CN107746518A - Special powder calcium zinc stabilizer of environment-friendly type PVC awning film and preparation method thereof - Google Patents
Special powder calcium zinc stabilizer of environment-friendly type PVC awning film and preparation method thereof Download PDFInfo
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- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
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Abstract
The invention discloses the special powder calcium zinc stabilizer of environment-friendly type PVC awning film, by weight, its preparing raw material includes：The calcium benzoate of 100 parts by weight, the zinc benzoate of 10~30 parts by weight, the nano imvite of 2~10 parts by weight, the nanomete talc powder of 5~10 parts by weight, the Tissuemat E of 7~10 parts by weight, the carbon nano-tube modification polyphosphazene polyethersulfone block copolymer of 5~10 parts by weight, four [β (hydroxy phenyl of 3,5 di-t-butyl 4) propionic ester] pentaerythritol esters of 5~9 parts by weight, the silane coupler KH 550 of 1 ~ 5 parts by weight, the silane coupler KH 560 of 1 ~ 5 parts by weight, the ultra-violet absorber UV 9 of the hexamethylene diamine of 1 ~ 5 parts by weight and 5~8 parts by weight.The present invention the special powder calcium zinc stabilizer good weatherability of environment-friendly type PVC awning film, it is not easy to change, can both improve the life-span of PVC awning films, its mechanical strength and heat resistance can be greatly improved again, also with it is environmentally friendly the characteristics of.
Description
Technical field
The invention belongs to chemical stabilizer technical field, more particularly it relates to which a kind of environment-friendly type PVC awning film is special
With powder calcium zinc stabilizer and preparation method thereof.Special powder calcium zinc stabilizer of environment-friendly type PVC awning film and preparation method thereof.
Background technology
As the development of agricultural, greenhouse quantity are more and more.Main material of polyvinyl chloride (PVC) material as awning film
Material, demand constantly increase.In the prior art, during preparing awning film, it usually needs add stabilizer to improve performance.
Generally, nontoxic calcium zinc compound stabilizer typically is used, it is universally acknowledged nontoxic, environment-benign heat stabilizer, and has price
Cheap, the advantages that lubricity is good.But calcium-zinc composite stabilizing agent in the market, on the one hand, weatherability is bad, holds
It is easy to change；On the other hand, addition content significantly reduces the intensity of PVC material compared with Gao Shihui.Both had therefore, it is necessary to develop one kind
There are good weatherability properties, the environment-friendly calcium-zinc compound stabilizer of the intensity of PVC material will not be reduced again.
The content of the invention
Therefore, one aspect of the present invention provides the special powder calcium zinc stabilizer of environment-friendly type PVC awning film, by weight
Meter, its preparing raw material include：
The calcium benzoate of 100 parts by weight, the zinc benzoate of 10~30 parts by weight, the nano imvite of 2~10 parts by weight, 5~10
The nanomete talc powder of parts by weight, the Tissuemat E of 7~10 parts by weight, carbon nano-tube modification polyphosphazene-polyethers of 5~10 parts by weight
Sulfone block copolymer, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol esters of 5~9 parts by weight, 1 ~ 5
The silane resin acceptor kh-550 of parts by weight, the silane coupler KH-560 of 1 ~ 5 parts by weight, the hexamethylene diamine of 1 ~ 5 parts by weight and 5~
The ultra-violet absorber UV-9 of 8 parts by weight；
Preferably, the special powder calcium zinc stabilizer of described environment-friendly type PVC awning film, by weight, its preparing raw material includes：
The calcium benzoate of 100 parts by weight, the zinc benzoate of 15~25 parts by weight, the nano imvite of 5~8 parts by weight, 6~8 weights
It is embedding to measure the nanomete talc powder of part, the Tissuemat E of 8~9 parts by weight, carbon nano-tube modification polyphosphazene-polyether sulfone of 6~8 parts by weight
Section copolymer, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol esters of 6~8 parts by weight, 2 ~ 4 weight
The silane resin acceptor kh-550, the silane coupler KH-560 of 2 ~ 4 parts by weight, the hexamethylene diamine of 2 ~ 4 parts by weight and 6~7 weights of part
Measure the ultra-violet absorber UV-9 of part；
It is highly preferred that the special powder calcium zinc stabilizer of described environment-friendly type PVC awning film, by weight, its preparing raw material bag
Include：
The calcium benzoate of 100 parts by weight, the zinc benzoate of 20 parts by weight, the nano imvite of 7 parts by weight, the nanometer of 8 parts by weight
Talcum powder, the Tissuemat E of 9 parts by weight, carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer of 7 parts by weight, 7 parts by weight
Four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol esters, the silane resin acceptor kh-550 of 3 parts by weight, 3
The silane coupler KH-560 of parts by weight, the hexamethylene diamine of 3 parts by weight and 6 parts by weight ultra-violet absorber UV-9.
