CN107128940A - A kind of preparation method of the composite modified attapulgite insulating unit material of nano strontium titanate/nano tin dioxide/nano-zinc sulfide - Google Patents
A kind of preparation method of the composite modified attapulgite insulating unit material of nano strontium titanate/nano tin dioxide/nano-zinc sulfide Download PDFInfo
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- CN107128940A CN107128940A CN201710274424.0A CN201710274424A CN107128940A CN 107128940 A CN107128940 A CN 107128940A CN 201710274424 A CN201710274424 A CN 201710274424A CN 107128940 A CN107128940 A CN 107128940A
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- 229960000892 attapulgite Drugs 0.000 title claims abstract description 61
- 229910052625 palygorskite Inorganic materials 0.000 title claims abstract description 61
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 239000005083 Zinc sulfide Substances 0.000 title claims abstract description 29
- 229910052984 zinc sulfide Inorganic materials 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 title claims abstract description 14
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims abstract description 34
- 239000011592 zinc chloride Substances 0.000 claims abstract description 17
- 235000005074 zinc chloride Nutrition 0.000 claims abstract description 17
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000000576 coating method Methods 0.000 claims abstract description 13
- 238000012545 processing Methods 0.000 claims abstract description 13
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 12
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- RXSHXLOMRZJCLB-UHFFFAOYSA-L strontium;diacetate Chemical compound [Sr+2].CC([O-])=O.CC([O-])=O RXSHXLOMRZJCLB-UHFFFAOYSA-L 0.000 claims abstract description 12
- 235000014121 butter Nutrition 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims abstract description 11
- 238000009413 insulation Methods 0.000 claims abstract description 11
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 238000010792 warming Methods 0.000 claims description 14
- 238000003760 magnetic stirring Methods 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 10
- 230000005684 electric field Effects 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 239000002002 slurry Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 229910052712 strontium Inorganic materials 0.000 claims description 5
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 4
- 239000011701 zinc Substances 0.000 claims description 4
- 229910052725 zinc Inorganic materials 0.000 claims description 4
- 238000004073 vulcanization Methods 0.000 claims description 3
- 240000007594 Oryza sativa Species 0.000 claims description 2
- 235000007164 Oryza sativa Nutrition 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 235000009566 rice Nutrition 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 2
- 239000002086 nanomaterial Substances 0.000 claims 2
- 229910001887 tin oxide Inorganic materials 0.000 claims 2
- 230000000694 effects Effects 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 abstract description 4
- 239000011941 photocatalyst Substances 0.000 abstract description 4
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 239000002689 soil Substances 0.000 abstract description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000004321 preservation Methods 0.000 description 5
- 238000004659 sterilization and disinfection Methods 0.000 description 4
- 230000001934 delay Effects 0.000 description 3
- 239000008236 heating water Substances 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 230000001954 sterilising effect Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
- 229910002113 barium titanate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000002734 clay mineral Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
- 229910052919 magnesium silicate Inorganic materials 0.000 description 1
- 235000019792 magnesium silicate Nutrition 0.000 description 1
- 239000000391 magnesium silicate Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/36—Silicates having base-exchange properties but not having molecular sieve properties
- C01B33/38—Layered base-exchange silicates, e.g. clays, micas or alkali metal silicates of kenyaite or magadiite type
- C01B33/40—Clays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/005—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing gelatineous or gel forming binders, e.g. gelatineous Al(OH)3, sol-gel binders
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00017—Aspects relating to the protection of the environment
Abstract
The invention discloses a kind of preparation method of the composite modified attapulgite insulating unit material of nano strontium titanate/nano tin dioxide/nano-zinc sulfide, the present invention is using sulfuric acid combination high-pressure pulse electric processing attapulgite, shale impurity and the carbonate impurities in original soil ore deposit can not only be removed, but also hole can be dredged, the specific surface area of attapulgite is improved, so as to improve the effect of heat insulation of attapulgite insulating unit；Then using the attapulgite after above-mentioned processing as carrier, zinc chloride and thioacetamide are raw material, attapulgite loaded nano-zinc sulfide is made by hydro-thermal method, again using take strontium acetate, butyl titanate and butter of tin as presoma pass through sol-gal process be made plural gel, then plural gel is coated into attapulgite loaded nano-zinc sulfide, produced through vacuum freeze drying, calcining, the composite has good heat-proof quality and photocatalysis performance, insulating unit is acted not only as, photocatalyst is also used as applied to insulating mold coating.
