts 30min under the conditions of 35 DEG C of maintenance system temperature, and product is through 200 DEG C of roasting 2h, 300 DEG C of roasting 2h, 400 DEG C
2h, 500 DEG C of roasting 3h are calcined, product washs 45min, filtering, 500mL water washings 3 through the 1000mL 10mol/L NaOH aqueous solution
Secondary, 500mL ethanol washs 3 times, in 53 DEG C, -0.07MPa vacuum drying 14min, obtains porous di-iron trioxide；
(3) 50 parts of iron chloride, 6 parts of acrylic acid, 26 parts of Isooctyl acrylate monomers, 13 parts of butyl acrylates and 0.3 part of styrax, are weighed
Methyl ether is added in reactor, mixing speed 85r/min, 25min is reacted under the conditions of 28 DEG C of maintenance system temperature, through 3000W
Lamp and high pressure mercury 5s, that is, obtain polyacrylate cladding iron chloride；
(4) 70 parts of ferric sulfate, 18 parts of retardation PES hot melt adhesives, 2 parts of polyvinyl alcohol and 5 parts of cupric oxide, are weighed and are added to high-speed mixer
In, mixing velocity 500r/min, 2min is reacted under the conditions of 160 DEG C of maintenance system temperature, that is, obtain retardation PES hot melt adhesive cladding sulphur
Sour iron；
(5) 60 parts of polyethylene, are weighed, 38 parts of retardation PES hot melt adhesives coat ferric sulfate, 31 parts of polyacrylate coat iron chloride, 33 parts
The own ester cladding iron ammonium sulfate of porous di-iron trioxide, 23 parts of polyacrylic acid, the different certain herbaceous plants with big flowers ester of 3 parts of pentaerythritol diphosphites two, 2
Part barium stearate is added in high-speed mixer, with high-speed mixer in 170 DEG C of hybrid reaction 2min of temperature, with extruder in temperature
173 DEG C of extruding pelletizations are spent, that is, obtain fire protection flame retarding polythene material.
Embodiment 3
A kind of fire protection flame retarding polythene material, its preparation method comprise the following steps：
(1) 50 parts of iron ammonium sulfates, 53 parts of Hexyl 2-propenoates, 26 parts of methyl acrylates and 1 part of benzoin methyl ether, is weighed to be added to
In reactor, mixing speed 78r/min, 20min is reacted under the conditions of 37 DEG C of maintenance system temperature, through 2000W high-pressure mercury light
According to 1, the own ester cladding iron ammonium sulfate of polyacrylic acid is obtained；
(2), weigh 50 parts of iron powders, 43 parts of zinc powders, 97 parts of zinc oxide and 44 parts of zinc oxalates to be added in ball mill, drum speed is
45r/min, reacts 30min under the conditions of 46 DEG C of maintenance system temperature, and product is through 200 DEG C of roasting 2h, 300 DEG C of roasting 2h, 400 DEG C
2h, 500 DEG C of roasting 3h are calcined, product washs 45min, filtering, 500mL water washings 3 through the 1000mL 10mol/L NaOH aqueous solution
Secondary, 500mL ethanol washs 3 times, in 53 DEG C, -0.07MPa vacuum drying 14min, obtains porous di-iron trioxide；
(3) 50 parts of iron chloride, 12 parts of acrylic acid, 35 parts of Isooctyl acrylate monomers, 27 parts of butyl acrylates and 1 part of styrax, are weighed
Methyl ether is added in reactor, mixing speed 100r/min, reacts 25min under the conditions of 36 DEG C of maintenance system temperature, warp
3000W lamp and high pressure mercury 1s, that is, obtain polyacrylate cladding iron chloride；
(4) 70 parts of ferric sulfate, 26 parts of retardation PES hot melt adhesives, 7 parts of polyvinyl alcohol and 9 parts of cupric oxide, are weighed and are added to high-speed mixer
In, mixing velocity 500r/min, 6min is reacted under the conditions of 160 DEG C of maintenance system temperature, that is, obtain retardation PES hot melt adhesive cladding sulphur
Sour iron；
(5) 60 parts of polyethylene, are weighed, 46 parts of retardation PES hot melt adhesives coat ferric sulfate, 39 parts of polyacrylate coat iron chloride, 45 parts
The own ester cladding iron ammonium sulfate of porous di-iron trioxide, 31 parts of polyacrylic acid, the different certain herbaceous plants with big flowers ester of 6 parts of pentaerythritol diphosphites two, 7
Part barium stearate is added in high-speed mixer, with high-speed mixer in 170 DEG C of hybrid reaction 8min of temperature, with extruder in temperature