In one embodiment, the preparation method of the carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer is：
（1）In 300 milliliters of round-bottomed flasks, by 0.41 gram of hexachlorocyclotriph,sphazene and 0.94 gram 4,4 '-dihydroxydiphenylsulisomer is molten
Then solution adds 1.5 milliliters of triethylamines, is placed in 50 DEG C of ultrasonic water baths and reacts 10 hours in 190 milliliters of acetonitriles, reaction knot
Shu Hou, solvent is centrifuged off, distinguishes washed product 5 times with deionized water and acetone, finally vacuum drying 25 is small at 50 DEG C
When obtain white polyphosphazene powder；
（2）Under nitrogen protection, 1.23 are added to being connected with the there-necked flask of mechanical agitation, air inlet pipe, water-taker and condenser pipe
Gram above-mentioned steps（1）Gained white polyphosphazene powder, 4.250 grams of diallyl bisphenol Ss, 3.811 grams of 4,4 '-difluorodiphenyl sulfones,
30 milliliters of sulfolane, 2.6 grams of potassium carbonate, 20 milliliters of toluene, 140 DEG C of backflows, band water raise temperature, steam toluene after 4 hours,
System temperature rises to 165 DEG C, reacts 20 hours, discharges in water, obtain bar shaped polymer, by obtained bar shaped polymer with smashing
Broken machine is smashed to pieces, then obtains polyphosphazene-polyethers within 24 hours with 50 DEG C of drying in vacuum drying oven after distilled water boiling washing 3 times, are placed on
Sulfone block copolymer；
（3）In 250 milliliters of round-bottomed flasks, above-mentioned steps are sequentially added（2）Gained polyphosphazene-polyethersulfone block copolymer 10
Gram, 1 gram of graphene oxide, 2.5 grams of CNT, 150 milliliters of dimethyl sulfoxide (DMSO), 1 milliliter of acetic acid, silane resin acceptor kh-550 2
Gram and 5 grams of silane coupler KH-560, system temperature rise to 50 DEG C, react 6 hours, discharge in water, obtain cotton-shaped production
Thing, the fluffy solid is washed respectively 3 times, be finally dried in vacuo at 50 DEG C described in obtaining within 24 hours with deionized water and ethanol
Carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer.
In one embodiment, the average grain diameter of the nanomete talc powder is 500-1000 nanometers；Preferably 600 receive
Rice.
In one embodiment, the average grain diameter of the nano imvite is 500-800 nanometers；Preferably 700 nanometers.
In a kind of preferred scheme, the special powder calcium zinc stabilizer of described environment-friendly type PVC awning film, by weight,
Its preparing raw material also includes：The sulfonated phosphazene modified nano-titanium dioxide of 5-9 parts by weight；Preferably 8 parts by weight.
In a kind of preferred scheme, the preparation method of the sulfonated phosphazene modified nano-titanium dioxide is：
In 250 milliliters of round-bottomed flasks, by 0.41 gram of hexachlorocyclotriph,sphazene and 0.92 gram 4,4 '-dihydroxydiphenylsulisomer is dissolved in
In 200 milliliters of acetonitriles, 1.3 milliliters of triethylamines are then added, is placed in 50 DEG C of ultrasonic water baths and reacts 4 hours, after reaction terminates, from
The heart removes solvent, distinguishes washed product 5 times with deionized water and acetone, is finally dried in vacuo 18 hours at 50 DEG C and obtains white
Polyphosphazene powder；
0.6 gram of above-mentioned white polyphosphazene powder is added in 100 milliliters of three-neck flasks, adds 10 milliliters of mass fractions 98%
The concentrated sulfuric acid, it is placed in 50 DEG C of water-baths, reacts 15 hours under mechanical stirring, after reaction terminates, product is slowly poured into cold water
In, and be stirred continuously, unreacted sulfuric acid is centrifuged off, product is then washed with deionized 5 times, finally the vacuum at 50 DEG C
Dry 48 hours and obtain sulfonated phosphazene powder；
0.7 gram of above-mentioned sulfonated phosphazene powder, 0.07 gram of epoxy resin E51, average grain diameter are added in 50 milliliters of three-neck flasks
For 0.5 gram of 150 nanometers of 3 grams of nano titanium oxide, 0.2 gram of silane resin acceptor kh-550 and silane coupler KH-560 with
And 10 milliliters of dimethyl sulfoxide (DMSO)s, heat up 120 DEG C after reacting 2 hours, be down to room temperature and slowly pour into product in cold water, and constantly
Stirring, is then washed with deionized product 5 times, and it is to obtain sulfonated phosphazene to change that 48 hours are finally dried in vacuo at 50 DEG C
Property nano titanium oxide.
The present invention also provides the preparation method of the special powder calcium zinc stabilizer of environment-friendly type PVC awning film, including：
Described recipe ingredient is added in homogenizer, 15min-60min, stir speed (S.S.) are stirred under the conditions of 50-100 DEG C
For 1000-2000r/min, obtained after cooling.
In a preferred approach, the preparation method of the special powder calcium zinc stabilizer of described environment-friendly type PVC awning film, at 80 DEG C
Under the conditions of stir 20min, stir speed (S.S.) 1700r/min.
Compared with prior art, beneficial effects of the present invention are：
1st, by the addition of carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer, the intensity, resistance to of material can be greatly improved
Time property and heat resistance.
2nd, by the addition of sulfonated phosphazene modified nano-titanium dioxide, the intensity, heat-resisting of material can further be improved
Property and toughness.
Embodiment
Raw material:
Nano imvite（700 nanometers of average grain diameter）, nanomete talc powder（600 nanometers of average grain diameter）, nano titanium oxide（It is average
200 nanometers of particle diameter）, silane resin acceptor kh-550, silane coupler KH-560 be purchased from Aladdin reagent.CNT is more wall carbon
Nanotube, average 10 microns of pipe range, average 50 nanometers of caliber, heap density 0.09g/cm3Scheme purchased from Shenzhen spirit.Graphene oxide is purchased
From permanent ball science and technology.Other raw materials are purchased from Chinese medicines group.