Description
Technical field
The present invention relates to a kind of preparation method of attapulgite modified insulating unit material, and in particular to a kind of nano barium titanate
The preparation method of the composite modified attapulgite insulating unit material of strontium/nano tin dioxide/nano-zinc sulfide.
Background technology
The research application of wall thermal insulation technology has positive role for the reduction and environmental protection of building energy consumption, and performance is excellent
Good wall thermal insulating heat-barrier material is the material base of energy-conservation, is played a multiplier effect in building heat preservation.It is wherein heat-insulated
Thermal insulation coatings occupy critical role in wall thermal insulating heat-barrier material, can save building energy consumption more than 30%.
Attapulgite is that a kind of crystal formation is 2:1 rich magnesium silicate clay mineral, its structure is layer chain, and outward appearance is in needle-like
Or threadiness.The specific surface area of attapulgite is big（160-210m2/g）, special layer chain crystal structure makes it have flourishing
Zeolites duct, forms aggregation loose structure, and gas is closed in the duct of countless small non-interconnected, makes convection heat transfer' heat-transfer by convection efficiency
Ignore, due to the thermal conductivity factor very little of gas, therefore attapulgite can be made into the good heat-insulation and heat-preservation painting of heat-insulating property
The insulating unit material of material.
Cheng Sheng, Wang Qunying et al. are at it《The attapulgite modified novel aqueous thermal-insulating external-wall coating as insulating unit
Prepare》Elaborated in one text after the HCl treatment that attapulgite uses 2mol/L, then concave convex rod is handled with Silane coupling agent KH550
Soil, can significantly improve the effect of heat insulation of attapulgite insulating unit, be added in insulating moulding coating, insulating moulding coating it is heat-insulated
Work well.But with the fast development and the fast development of coatings industry of living standards of the people, to the functionalization of coating
It is required that more and more higher, attapulgite modified function made from above-mentioned document is relatively simple, only it is applied to as insulating unit heat-insulated
Coating.Therefore, the present invention have studied a kind of nano strontium titanate/composite modified attapulgite of nano tin dioxide/nano-zinc sulfide every
The preparation method of hot cell material, it is obtained attapulgite modified with good heat-proof quality and photocatalysis performance, not only may be used
As insulating unit, to be also used as photocatalyst applied to insulating mold coating, heat-insulation and heat-preservation, environment purification, sterilization are played
The effect of sterilization.
The content of the invention
It is an object of the invention to a kind of nano strontium titanate/composite modified attapulgite of nano tin dioxide/nano-zinc sulfide
The preparation method of insulating unit material.It is produced by the present invention attapulgite modified with good heat-proof quality and photocatalytic
Can, insulating unit is acted not only as, photocatalyst is also used as applied to insulating mold coating, heat-insulation and heat-preservation, purification is played
The effect of environment, disinfection.