180 DEG C of extruding pelletizations are spent, that is, obtain fire protection flame retarding polythene material.
Embodiment 4
A kind of fire protection flame retarding polythene material, its preparation method comprise the following steps：
(1) 50 parts of iron ammonium sulfates, 40 parts of Hexyl 2-propenoates, 15 parts of methyl acrylates and 0.7 part of benzoin methyl ether, is weighed to add
Into reactor, mixing speed 70r/min, 20min is reacted under the conditions of 30 DEG C of maintenance system temperature, through 2000W high-pressure sodium lamps
Illumination 3s, obtain the own ester cladding iron ammonium sulfate of polyacrylic acid；
(2), weigh 50 parts of iron powders, 39 parts of zinc powders, 85 parts of zinc oxide and 36 parts of zinc oxalates to be added in ball mill, drum speed is
36r/min, reacts 30min under the conditions of 38 DEG C of maintenance system temperature, and product is through 200 DEG C of roasting 2h, 300 DEG C of roasting 2h, 400 DEG C
2h, 500 DEG C of roasting 3h are calcined, product washs 45min, filtering, 500mL water washings 3 through the 1000mL 10mol/L NaOH aqueous solution
Secondary, 500mL ethanol washs 3 times, in 53 DEG C, -0.07MPa vacuum drying 14min, obtains porous di-iron trioxide；
(3) 50 parts of iron chloride, are weighed, 10 parts of acrylic acid, 28 parts of Isooctyl acrylate monomers, 15 parts of butyl acrylates and 0.5 part are rested in peace
Fragrant methyl ether is added in reactor, mixing speed 90r/min, reacts 25min under the conditions of 30 DEG C of maintenance system temperature, warp
3000W lamp and high pressure mercury 2s, that is, obtain polyacrylate cladding iron chloride；
(4) 70 parts of ferric sulfate, 20 parts of retardation PES hot melt adhesives, 5 parts of polyvinyl alcohol and 6 parts of cupric oxide, are weighed and are added to high-speed mixer
In, mixing velocity 500r/min, 3min is reacted under the conditions of 160 DEG C of maintenance system temperature, that is, obtain retardation PES hot melt adhesive cladding sulphur
Sour iron；
(5) 60 parts of polyethylene, are weighed, 45 parts of retardation PES hot melt adhesives coat ferric sulfate, 35 parts of polyacrylate coat iron chloride, 40 parts
The own ester cladding iron ammonium sulfate of porous di-iron trioxide, 27 parts of polyacrylic acid, the different certain herbaceous plants with big flowers ester of 4 parts of pentaerythritol diphosphites two, 5
Part barium stearate is added in high-speed mixer, with high-speed mixer in 170 DEG C of hybrid reaction 4min of temperature, with extruder in temperature
176 DEG C of extruding pelletizations are spent, that is, obtain fire protection flame retarding polythene material.
Embodiment 5
A kind of fire protection flame retarding polythene material, its preparation method comprise the following steps：
(1) 50 parts of iron ammonium sulfates, 44 parts of Hexyl 2-propenoates, 17 parts of methyl acrylates and 0.8 part of benzoin methyl ether, is weighed to add
Into reactor, mixing speed 73r/min, 20min is reacted under the conditions of 33 DEG C of maintenance system temperature, through 2000W high-pressure sodium lamps
Illumination 6s, obtain the own ester cladding iron ammonium sulfate of polyacrylic acid；
(2), weigh 50 parts of iron powders, 41 parts of zinc powders, 92 parts of zinc oxide and 40 parts of zinc oxalates to be added in ball mill, drum speed is
43r/min, reacts 30min under the conditions of 45 DEG C of maintenance system temperature, and product is through 200 DEG C of roasting 2h, 300 DEG C of roasting 2h, 400 DEG C
2h, 500 DEG C of roasting 3h are calcined, product washs 45min, filtering, 500mL water washings 3 through the 1000mL 10mol/L NaOH aqueous solution
Secondary, 500mL ethanol washs 3 times, in 53 DEG C, -0.07MPa vacuum drying 14min, obtains porous di-iron trioxide；