Embodiment 1
Successively by the calcium benzoate of 100 parts by weight, the zinc benzoate of 10 parts by weight, the nano imvite of 2 parts by weight, 5 parts by weight
Nanomete talc powder, the Tissuemat Es of 7 parts by weight, carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer of 5 parts by weight, 5
Four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol esters, the silane coupler of 1 parts by weight of parts by weight
KH-550, the silane coupler KH-560 of 1 parts by weight, the ultra-violet absorber UV-9 of the hexamethylene diamine of 1 parts by weight and 5 parts by weight
Add in homogenizer, 20min is stirred under the conditions of 80 DEG C, stir speed (S.S.) 1700r/min, Ca Zn composite is obtained after cooling
Stabilizer；
The preparation method of the carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer is：
（1）In 300 milliliters of round-bottomed flasks, by 0.41 gram of hexachlorocyclotriph,sphazene and 0.94 gram 4,4 '-dihydroxydiphenylsulisomer is molten
Then solution adds 1.5 milliliters of triethylamines, is placed in 50 DEG C of ultrasonic water baths and reacts 10 hours in 190 milliliters of acetonitriles, reaction knot
Shu Hou, solvent is centrifuged off, distinguishes washed product 5 times with deionized water and acetone, finally vacuum drying 25 is small at 50 DEG C
When obtain white polyphosphazene powder；
（2）Under nitrogen protection, 1.23 are added to being connected with the there-necked flask of mechanical agitation, air inlet pipe, water-taker and condenser pipe
Gram above-mentioned steps（1）Gained white polyphosphazene powder, 4.250 grams of diallyl bisphenol Ss, 3.811 grams of 4,4 '-difluorodiphenyl sulfones,
30 milliliters of sulfolane, 2.6 grams of potassium carbonate, 20 milliliters of toluene, 140 DEG C of backflows, band water raise temperature, steam toluene after 4 hours,
System temperature rises to 165 DEG C, reacts 20 hours, discharges in water, obtain bar shaped polymer, by obtained bar shaped polymer with smashing
Broken machine is smashed to pieces, then obtains polyphosphazene-polyethers within 24 hours with 50 DEG C of drying in vacuum drying oven after distilled water boiling washing 3 times, are placed on
Sulfone block copolymer；
（3）In 250 milliliters of round-bottomed flasks, above-mentioned steps are sequentially added（2）Gained polyphosphazene-polyethersulfone block copolymer 10
Gram, 1 gram of graphene oxide, 2.5 grams of CNT, 150 milliliters of dimethyl sulfoxide (DMSO), 1 milliliter of acetic acid, silane resin acceptor kh-550 2
Gram and 5 grams of silane coupler KH-560, system temperature rise to 50 DEG C, react 6 hours, discharge in water, obtain cotton-shaped production
Thing, the fluffy solid is washed respectively 3 times, be finally dried in vacuo at 50 DEG C described in obtaining within 24 hours with deionized water and ethanol
Carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer.
Embodiment 2
Successively by the calcium benzoate of 100 parts by weight, the zinc benzoate of 30 parts by weight, the nano imvite of 10 parts by weight, 10 weight
Carbon nano-tube modification polyphosphazene-polyethersulfone block copolymerization of the nanomete talc powder of part, the Tissuemat E of 10 parts by weight, 10 parts by weight
Thing, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol esters of 9 parts by weight, 5 parts by weight it is silane coupled
Agent KH-550, the silane coupler KH-560 of 5 parts by weight, the ultra-violet absorber of the hexamethylene diamine of 5 parts by weight and 8 parts by weight
UV-9 is added in homogenizer, and 20min is stirred under the conditions of 80 DEG C, stir speed (S.S.) 1700r/min, calcium zinc is obtained after cooling
Compound stabilizer；
The preparation method of the carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer is：
（1）In 300 milliliters of round-bottomed flasks, by 0.41 gram of hexachlorocyclotriph,sphazene and 0.94 gram 4,4 '-dihydroxydiphenylsulisomer is molten
Then solution adds 1.5 milliliters of triethylamines, is placed in 50 DEG C of ultrasonic water baths and reacts 10 hours in 190 milliliters of acetonitriles, reaction knot
Shu Hou, solvent is centrifuged off, distinguishes washed product 5 times with deionized water and acetone, finally vacuum drying 25 is small at 50 DEG C
When obtain white polyphosphazene powder；
（2）Under nitrogen protection, 1.23 are added to being connected with the there-necked flask of mechanical agitation, air inlet pipe, water-taker and condenser pipe
Gram above-mentioned steps（1）Gained white polyphosphazene powder, 4.250 grams of diallyl bisphenol Ss, 3.811 grams of 4,4 '-difluorodiphenyl sulfones,
30 milliliters of sulfolane, 2.6 grams of potassium carbonate, 20 milliliters of toluene, 140 DEG C of backflows, band water raise temperature, steam toluene after 4 hours,
System temperature rises to 165 DEG C, reacts 20 hours, discharges in water, obtain bar shaped polymer, by obtained bar shaped polymer with smashing
Broken machine is smashed to pieces, then obtains polyphosphazene-polyethers within 24 hours with 50 DEG C of drying in vacuum drying oven after distilled water boiling washing 3 times, are placed on
Sulfone block copolymer；
（3）In 250 milliliters of round-bottomed flasks, above-mentioned steps are sequentially added（2）Gained polyphosphazene-polyethersulfone block copolymer 10
Gram, 1 gram of graphene oxide, 2.5 grams of CNT, 150 milliliters of dimethyl sulfoxide (DMSO), 1 milliliter of acetic acid, silane resin acceptor kh-550 2
Gram and 5 grams of silane coupler KH-560, system temperature rise to 50 DEG C, react 6 hours, discharge in water, obtain cotton-shaped production
Thing, the fluffy solid is washed respectively 3 times, be finally dried in vacuo at 50 DEG C described in obtaining within 24 hours with deionized water and ethanol
Carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer.