To achieve the above object, the present invention is adopted the following technical scheme that：
A kind of preparation side of the composite modified attapulgite insulating unit material of nano strontium titanate/nano tin dioxide/nano-zinc sulfide
Method, comprises the following steps：
（1）According to solid-to-liquid ratio 1:20~30 are added to attapulgite in the sulfuric acid solution that molar concentration is 1mol/L, and water-bath adds
Heat is to 70~80 DEG C, then to carrying out high-pressure pulse electric processing, and electric-field intensity is 40~50kV/cm, and impulse electric field frequency is
300~400Hz, processing time be 3~6s, after being disposed under 1500~2500r/min rotating speed stirring 20~
30min, filter, washing, after drying power for 200~300W microwave under heat 30~50min, then power be 400~
15~25min is heated under 500W microwave, room temperature is cooled to, it is stand-by；
（2）According to mol ratio 1:1:0.4-0.6 weighs strontium acetate, butyl titanate and butter of tin, and strontium acetate then is dissolved in into 3
In the distilled water of~4 times of quality, solution A is obtained；In the isopropanol that butyl titanate is dissolved in 15~20 times of volumes, solution B is obtained；Will
Butter of tin is dissolved in distilled water and is configured to the solution that concentration is 0.5mol/L, obtains solution C；
（3）Solution A is slowly added into solution B under magnetic stirring, continues to stir 2~4min, then again in magnetic agitation
Under be slowly added to solution C, continue to stir 3~5min, in being slowly added to the ammonia spirit that mass fraction is 5% under magnetic agitation, adjust
Solution PH=7~8 are saved, continues to stir to gel appearance, is washed with water to no Cl-；
（4）According to mass ratio 1:4 weigh thioacetamide and zinc chloride, stand-by；
（5）The step of taking equivalent to 4~6 times of quality of zinc chloride（1）The stirring that adds water of obtained attapulgite is made weight concentration and is
50~55% slurries, ultrasonic disperse 15~25min is stand-by；
（6）In the water that zinc chloride is dissolved in 10~15 times of quality, thioacetamide is added, is stirred after stirring in magnetic force
Mix lower addition step（5）Obtained slurries, 20~30min of ultrasonic disperse, the constant temperature stirring reaction 1 under 60~70 DEG C of bath temperatures
~3h, is cooled to room temperature, and suction filtration, washes clean is dried under vacuum to constant weight at a temperature of 70~80 DEG C, produces attapulgite loaded
Nano-zinc sulfide；
（7）According to mass ratio 1:3~4 by step（3）Obtained gel and step（6）Obtained attapulgite loaded nanometer vulcanization
Zinc is mixed, and 10~15min is stirred under 1500~2000r/min rotating speed, stands 24~48h, is placed in after filtering in liquid nitrogen fast
Quickly cooling is frozen, then put temperature be -35~-50 DEG C, vacuum be 24~48h of vacuum freeze drying under conditions of 8-12Pa, it is dry
After dry at 290~340 DEG C 1~2h of pre-burning, be warming up to 460~520 DEG C, 1.5~2.5h of constant temperature, then be warming up to 570~630
DEG C, 1~2h of constant temperature, then it is warming up to 680~760 DEG C, 0.5~1.5h of insulation, natural cooling, next day taking-up, receiving needed for producing
The rice composite modified attapulgite insulating unit material of strontium titanates/nano tin dioxide/nano-zinc sulfide.
Step（5）Described in ultrasonic power be 200~300W.
Step（6）Described in ultrasonic power be 150~250W.
Beneficial effects of the present invention：
The present invention is handled attapulgite using sulfuric acid combination high-pressure pulse electric, can not only remove the mud in original soil ore deposit
Matter impurity and carbonate impurities, but also hole can be dredged, the specific surface area of attapulgite is greatly improved, so as to significantly improve
The effect of heat insulation of attapulgite insulating unit；Then using the attapulgite after above-mentioned processing as carrier, zinc chloride and thioacetyl
Amine is raw material, and attapulgite loaded nano-zinc sulfide is made by hydro-thermal method, then to take strontium acetate, butyl titanate and four chlorinations
Tin is that plural gel is made by sol-gal process in presoma, and plural gel then is coated into attapulgite loaded nanometer vulcanizes
Zinc, through vacuum freeze drying, calcining produce nano strontium titanate/composite modified attapulgite of nano tin dioxide/nano-zinc sulfide every
Hot cell material, the composite has good heat-proof quality and photocatalysis performance, acts not only as insulating unit, may be used also
To be applied to insulating mold coating as photocatalyst, play a part of heat-insulation and heat-preservation, environment purification, disinfection.