(3) 50 parts of iron chloride, are weighed, 11 parts of acrylic acid, 33 parts of Isooctyl acrylate monomers, 26 parts of butyl acrylates and 0.6 part are rested in peace
Fragrant methyl ether is added in reactor, mixing speed 96r/min, reacts 25min under the conditions of 29 DEG C of maintenance system temperature, warp
3000W lamp and high pressure mercury 4s, that is, obtain polyacrylate cladding iron chloride；
(4) 70 parts of ferric sulfate, 23 parts of retardation PES hot melt adhesives, 6 parts of polyvinyl alcohol and 7 parts of cupric oxide, are weighed and are added to high-speed mixer
In, mixing velocity 500r/min, 4min is reacted under the conditions of 160 DEG C of maintenance system temperature, that is, obtain retardation PES hot melt adhesive cladding sulphur
Sour iron；
(5) 60 parts of polyethylene, are weighed, 39 parts of retardation PES hot melt adhesives coat ferric sulfate, 37 parts of polyacrylate coat iron chloride, 44 parts
The own ester cladding iron ammonium sulfate of porous di-iron trioxide, 30 parts of polyacrylic acid, the different certain herbaceous plants with big flowers ester of 4 parts of pentaerythritol diphosphites two, 6
Part barium stearate is added in high-speed mixer, with high-speed mixer in 170 DEG C of hybrid reaction 4min of temperature, with extruder in temperature
179 DEG C of extruding pelletizations are spent, that is, obtain fire protection flame retarding polythene material.
Embodiment 6
A kind of fire protection flame retarding polythene material, its preparation method comprise the following steps：
(1) 50 parts of iron ammonium sulfates, 43 parts of Hexyl 2-propenoates, 19 parts of methyl acrylates and 0.6 part of benzoin methyl ether, is weighed to add
Into reactor, mixing speed 58r/min, 20min is reacted under the conditions of 30 DEG C of maintenance system temperature, through 2000W high-pressure sodium lamps
Illumination 7s, obtain the own ester cladding iron ammonium sulfate of polyacrylic acid；
(2), weigh 50 parts of iron powders, 36 parts of zinc powders, 87 parts of zinc oxide and 33 parts of zinc oxalates to be added in ball mill, drum speed is
37r/min, reacts 30min under the conditions of 36 DEG C of maintenance system temperature, and product is through 200 DEG C of roasting 2h, 300 DEG C of roasting 2h, 400 DEG C
2h, 500 DEG C of roasting 3h are calcined, product washs 45min, filtering, 500mL water washings 3 through the 1000mL 10mol/L NaOH aqueous solution
Secondary, 500mL ethanol washs 3 times, in 53 DEG C, -0.07MPa vacuum drying 14min, obtains porous di-iron trioxide；
(3) 50 parts of iron chloride, are weighed, 11 parts of acrylic acid, 31 parts of Isooctyl acrylate monomers, 14 parts of butyl acrylates and 0.7 part are rested in peace
Fragrant methyl ether is added in reactor, mixing speed 93r/min, reacts 25min under the conditions of 32 DEG C of maintenance system temperature, warp
3000W lamp and high pressure mercury 2s, that is, obtain polyacrylate cladding iron chloride；
(4) 70 parts of ferric sulfate, 19 parts of retardation PES hot melt adhesives, 6 parts of polyvinyl alcohol and 7 parts of cupric oxide, are weighed and are added to high-speed mixer
In, mixing velocity 500r/min, 3min is reacted under the conditions of 160 DEG C of maintenance system temperature, that is, obtain retardation PES hot melt adhesive cladding sulphur
Sour iron；
(5) 60 parts of polyethylene, are weighed, 44 parts of retardation PES hot melt adhesives coat ferric sulfate, 32 parts of polyacrylate coat iron chloride, 41 parts
The own ester cladding iron ammonium sulfate of porous di-iron trioxide, 30 parts of polyacrylic acid, the different certain herbaceous plants with big flowers ester of 5 parts of pentaerythritol diphosphites two, 6
Part barium stearate is added in high-speed mixer, with high-speed mixer in 170 DEG C of hybrid reaction 7min of temperature, with extruder in temperature