Embodiment 3
Successively by the calcium benzoate of 100 parts by weight, the zinc benzoate of 20 parts by weight, the nano imvite of 7 parts by weight, 8 parts by weight
Nanomete talc powder, the Tissuemat Es of 9 parts by weight, carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer of 7 parts by weight, 7
Four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol esters, the silane coupler of 3 parts by weight of parts by weight
KH-550, the silane coupler KH-560 of 3 parts by weight, the ultra-violet absorber UV-9 of the hexamethylene diamine of 3 parts by weight and 6 parts by weight
Add in homogenizer, 20min is stirred under the conditions of 80 DEG C, stir speed (S.S.) 1700r/min, Ca Zn composite is obtained after cooling
Stabilizer；
The preparation method of the carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer is：
（1）In 300 milliliters of round-bottomed flasks, by 0.41 gram of hexachlorocyclotriph,sphazene and 0.94 gram 4,4 '-dihydroxydiphenylsulisomer is molten
Then solution adds 1.5 milliliters of triethylamines, is placed in 50 DEG C of ultrasonic water baths and reacts 10 hours in 190 milliliters of acetonitriles, reaction knot
Shu Hou, solvent is centrifuged off, distinguishes washed product 5 times with deionized water and acetone, finally vacuum drying 25 is small at 50 DEG C
When obtain white polyphosphazene powder；
（2）Under nitrogen protection, 1.23 are added to being connected with the there-necked flask of mechanical agitation, air inlet pipe, water-taker and condenser pipe
Gram above-mentioned steps（1）Gained white polyphosphazene powder, 4.250 grams of diallyl bisphenol Ss, 3.811 grams of 4,4 '-difluorodiphenyl sulfones,
30 milliliters of sulfolane, 2.6 grams of potassium carbonate, 20 milliliters of toluene, 140 DEG C of backflows, band water raise temperature, steam toluene after 4 hours,
System temperature rises to 165 DEG C, reacts 20 hours, discharges in water, obtain bar shaped polymer, by obtained bar shaped polymer with smashing
Broken machine is smashed to pieces, then obtains polyphosphazene-polyethers within 24 hours with 50 DEG C of drying in vacuum drying oven after distilled water boiling washing 3 times, are placed on
Sulfone block copolymer；
（3）In 250 milliliters of round-bottomed flasks, above-mentioned steps are sequentially added（2）Gained polyphosphazene-polyethersulfone block copolymer 10
Gram, 1 gram of graphene oxide, 2.5 grams of CNT, 150 milliliters of dimethyl sulfoxide (DMSO), 1 milliliter of acetic acid, silane resin acceptor kh-550 2
Gram and 5 grams of silane coupler KH-560, system temperature rise to 50 DEG C, react 6 hours, discharge in water, obtain cotton-shaped production
Thing, the fluffy solid is washed respectively 3 times, be finally dried in vacuo at 50 DEG C described in obtaining within 24 hours with deionized water and ethanol
Carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer.
Embodiment 4
Successively by the calcium benzoate of 100 parts by weight, the zinc benzoate of 20 parts by weight, the nano imvite of 7 parts by weight, 8 parts by weight
Nanomete talc powder, the Tissuemat Es of 9 parts by weight, carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer of 7 parts by weight, 7
Four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol esters, the silane coupler of 3 parts by weight of parts by weight
KH-550, the silane coupler KH-560 of 3 parts by weight, the ultra-violet absorber UV-9 of the hexamethylene diamine of 3 parts by weight and 6 parts by weight
And 5 parts by weight sulfonated phosphazene modified nano-titanium dioxide add homogenizer in, stirred under the conditions of 80 DEG C
20min, stir speed (S.S.) 1700r/min, calcium-zinc composite stabilizing agent is obtained after cooling；
The preparation method of the carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer is：
（1）In 300 milliliters of round-bottomed flasks, by 0.41 gram of hexachlorocyclotriph,sphazene and 0.94 gram 4,4 '-dihydroxydiphenylsulisomer is molten
Then solution adds 1.5 milliliters of triethylamines, is placed in 50 DEG C of ultrasonic water baths and reacts 10 hours in 190 milliliters of acetonitriles, reaction knot
Shu Hou, solvent is centrifuged off, distinguishes washed product 5 times with deionized water and acetone, finally vacuum drying 25 is small at 50 DEG C
When obtain white polyphosphazene powder；
（2）Under nitrogen protection, 1.23 are added to being connected with the there-necked flask of mechanical agitation, air inlet pipe, water-taker and condenser pipe
Gram above-mentioned steps（1）Gained white polyphosphazene powder, 4.250 grams of diallyl bisphenol Ss, 3.811 grams of 4,4 '-difluorodiphenyl sulfones,
30 milliliters of sulfolane, 2.6 grams of potassium carbonate, 20 milliliters of toluene, 140 DEG C of backflows, band water raise temperature, steam toluene after 4 hours,
System temperature rises to 165 DEG C, reacts 20 hours, discharges in water, obtain bar shaped polymer, by obtained bar shaped polymer with smashing
Broken machine is smashed to pieces, then obtains polyphosphazene-polyethers within 24 hours with 50 DEG C of drying in vacuum drying oven after distilled water boiling washing 3 times, are placed on
Sulfone block copolymer；
（3）In 250 milliliters of round-bottomed flasks, above-mentioned steps are sequentially added（2）Gained polyphosphazene-polyethersulfone block copolymer 10