Embodiment
Embodiment 1
A kind of preparation side of the composite modified attapulgite insulating unit material of nano strontium titanate/nano tin dioxide/nano-zinc sulfide
Method, comprises the following steps：
（1）According to solid-to-liquid ratio 1:20 are added to attapulgite in the sulfuric acid solution that molar concentration is 1mol/L, and heating water bath is extremely
70 DEG C, then to carrying out high-pressure pulse electric processing, electric-field intensity is 40kV/cm, and impulse electric field frequency is 300Hz, during processing
Between be 6s, stirring 30min under 1500r/min rotating speed after being disposed, filter, washing, after drying power be 200W
Microwave under heat 50min, then heat 25min in the case where power is 400W microwave, be cooled to room temperature, it is stand-by；
（2）According to mol ratio 1:1:0.5 weighs strontium acetate, butyl titanate and butter of tin, and strontium acetate then is dissolved in into 3 times of matter
In the distilled water of amount, solution A is obtained；In the isopropanol that butyl titanate is dissolved in 15 times of volumes, solution B is obtained；Butter of tin is molten
The solution that concentration is 0.5mol/L is configured in distilled water, solution C is obtained；
（3）Solution A is slowly added into solution B under magnetic stirring, continues to stir 2min, then delays under magnetic stirring again
It is slow to add solution C, continue to stir 3min, in being slowly added to the ammonia spirit that mass fraction is 5% under magnetic agitation, adjust solution
PH=7, continue to stir to gel appearance, are washed with water to no Cl-；
（4）According to mass ratio 1:4 weigh thioacetamide and zinc chloride, stand-by；
（5）The step of taking equivalent to 4 times of quality of zinc chloride（1）Weight concentration is made for 50% in the stirring that adds water of obtained attapulgite
Slurries, ultrasonic disperse 15min is stand-by；
（6）In the water that zinc chloride is dissolved in 10 times of quality, thioacetamide is added, after stirring under magnetic stirring
Add step（5）Obtained slurries, ultrasonic disperse 20min, constant temperature stirring reaction 3h, is cooled to room under 60 DEG C of bath temperatures
Temperature, suction filtration, washes clean is dried under vacuum to constant weight at a temperature of 70 DEG C, produces attapulgite loaded nano-zinc sulfide；
（7）According to mass ratio 1:3 by step（3）Obtained gel and step（6）Obtained attapulgite loaded nano-zinc sulfide
Mixing, stirs 15min under 1500r/min rotating speed, stands 24h, snap frozen in liquid nitrogen is placed in after filtering, is then put in temperature
It is vacuum freeze drying 24h under conditions of 8Pa to spend for -35 DEG C, vacuum, after drying at 290 DEG C pre-burning 2h, be warming up to 460
DEG C, constant temperature 2.5h, then be warming up to 570 DEG C, constant temperature 2h, then it is warming up to 680 DEG C, 1.5h is incubated, natural cooling, next day takes out, i.e.,
Obtain the required composite modified attapulgite insulating unit material of nano strontium titanate/nano tin dioxide/nano-zinc sulfide.
Step（5）Described in ultrasonic power be 300W.
Step（6）Described in ultrasonic power be 250W.
Embodiment 2
A kind of preparation side of the composite modified attapulgite insulating unit material of nano strontium titanate/nano tin dioxide/nano-zinc sulfide
Method, comprises the following steps：
（1）According to solid-to-liquid ratio 1:25 are added to attapulgite in the sulfuric acid solution that molar concentration is 1mol/L, and heating water bath is extremely
75 DEG C, then to carrying out high-pressure pulse electric processing, electric-field intensity is 45kV/cm, and impulse electric field frequency is 350Hz, during processing
Between be 5s, stirring 25min under 2000r/min rotating speed after being disposed, filter, washing, after drying power be 250W
Microwave under heat 40min, then heat 20min in the case where power is 450W microwave, be cooled to room temperature, it is stand-by；
（2）According to mol ratio 1:1:0.5 weighs strontium acetate, butyl titanate and butter of tin, and strontium acetate then is dissolved in into 3.5 times
In the distilled water of quality, solution A is obtained；In the isopropanol that butyl titanate is dissolved in 18 times of volumes, solution B is obtained；By butter of tin
It is dissolved in distilled water and is configured to the solution that concentration is 0.5mol/L, obtains solution C；
（3）Solution A is slowly added into solution B under magnetic stirring, continues to stir 3min, then delays under magnetic stirring again
It is slow to add solution C, continue to stir 4min, in being slowly added to the ammonia spirit that mass fraction is 5% under magnetic agitation, adjust solution