174 DEG C of extruding pelletizations are spent, that is, obtain fire protection flame retarding polythene material.
Embodiment 7
A kind of fire protection flame retarding polythene material, its preparation method comprise the following steps：
(1) 50 parts of iron ammonium sulfates, 50 parts of Hexyl 2-propenoates, 12 parts of methyl acrylates and 0.7 part of benzoin methyl ether, is weighed to add
Into reactor, mixing speed 76r/min, 20min is reacted under the conditions of 29 DEG C of maintenance system temperature, through 2000W high-pressure sodium lamps
Illumination 3s, obtain the own ester cladding iron ammonium sulfate of polyacrylic acid；
(2), weigh 50 parts of iron powders, 41 parts of zinc powders, 96 parts of zinc oxide and 37 parts of zinc oxalates to be added in ball mill, drum speed is
44r/min, reacts 30min under the conditions of 40 DEG C of maintenance system temperature, and product is through 200 DEG C of roasting 2h, 300 DEG C of roasting 2h, 400 DEG C
2h, 500 DEG C of roasting 3h are calcined, product washs 45min, filtering, 500mL water washings 3 through the 1000mL 10mol/L NaOH aqueous solution
Secondary, 500mL ethanol washs 3 times, in 53 DEG C, -0.07MPa vacuum drying 14min, obtains porous di-iron trioxide；
(3) 50 parts of iron chloride, 8 parts of acrylic acid, 28 parts of Isooctyl acrylate monomers, 19 parts of butyl acrylates and 0.6 part of styrax, are weighed
Methyl ether is added in reactor, mixing speed 97r/min, 25min is reacted under the conditions of 34 DEG C of maintenance system temperature, through 3000W
Lamp and high pressure mercury 3s, that is, obtain polyacrylate cladding iron chloride；
(4) 70 parts of ferric sulfate, 23 parts of retardation PES hot melt adhesives, 4 parts of polyvinyl alcohol and 7 parts of cupric oxide, are weighed and are added to high-speed mixer
In, mixing velocity 500r/min, 3min is reacted under the conditions of 160 DEG C of maintenance system temperature, that is, obtain retardation PES hot melt adhesive cladding sulphur
Sour iron；
(5) 60 parts of polyethylene, are weighed, 45 parts of retardation PES hot melt adhesives coat ferric sulfate, 38 parts of polyacrylate coat iron chloride, 41 parts
The own ester cladding iron ammonium sulfate of porous di-iron trioxide, 27 parts of polyacrylic acid, the different certain herbaceous plants with big flowers ester of 5 parts of pentaerythritol diphosphites two, 4
Part barium stearate is added in high-speed mixer, with high-speed mixer in 170 DEG C of hybrid reaction 3min of temperature, with extruder in temperature
176 DEG C of extruding pelletizations are spent, that is, obtain fire protection flame retarding polythene material.
Embodiment 8
A kind of fire protection flame retarding polythene material, its preparation method comprise the following steps：
(1) 50 parts of iron ammonium sulfates, 39 parts of Hexyl 2-propenoates, 19 parts of methyl acrylates and 0.7 part of benzoin methyl ether, is weighed to add
Into reactor, mixing speed 72r/min, 20min is reacted under the conditions of 35 DEG C of maintenance system temperature, through 2000W high-pressure sodium lamps
Illumination 3s, obtain the own ester cladding iron ammonium sulfate of polyacrylic acid；
(2), weigh 50 parts of iron powders, 41 parts of zinc powders, 96 parts of zinc oxide and 43 parts of zinc oxalates to be added in ball mill, drum speed is
44r/min, reacts 30min under the conditions of 41 DEG C of maintenance system temperature, and product is through 200 DEG C of roasting 2h, 300 DEG C of roasting 2h, 400 DEG C
2h, 500 DEG C of roasting 3h are calcined, product washs 45min, filtering, 500mL water washings 3 through the 1000mL 10mol/L NaOH aqueous solution
Secondary, 500mL ethanol washs 3 times, in 53 DEG C, -0.07MPa vacuum drying 14min, obtains porous di-iron trioxide；
(3) 50 parts of iron chloride, are weighed, 10 parts of acrylic acid, 34 parts of Isooctyl acrylate monomers, 26 parts of butyl acrylates and 0.6 part are rested in peace
Fragrant methyl ether is added in reactor, mixing speed 91r/min, reacts 25min under the conditions of 35 DEG C of maintenance system temperature, warp
3000W lamp and high pressure mercury 2s, that is, obtain polyacrylate cladding iron chloride；
(4) 70 parts of ferric sulfate, 25 parts of retardation PES hot melt adhesives, 6 parts of polyvinyl alcohol and 6 parts of cupric oxide, are weighed and are added to high-speed mixer
In, mixing velocity 500r/min, 4min is reacted under the conditions of 160 DEG C of maintenance system temperature, that is, obtain retardation PES hot melt adhesive cladding sulphur
Sour iron；
(5) 60 parts of polyethylene, are weighed, 39 parts of retardation PES hot melt adhesives coat ferric sulfate, 32 parts of polyacrylate coat iron chloride, 44 parts
The own ester cladding iron ammonium sulfate of porous di-iron trioxide, 30 parts of polyacrylic acid, the different certain herbaceous plants with big flowers ester of 5 parts of pentaerythritol diphosphites two, 4
Part barium stearate is added in high-speed mixer, with high-speed mixer in 170 DEG C of hybrid reaction 6min of temperature, with extruder in temperature