Gram, 1 gram of graphene oxide, 2.5 grams of CNT, 150 milliliters of dimethyl sulfoxide (DMSO), 1 milliliter of acetic acid, silane resin acceptor kh-550 2
Gram and 5 grams of silane coupler KH-560, system temperature rise to 50 DEG C, react 6 hours, discharge in water, obtain cotton-shaped production
Thing, the fluffy solid is washed respectively 3 times, be finally dried in vacuo at 50 DEG C described in obtaining within 24 hours with deionized water and ethanol
Carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer；
The preparation method of the sulfonated phosphazene modified nano-titanium dioxide is：
In 250 milliliters of round-bottomed flasks, by 0.41 gram of hexachlorocyclotriph,sphazene and 0.92 gram 4,4 '-dihydroxydiphenylsulisomer is dissolved in
In 200 milliliters of acetonitriles, 1.3 milliliters of triethylamines are then added, is placed in 50 DEG C of ultrasonic water baths and reacts 4 hours, after reaction terminates, from
The heart removes solvent, distinguishes washed product 5 times with deionized water and acetone, is finally dried in vacuo 18 hours at 50 DEG C and obtains white
Polyphosphazene powder；
0.6 gram of above-mentioned white polyphosphazene powder is added in 100 milliliters of three-neck flasks, adds 10 milliliters of mass fractions 98%
The concentrated sulfuric acid, it is placed in 50 DEG C of water-baths, reacts 15 hours under mechanical stirring, after reaction terminates, product is slowly poured into cold water
In, and be stirred continuously, unreacted sulfuric acid is centrifuged off, product is then washed with deionized 5 times, finally the vacuum at 50 DEG C
Dry 48 hours and obtain sulfonated phosphazene powder；
0.7 gram of above-mentioned sulfonated phosphazene powder, 0.07 gram of epoxy resin E51, average grain diameter are added in 50 milliliters of three-neck flasks
For 0.5 gram of 150 nanometers of 3 grams of nano titanium oxide, 0.2 gram of silane resin acceptor kh-550 and silane coupler KH-560 with
And 10 milliliters of dimethyl sulfoxide (DMSO)s, heat up 120 DEG C after reacting 2 hours, be down to room temperature and slowly pour into product in cold water, and constantly
Stirring, is then washed with deionized product 5 times, and it is to obtain sulfonated phosphazene to change that 48 hours are finally dried in vacuo at 50 DEG C
Property nano titanium oxide.
Comparative example 1
Successively by the calcium benzoate of 100 parts by weight, the zinc benzoate of 20 parts by weight, the nano imvite of 7 parts by weight, 8 parts by weight
Nanomete talc powder, Tissuemat E, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester] of 7 parts by weight of 9 parts by weight
Pentaerythritol ester, the silane resin acceptor kh-550 of 3 parts by weight, the silane coupler KH-560 of 3 parts by weight, 3 parts by weight oneself two
Amine and the ultra-violet absorber UV-9 of 6 parts by weight are added in homogenizer, and 20min, stirring speed are stirred under the conditions of 80 DEG C
Rate is 1700r/min, and calcium-zinc composite stabilizing agent is obtained after cooling.
Comparative example 2
Successively by the calcium benzoate of 100 parts by weight, the zinc benzoate of 20 parts by weight, the nano imvite of 7 parts by weight, 8 parts by weight
Nanomete talc powder, the Tissuemat Es of 9 parts by weight, polyphosphazene-polyethersulfone block copolymer of 7 parts by weight, the four of 7 parts by weight
[β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol ester, the silane resin acceptor kh-550 of 3 parts by weight, 3 weight
The silane coupler KH-560 of part, the hexamethylene diamine of 3 parts by weight and 6 parts by weight ultra-violet absorber UV-9 add high-speed stirred
In machine, 20min, stir speed (S.S.) 1700r/min are stirred under the conditions of 80 DEG C, calcium-zinc composite stabilizing agent is obtained after cooling and adds height
In fast mixer, 8min is stirred under the conditions of 70 DEG C, stir speed (S.S.) 1300r/min, calcium-zinc composite stabilizing agent is obtained after cooling；
The preparation method of the polyphosphazene-polyethersulfone block copolymer is：
（1）In 300 milliliters of round-bottomed flasks, by 0.41 gram of hexachlorocyclotriph,sphazene and 0.94 gram 4,4 '-dihydroxydiphenylsulisomer is molten
Then solution adds 1.5 milliliters of triethylamines, is placed in 50 DEG C of ultrasonic water baths and reacts 10 hours in 190 milliliters of acetonitriles, reaction knot
Shu Hou, solvent is centrifuged off, distinguishes washed product 5 times with deionized water and acetone, finally vacuum drying 25 is small at 50 DEG C
When obtain white polyphosphazene powder；
（2）Under nitrogen protection, 1.23 are added to being connected with the there-necked flask of mechanical agitation, air inlet pipe, water-taker and condenser pipe
Gram above-mentioned steps（1）Gained white polyphosphazene powder, 4.250 grams of diallyl bisphenol Ss, 3.811 grams of 4,4 '-difluorodiphenyl sulfones,
30 milliliters of sulfolane, 2.6 grams of potassium carbonate, 20 milliliters of toluene, 140 DEG C of backflows, band water raise temperature, steam toluene after 4 hours,
System temperature rises to 165 DEG C, reacts 20 hours, discharges in water, obtain bar shaped polymer, by obtained bar shaped polymer with smashing
Broken machine is smashed to pieces, then obtains polyphosphazene-polyethers within 24 hours with 50 DEG C of drying in vacuum drying oven after distilled water boiling washing 3 times, are placed on
Sulfone block copolymer.