PH=7.5, continue to stir to gel appearance, are washed with water to no Cl-；
（4）According to mass ratio 1:4 weigh thioacetamide and zinc chloride, stand-by；
（5）The purifying attapulgite taken equivalent to 5 times of quality of zinc chloride add water stirring be made weight concentration be 52% slurries, surpass
Sound disperses 20min, stand-by；
（6）In the water that zinc chloride is dissolved in 12 times of quality, thioacetamide is added, after stirring under magnetic stirring
Add step（5）Obtained slurries, ultrasonic disperse 25min, constant temperature stirring reaction 2h, is cooled to room under 65 DEG C of bath temperatures
Temperature, suction filtration, washes clean is dried under vacuum to constant weight at a temperature of 75 DEG C, produces attapulgite loaded nano-zinc sulfide；
（7）According to mass ratio 1:3.5 by step（3）Obtained gel and step（6）Obtained attapulgite loaded nanometer vulcanization
Zinc is mixed, and 12min is stirred under 1800r/min rotating speed, stands 36h, snap frozen in liquid nitrogen is placed in after filtering, is then put
Temperature is -40 DEG C, vacuum is vacuum freeze drying 36h under conditions of 10Pa, after drying at 310 DEG C pre-burning 1.5h, heating
To 490 DEG C, constant temperature 2h, then be warming up to 600 DEG C, constant temperature 1.5h, then it is warming up to 620 DEG C, 1h is incubated, natural cooling, next day takes out,
Produce the required composite modified attapulgite insulating unit material of nano strontium titanate/nano tin dioxide/nano-zinc sulfide.
Step（5）Described in ultrasonic power be 250W.
Step（6）Described in ultrasonic power be 200W.
Embodiment 3
A kind of preparation side of the composite modified attapulgite insulating unit material of nano strontium titanate/nano tin dioxide/nano-zinc sulfide
Method, comprises the following steps：
（1）According to solid-to-liquid ratio 1:30 are added to attapulgite in the sulfuric acid solution that molar concentration is 1mol/L, and heating water bath is extremely
80 DEG C, then to carrying out high-pressure pulse electric processing, electric-field intensity is 50kV/cm, and impulse electric field frequency is 400Hz, during processing
Between be 3s, stirring 20min under 2500r/min rotating speed after being disposed, filter, washing, after drying power be 300W
Microwave under heat 30min, then heat 15min in the case where power is 500W microwave, be cooled to room temperature, it is stand-by；
（2）According to mol ratio 1:1:0.6 weighs strontium acetate, butyl titanate and butter of tin, and strontium acetate then is dissolved in into 4 times of matter
In the distilled water of amount, solution A is obtained；In the isopropanol that butyl titanate is dissolved in 20 times of volumes, solution B is obtained；Butter of tin is molten
The solution that concentration is 0.5mol/L is configured in distilled water, solution C is obtained；
（3）Solution A is slowly added into solution B under magnetic stirring, continues to stir 4min, then delays under magnetic stirring again
It is slow to add solution C, continue to stir 5min, in being slowly added to the ammonia spirit that mass fraction is 5% under magnetic agitation, adjust solution
PH=8, continue to stir to gel appearance, are washed with water to no Cl-；
（4）According to mass ratio 1:4 weigh thioacetamide and zinc chloride, stand-by；
（5）The step of taking equivalent to 6 times of quality of zinc chloride（1）Weight concentration is made for 55% in the stirring that adds water of obtained attapulgite
Slurries, ultrasonic disperse 25min is stand-by；
（6）In the water that zinc chloride is dissolved in 15 times of quality, thioacetamide is added, after stirring under magnetic stirring
Add step（5）Obtained slurries, ultrasonic disperse 30min, constant temperature stirring reaction 1h, is cooled to room under 70 DEG C of bath temperatures
Temperature, suction filtration, washes clean is dried under vacuum to constant weight at a temperature of 80 DEG C, produces attapulgite loaded nano-zinc sulfide；
（7）According to mass ratio 1:4 by step（3）Obtained gel and step（6）Obtained attapulgite loaded nano-zinc sulfide
Mixing, stirs 10min under 2000r/min rotating speed, stands 48h, snap frozen in liquid nitrogen is placed in after filtering, is then put in temperature
It is vacuum freeze drying 48h under conditions of 12Pa to spend for -50 DEG C, vacuum, after drying at 340 DEG C pre-burning 1h, be warming up to 520
DEG C, constant temperature 1.5h, then be warming up to 630 DEG C, constant temperature 1h, then it is warming up to 760 DEG C, 0.5h is incubated, natural cooling, next day takes out, i.e.,
Obtain the required composite modified attapulgite insulating unit material of nano strontium titanate/nano tin dioxide/nano-zinc sulfide.