178 DEG C of extruding pelletizations are spent, that is, obtain fire protection flame retarding polythene material.
Reference examples 1
In this reference examples, the own ester cladding iron ammonium sulfate of polyacrylic acid, other components and preparation method and the phase of embodiment 1 are not added
Together.
Reference examples 2
In this reference examples, porous di-iron trioxide is not added, and other components and preparation method are same as Example 1.
Reference examples 3
In this reference examples, polyacrylate cladding iron chloride is not added, other components and preparation method are same as Example 1.
Reference examples 4
In this reference examples, retardation PES hot melt adhesive cladding ferric sulfate is not added, other components and preparation method are same as Example 1.
Reference examples 5
In this reference examples, the own ester cladding sulfuric acid of polyacrylic acid selected in formula in common iron ammonium sulfate alternate embodiment 1 is sub-
Iron ammonium, other components and preparation method are same as Example 1.
Reference examples 6
In this reference examples, from the porous di-iron trioxide in common di-iron trioxide alternate embodiment 1, other components in formula
It is same as Example 1 with preparation method.
Reference examples 7
The polyacrylate cladding iron chloride selected in this reference examples, in formula in common iron chloride alternate embodiment 1, other groups
Divide same as Example 1 with preparation method.
Reference examples 8
The retardation PES hot melt adhesive cladding ferric sulfate selected in this reference examples, in formula in common ferric sulfate alternate embodiment 1, other groups
Divide same as Example 1 with preparation method.
The performance parameter of fire protection flame retarding polythene material made from the embodiment 1 of table 1 and reference examples 1~8
| Embodiment 1 | Reference examples 1 | Reference examples 2 | Reference examples 3 | Reference examples 4 | Reference examples 5 | Reference examples 6 | Reference examples 7 | Reference examples 8 | |
| Oxygen index (OI) | 40 | 37 | 36 | 33 | 32 | 38 | 35 | 32 | 31 |
| Fire-protection rating | A2 | B1 | B1 | B2 | B2 | B1 | B1 | B2 | B2 |
Described above is the preferred embodiment of the invention, it is noted that for those skilled in the art,
On the premise of the inventive principle is not departed from, some improvements and modifications can also be made, these improvements and modifications are also considered as the hair
Bright protection domain.
Claims (3)
- A kind of 1. preparation method of fire protection flame retarding polythene material, it is characterised in that：Including following raw material components：Polyethylene, PES PUR cladding ferric sulfate, polyacrylate cladding iron chloride, porous di-iron trioxide, the own ester cladding ferrous sulfate of polyacrylic acid The different certain herbaceous plants with big flowers ester of ammonium, pentaerythritol diphosphite two, barium stearate, described polyethylene, retardation PES hot melt adhesive cladding ferric sulfate, poly- third The own ester cladding iron ammonium sulfate of olefin(e) acid ester cladding iron chloride, porous di-iron trioxide, polyacrylic acid, pentaerythritol diphosphite Two different certain herbaceous plants with big flowers esters, the quality parts ratio of barium stearate are 60：38~46：31~39：33~45：23~31：3~6：2~7, wherein, Described retardation PES hot melt adhesive cladding ferric sulfate is reacted by ferric sulfate, retardation PES hot melt adhesive, polyvinyl alcohol and cupric oxide to be made, described sulphur Sour iron, retardation PES hot melt adhesive, the quality parts ratio of polyvinyl alcohol and cupric oxide are 70：18~26：2~7：5~9, described polypropylene Acid esters coats iron chloride and reacts obtained by iron chloride, acrylic acid, Isooctyl acrylate monomer, butyl acrylate and benzoin methyl ether, institute The quality parts ratio of iron chloride, acrylic acid, Isooctyl acrylate monomer, butyl acrylate and the benzoin methyl ether stated is 50：6~12： 26~35：13~27：0.3~1, described porous di-iron trioxide is reacted by iron powder, zinc powder, zinc oxide and zinc oxalate to be made, Described iron powder, zinc powder, the quality parts ratio of zinc oxide and zinc oxalate are 50：35~43：80~97：31~44, described is poly- Hexyl 2-propenoate coats iron ammonium sulfate and reacts system by iron ammonium sulfate, Hexyl 2-propenoate, methyl acrylate and benzoin methyl ether , described iron ammonium sulfate, Hexyl 2-propenoate, the quality parts ratio of methyl acrylate and benzoin methyl ether are 50：35~53： 10~26：0.5~1.