Comparative example 3
Successively by the calcium benzoate of 100 parts by weight, the zinc benzoate of 20 parts by weight, the nano imvite of 7 parts by weight, 8 parts by weight
Nanomete talc powder, the Tissuemat E of 9 parts by weight, the polyphosphazene of 7 parts by weight, four [β-(3,5- di-t-butyl -4- of 7 parts by weight
Hydroxy phenyl) propionic ester] pentaerythritol ester, the silane resin acceptor kh-550 of 3 parts by weight, the silane coupler KH- of 3 parts by weight
560th, the hexamethylene diamine of 3 parts by weight and the ultra-violet absorber UV-9 of 6 parts by weight are added in homogenizer, under the conditions of 80 DEG C
20min, stir speed (S.S.) 1700r/min are stirred, calcium-zinc composite stabilizing agent is obtained after cooling and is added in homogenizer, at 70 DEG C
Under the conditions of stir 8min, stir speed (S.S.) 1300r/min, calcium-zinc composite stabilizing agent is obtained after cooling；
The preparation method of the polyphosphazene is：
In 300 milliliters of round-bottomed flasks, by 0.41 gram of hexachlorocyclotriph,sphazene and 0.94 gram 4,4 '-dihydroxydiphenylsulisomer is dissolved in
In 190 milliliters of acetonitriles, 1.5 milliliters of triethylamines are then added, is placed in 50 DEG C of ultrasonic water baths and reacts 10 hours, after reaction terminates,
Solvent is centrifuged off, washed product is distinguished 5 times with deionized water and acetone, is finally dried in vacuo 25 hours and obtains at 50 DEG C
White polyphosphazene powder.
Comparative example 4
Successively by the calcium benzoate of 100 parts by weight, the zinc benzoate of 20 parts by weight, the nano imvite of 7 parts by weight, 8 parts by weight
Nanomete talc powder, the Tissuemat Es of 9 parts by weight, carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer of 7 parts by weight, 7
Four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol esters, the silane coupler of 3 parts by weight of parts by weight
KH-550, the silane coupler KH-560 of 3 parts by weight, the hexamethylene diamine of 3 parts by weight, 6 parts by weight ultra-violet absorber UV-9 with
And 8 parts by weight polyphosphazene modified nano-titanium dioxide add homogenizer in, 20min is stirred under the conditions of 80 DEG C, stir
Speed is 1700r/min, and calcium-zinc composite stabilizing agent is obtained after cooling；
The preparation method of the carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer is：
（1）In 300 milliliters of round-bottomed flasks, by 0.41 gram of hexachlorocyclotriph,sphazene and 0.94 gram 4,4 '-dihydroxydiphenylsulisomer is molten
Then solution adds 1.5 milliliters of triethylamines, is placed in 50 DEG C of ultrasonic water baths and reacts 10 hours in 190 milliliters of acetonitriles, reaction knot
Shu Hou, solvent is centrifuged off, distinguishes washed product 5 times with deionized water and acetone, finally vacuum drying 25 is small at 50 DEG C
When obtain white polyphosphazene powder；
（2）Under nitrogen protection, 1.23 are added to being connected with the there-necked flask of mechanical agitation, air inlet pipe, water-taker and condenser pipe
Gram above-mentioned steps（1）Gained white polyphosphazene powder, 4.250 grams of diallyl bisphenol Ss, 3.811 grams of 4,4 '-difluorodiphenyl sulfones,
30 milliliters of sulfolane, 2.6 grams of potassium carbonate, 20 milliliters of toluene, 140 DEG C of backflows, band water raise temperature, steam toluene after 4 hours,
System temperature rises to 165 DEG C, reacts 20 hours, discharges in water, obtain bar shaped polymer, by obtained bar shaped polymer with smashing
Broken machine is smashed to pieces, then obtains polyphosphazene-polyethers within 24 hours with 50 DEG C of drying in vacuum drying oven after distilled water boiling washing 3 times, are placed on
Sulfone block copolymer；
（3）In 250 milliliters of round-bottomed flasks, above-mentioned steps are sequentially added（2）Gained polyphosphazene-polyethersulfone block copolymer 10
Gram, 1 gram of graphene oxide, 2.5 grams of CNT, 150 milliliters of dimethyl sulfoxide (DMSO), 1 milliliter of acetic acid, silane resin acceptor kh-550 2
Gram and 5 grams of silane coupler KH-560, system temperature rise to 50 DEG C, react 6 hours, discharge in water, obtain cotton-shaped production
Thing, the fluffy solid is washed respectively 3 times, be finally dried in vacuo at 50 DEG C described in obtaining within 24 hours with deionized water and ethanol
Carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer；
The preparation method of the polyphosphazene modified nano-titanium dioxide is：
In 250 milliliters of round-bottomed flasks, by 0.41 gram of hexachlorocyclotriph,sphazene and 0.92 gram 4,4 '-dihydroxydiphenylsulisomer is dissolved in
In 200 milliliters of acetonitriles, 1.3 milliliters of triethylamines are then added, is placed in 50 DEG C of ultrasonic water baths and reacts 4 hours, after reaction terminates, from
The heart removes solvent, distinguishes washed product 5 times with deionized water and acetone, is finally dried in vacuo 18 hours at 50 DEG C and obtains white
Polyphosphazene powder；
0.7 gram of above-mentioned polyphosphazene powder, 0.07 gram of epoxy resin E51, average grain diameter are added in 50 milliliters of three-neck flasks is
150 nanometers of 0.5 gram of 3 grams of nano titanium oxide, 0.2 gram of silane resin acceptor kh-550 and silane coupler KH-560 and
10 milliliters of dimethyl sulfoxide (DMSO)s, heat up 120 DEG C after reacting 2 hours, be down to room temperature and slowly pour into product in cold water, and constantly stir
Mix, product is then washed with deionized 5 times, be finally dried in vacuo at 50 DEG C 48 hours and obtain polyphosphazene modified Nano
Titanium dioxide.