Step（5）Described in ultrasonic power be 200W.
Step（6）Described in ultrasonic power be 1500W.
Claims (3)
1. a kind of preparation of the composite modified attapulgite insulating unit material of nano strontium titanate/nano tin dioxide/nano-zinc sulfide
Method, it is characterised in that comprise the following steps：
(1) according to solid-to-liquid ratio 1:20~30 are added to attapulgite in the sulfuric acid solution that molar concentration is 1mol/L, and water-bath adds
Heat is to 70~80 DEG C, then to carrying out high-pressure pulse electric processing, and electric-field intensity is 40~50kV/cm, and impulse electric field frequency is
300~400Hz, processing time be 3~6s, after being disposed under 1500~2500r/min rotating speed stirring 20~
30min, filter, washing, after drying power for 200~300W microwave under heat 30~50min, then power be 400~
15~25min is heated under 500W microwave, room temperature is cooled to, it is stand-by；
(2) according to mol ratio 1:1:0.4~0.6 weighs strontium acetate, butyl titanate and butter of tin, is then dissolved in strontium acetate
In the distilled water of 3~4 times of quality, solution A is obtained；In the isopropanol that butyl titanate is dissolved in 15~20 times of volumes, solution B is obtained；
Butter of tin is dissolved in distilled water and is configured to the solution that concentration is 0.5mol/L, solution C is obtained；
(3) solution A is slowly added into solution B under magnetic stirring, continues to stir 2~4min, then again in magnetic agitation
Under be slowly added to solution C, continue to stir 3~5min, in being slowly added to the ammonia spirit that mass fraction is 5% under magnetic agitation, adjust
Solution PH=7~8 are saved, continues to stir to gel appearance, is washed with water to no Cl-；
(4) according to mass ratio 1:4 weigh thioacetamide and zinc chloride, stand-by；
(5) the step of taking equivalent to 4~6 times of quality of zinc chloride（1）The stirring that adds water of obtained attapulgite is made weight concentration and is
50~55% slurries, ultrasonic disperse 15~25min is stand-by；
(6) zinc chloride is dissolved in the water of 10~15 times of quality, adds thioacetamide, stirred after stirring in magnetic force
Mix lower addition step（5）Obtained slurries, 20~30min of ultrasonic disperse, the constant temperature stirring reaction 1 under 60~70 DEG C of bath temperatures
~3h, is cooled to room temperature, and suction filtration, washes clean is dried under vacuum to constant weight at a temperature of 70~80 DEG C, produces attapulgite loaded
Nano-zinc sulfide；
(7) according to mass ratio 1:3~4 by step（3）Obtained gel and step（6）Obtained attapulgite loaded nanometer vulcanization
Zinc is mixed, and 10~15min is stirred under 1500~2000r/min rotating speed, stands 24~48h, is placed in after filtering in liquid nitrogen fast
Quickly cooling is frozen, then put temperature be -35~-50 DEG C, vacuum be 24~48h of vacuum freeze drying under conditions of 8-12Pa, it is dry
After dry at 290~340 DEG C 1~2h of pre-burning, be warming up to 460~520 DEG C, 1.5~2.5h of constant temperature, then be warming up to 570~630
DEG C, 1~2h of constant temperature, then it is warming up to 680~760 DEG C, 0.5~1.5h of insulation, natural cooling, next day taking-up, receiving needed for producing
The rice composite modified attapulgite insulating unit material of strontium titanates/nano tin dioxide/nano-zinc sulfide.
2. a kind of light catalyzed coating according to claim 1 is compound with attapulgite loaded strontium titanates/tin oxide/zinc sulphide
The preparation method of nano material, it is characterised in that step（5）Described in ultrasonic power be 200~300W.
3. a kind of light catalyzed coating according to claim 1 is compound with attapulgite loaded strontium titanates/tin oxide/zinc sulphide
The preparation method of nano material, it is characterised in that step（6）Described in ultrasonic power be 150~250W.
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