- A kind of 2. preparation method of fire protection flame retarding polythene material according to claim 1, it is characterised in that：Described fire prevention Fire-retardant polyethylene material is as made from following preparation method：(1), by iron ammonium sulfate, Hexyl 2-propenoate, methyl acrylate and Benzoin methyl ether is 50 according to quality parts ratio：35~53：10~26：0.5~1 is added in reactor, mixing speed 65 ~78r/min, 20min is reacted under the conditions of 25~37 DEG C of maintenance system temperature, through 2000W 1~7s of lamp and high pressure mercury, is obtained The own ester cladding iron ammonium sulfate of polyacrylic acid；(2), by iron powder, zinc powder, zinc oxide and zinc oxalate according to quality parts ratio 50：35 ~43：80~97：31~44 are added in ball mill, and drum speed is 30~45r/min, 35~46 DEG C of maintenance system temperature Under the conditions of react 30min, product is through 200 DEG C of roasting 2h, 300 DEG C of roasting 2h, 400 DEG C of roasting 2h, 500 DEG C of roasting 3h, product warp The 1000mL 10mol/L NaOH aqueous solution washs 45min, and filtering, 500mL water washings 3 times, 500mL ethanol wash 3 times, in 53 DEG C, -0.07MPa vacuum drying 14min, obtain porous di-iron trioxide；(3), by iron chloride, acrylic acid, Isooctyl acrylate monomer, Butyl acrylate and benzoin methyl ether are according to quality parts ratio 50：6~12：26~35：13~27：0.3~1 is added to reactor In, mixing speed is 85~100r/min, 25min is reacted under the conditions of 28~36 DEG C of maintenance system temperature, through 3000W high-pressure mercuries Light shines 1~5s, that is, obtains polyacrylate cladding iron chloride；(4), by ferric sulfate, retardation PES hot melt adhesive, polyvinyl alcohol and oxidation Copper is according to quality parts ratio 70：18~26：2~7：5~9 are added in high-speed mixer, mixing velocity 500r/min, maintain 2~6min is reacted under the conditions of 160 DEG C of system temperature, that is, obtains retardation PES hot melt adhesive cladding ferric sulfate；(5), by polyethylene, PES heat Melten gel cladding ferric sulfate, polyacrylate cladding iron chloride, porous di-iron trioxide, the own ester cladding ferrous sulfate of polyacrylic acid The different certain herbaceous plants with big flowers ester of ammonium, pentaerythritol diphosphite two, barium stearate are according to quality parts ratio 60：38~46：31~39：33~45： 23~31：3~6：2~7 are added in high-speed mixer, with high-speed mixer in 170 DEG C of 2~8min of hybrid reaction of temperature, use Extruder obtains fire protection flame retarding polythene material in 173~180 DEG C of extruding pelletizations of temperature.
- A kind of 3. preparation method of fire protection flame retarding polythene material according to claim 2, it is characterised in that：Described PES The fusing point of PUR is 150~155 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108410309A (en) * | 2018-03-16 | 2018-08-17 | 杭州鼎好新材料有限公司 | A kind of polyvinyl chloride-based floor paint and preparation method thereof |
| NO346554B1 (en) * | 2019-08-09 | 2022-10-03 | Klingelberg Products As | Flame retardant, method for its manufacture and article comprising such flame retardant |
-
2017
- 2017-10-12 CN CN201710947984.8A patent/CN107586408A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108410309A (en) * | 2018-03-16 | 2018-08-17 | 杭州鼎好新材料有限公司 | A kind of polyvinyl chloride-based floor paint and preparation method thereof |
| NO346554B1 (en) * | 2019-08-09 | 2022-10-03 | Klingelberg Products As | Flame retardant, method for its manufacture and article comprising such flame retardant |
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