Test condition
1st, weatherability is tested：Embodiment 1-4 and comparative example 1-4 calcium-zinc composite stabilizing agent are irradiated into 50h under ultraviolet light, it is ultraviolet
The model UVA-340 types of light lamp, ultraviolet tube number are 2, and each ultraviolet tube is 40w, and it is steady to test above-mentioned Ca Zn composite
Determine the aberration of agent.
2nd, prepare PVC board using embodiment 1-4 and comparative example 1-4 calcium-zinc composite stabilizing agent and test the sheet material
Intensity, specific method are：
A, by weight, by safe 100 parts of SG-7 types polyvinyl chloride resin, 40 parts of di-n-octyl phthalate, embodiment 1- in Xinjiang
4 parts of 10 parts of any one calcium-zinc composite stabilizing agent and PVC processing aids (ACR401) are put into mixed at a high speed in 4 and comparative example 1-4
Mixed in conjunction machine to temperature of charge reach 100 DEG C when, continue to mix to temperature of charge reach 120 DEG C when, material is first discharged into crowded
Go out in machine, the extruder for extruding PVC uses draw ratio as 1 to 30, the extruder that 6th area that compression ratio is 5.5 are heated, and screw rod is straight
Footpath is 120, using pressure charging type hopper.Temperature control is 130 DEG C of an area；2nd area are 145 DEG C, and 3rd area are 155 DEG C；4th area
165℃；Then five 175 DEG C of areas, six 185 DEG C of areas, 170 DEG C of flange, 185 DEG C of head are extruded and drawn from co-extruding machine head and be molded
To awning film.
Test result see the table below
| Example | Stable aberration | Tensile strength | Elongation at break | Heat distortion temperature |
| Embodiment 1 | 0.02 | 25Mpa | 158.0% | 110℃ |
| Embodiment 2 | 0.02 | 27Mpa | 166% | 102℃ |
| Embodiment 3 | 0.01 | 36 Mpa | 148% | 120℃ |
| Embodiment 4 | 0 | 46Mpa | 138% | 127℃ |
| Comparative example 1 | 0.71 | 13 Mpa | 175% | 78℃ |
| Comparative example 2 | 0.15 | 16 Mpa | 153% | 88℃ |
| Comparative example 3 | 0.22 | 18Mpa | 161% | 83℃ |
| Comparative example 4 | 0.01 | 29 Mpa | 105% | 123℃ |
Claims (10)
1. the special powder calcium zinc stabilizer of environment-friendly type PVC awning film, it is characterised in that by weight, its preparing raw material includes：
The calcium benzoate of 100 parts by weight, the zinc benzoate of 10~30 parts by weight, the nano imvite of 2~10 parts by weight, 5~10
The nanomete talc powder of parts by weight, the Tissuemat E of 7~10 parts by weight, carbon nano-tube modification polyphosphazene-polyethers of 5~10 parts by weight
Sulfone block copolymer, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol esters of 5~9 parts by weight, 1 ~ 5
The silane resin acceptor kh-550 of parts by weight, the silane coupler KH-560 of 1 ~ 5 parts by weight, the hexamethylene diamine of 1 ~ 5 parts by weight and 5~
The ultra-violet absorber UV-9 of 8 parts by weight.
2. the special powder calcium zinc stabilizer of environment-friendly type PVC awning film according to claim 1, it is characterised in that by weight
Part meter, its preparing raw material include：
The calcium benzoate of 100 parts by weight, the zinc benzoate of 15~25 parts by weight, the nano imvite of 5~8 parts by weight, 6~8 weights
It is embedding to measure the nanomete talc powder of part, the Tissuemat E of 8~9 parts by weight, carbon nano-tube modification polyphosphazene-polyether sulfone of 6~8 parts by weight
Section copolymer, four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol esters of 6~8 parts by weight, 2 ~ 4 weight
The silane resin acceptor kh-550, the silane coupler KH-560 of 2 ~ 4 parts by weight, the hexamethylene diamine of 2 ~ 4 parts by weight and 6~7 weights of part
Measure the ultra-violet absorber UV-9 of part.
3. the special powder calcium zinc stabilizer of environment-friendly type PVC awning film according to claim 2, it is characterised in that by weight
Part meter, its preparing raw material include：
The calcium benzoate of 100 parts by weight, the zinc benzoate of 20 parts by weight, the nano imvite of 7 parts by weight, the nanometer of 8 parts by weight
Talcum powder, the Tissuemat E of 9 parts by weight, carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer of 7 parts by weight, 7 parts by weight
Four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic ester] pentaerythritol esters, the silane resin acceptor kh-550 of 3 parts by weight, 3
The silane coupler KH-560 of parts by weight, the hexamethylene diamine of 3 parts by weight and 6 parts by weight ultra-violet absorber UV-9.
4. the special powder calcium zinc stabilizer of environment-friendly type PVC awning film according to claim any one of 1-3, its feature exist
In the preparation method of the carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer is：
（1）In 300 milliliters of round-bottomed flasks, by 0.41 gram of hexachlorocyclotriph,sphazene and 0.94 gram 4,4 '-dihydroxydiphenylsulisomer is molten
Then solution adds 1.5 milliliters of triethylamines, is placed in 50 DEG C of ultrasonic water baths and reacts 10 hours in 190 milliliters of acetonitriles, reaction knot
Shu Hou, solvent is centrifuged off, distinguishes washed product 5 times with deionized water and acetone, finally vacuum drying 25 is small at 50 DEG C
When obtain white polyphosphazene powder；
（2）Under nitrogen protection, 1.23 are added to being connected with the there-necked flask of mechanical agitation, air inlet pipe, water-taker and condenser pipe
Gram above-mentioned steps（1）Gained white polyphosphazene powder, 4.250 grams of diallyl bisphenol Ss, 3.811 grams of 4,4 '-difluorodiphenyl sulfones,
30 milliliters of sulfolane, 2.6 grams of potassium carbonate, 20 milliliters of toluene, 140 DEG C of backflows, band water raise temperature, steam toluene after 4 hours,
System temperature rises to 165 DEG C, reacts 20 hours, discharges in water, obtain bar shaped polymer, by obtained bar shaped polymer with smashing
Broken machine is smashed to pieces, then obtains polyphosphazene-polyethers within 24 hours with 50 DEG C of drying in vacuum drying oven after distilled water boiling washing 3 times, are placed on
Sulfone block copolymer；
（3）In 250 milliliters of round-bottomed flasks, above-mentioned steps are sequentially added（2）Gained polyphosphazene-polyethersulfone block copolymer 10
Gram, 1 gram of graphene oxide, 2.5 grams of CNT, 150 milliliters of dimethyl sulfoxide (DMSO), 1 milliliter of acetic acid, silane resin acceptor kh-550 2
Gram and 5 grams of silane coupler KH-560, system temperature rise to 50 DEG C, react 6 hours, discharge in water, obtain cotton-shaped production
Thing, the fluffy solid is washed respectively 3 times, be finally dried in vacuo at 50 DEG C described in obtaining within 24 hours with deionized water and ethanol
Carbon nano-tube modification polyphosphazene-polyethersulfone block copolymer.
5. the special powder calcium zinc stabilizer of environment-friendly type PVC awning film according to claim any one of 1-3, its feature exist
In the average grain diameter of the nanomete talc powder is 500-1000 nanometers.
6. the special powder calcium zinc stabilizer of environment-friendly type PVC awning film according to claim any one of 1-3, its feature exist
In the average grain diameter of the nano imvite is 500-800 nanometers.
7. the special powder calcium zinc stabilizer of environment-friendly type PVC awning film according to claim any one of 1-3, its feature exist
In by weight, its preparing raw material also includes：The sulfonated phosphazene modified nano-titanium dioxide of 5-9 parts by weight.
8. the special powder calcium zinc stabilizer of environment-friendly type PVC awning film according to claim 7, it is characterised in that the sulphur
Change polyphosphazene modified nano-titanium dioxide preparation method be：
In 250 milliliters of round-bottomed flasks, by 0.41 gram of hexachlorocyclotriph,sphazene and 0.92 gram 4,4 '-dihydroxydiphenylsulisomer is dissolved in
In 200 milliliters of acetonitriles, 1.3 milliliters of triethylamines are then added, is placed in 50 DEG C of ultrasonic water baths and reacts 4 hours, after reaction terminates, from
The heart removes solvent, distinguishes washed product 5 times with deionized water and acetone, is finally dried in vacuo 18 hours at 50 DEG C and obtains white
Polyphosphazene powder；
0.6 gram of above-mentioned white polyphosphazene powder is added in 100 milliliters of three-neck flasks, adds 10 milliliters of mass fractions 98%
The concentrated sulfuric acid, it is placed in 50 DEG C of water-baths, reacts 15 hours under mechanical stirring, after reaction terminates, product is slowly poured into cold water
In, and be stirred continuously, unreacted sulfuric acid is centrifuged off, product is then washed with deionized 5 times, finally the vacuum at 50 DEG C
Dry 48 hours and obtain sulfonated phosphazene powder；
0.7 gram of above-mentioned sulfonated phosphazene powder, 0.07 gram of epoxy resin E51, average grain diameter are added in 50 milliliters of three-neck flasks
For 0.5 gram of 150 nanometers of 3 grams of nano titanium oxide, 0.2 gram of silane resin acceptor kh-550 and silane coupler KH-560 with
And 10 milliliters of dimethyl sulfoxide (DMSO)s, heat up 120 DEG C after reacting 2 hours, be down to room temperature and slowly pour into product in cold water, and constantly
Stirring, is then washed with deionized product 5 times, and it is to obtain sulfonated phosphazene to change that 48 hours are finally dried in vacuo at 50 DEG C
Property nano titanium oxide.
9. the preparation method of the special powder calcium zinc stabilizer of environment-friendly type PVC awning film, it is characterised in that including：
Recipe ingredient any one of claim 1-8 is added in homogenizer, stirred under the conditions of 50-100 DEG C
15min-60min, stir speed (S.S.) 1000-2000r/min, obtained after cooling.
10. the preparation method of the special powder calcium zinc stabilizer of environment-friendly type PVC awning film according to claim 9, its feature
It is, 20min, stir speed (S.S.) 1700r/min is stirred under the conditions of 80 DEG C.
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| CN102391592A (en) * | 2011-07-29 | 2012-03-28 | 广东若天新材料科技有限公司 | Environmental-friendly calcium-zinc stabilizer for PVC (Polyvinyl Chloride) rolling film and preparation method thereof |
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| CN102391592A (en) * | 2011-07-29 | 2012-03-28 | 广东若天新材料科技有限公司 | Environmental-friendly calcium-zinc stabilizer for PVC (Polyvinyl Chloride) rolling film and preparation method thereof |
| CN104624067A (en) * | 2014-12-25 | 2015-05-20 | 长春工业大学 | Imidazole functionalized polyether sulfone anion-exchange membrane and preparation method thereof |
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