CN106179521A - A kind of preparation method of the magnetic attapulgite clay of loaded composite photocatalysis agent - Google Patents
A kind of preparation method of the magnetic attapulgite clay of loaded composite photocatalysis agent Download PDFInfo
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- CN106179521A CN106179521A CN201610536347.7A CN201610536347A CN106179521A CN 106179521 A CN106179521 A CN 106179521A CN 201610536347 A CN201610536347 A CN 201610536347A CN 106179521 A CN106179521 A CN 106179521A
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- 229960000892 attapulgite Drugs 0.000 title claims abstract description 69
- 229910052625 palygorskite Inorganic materials 0.000 title claims abstract description 69
- 239000004927 clay Substances 0.000 title claims abstract description 60
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 19
- 239000002131 composite material Substances 0.000 title claims abstract description 19
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 18
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 11
- 239000012153 distilled water Substances 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims abstract description 4
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 4
- 230000007935 neutral effect Effects 0.000 claims abstract description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 4
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 7
- 239000011941 photocatalyst Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 230000006837 decompression Effects 0.000 claims description 3
- 238000005304 joining Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 238000001556 precipitation Methods 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- JGPSMWXKRPZZRG-UHFFFAOYSA-N zinc;dinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O JGPSMWXKRPZZRG-UHFFFAOYSA-N 0.000 claims description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims 1
- 229910052738 indium Inorganic materials 0.000 claims 1
- 229960000935 dehydrated alcohol Drugs 0.000 abstract description 8
- 238000010521 absorption reaction Methods 0.000 abstract description 6
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 abstract 1
- 229960004756 ethanol Drugs 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 7
- 238000004043 dyeing Methods 0.000 description 6
- 229910001385 heavy metal Inorganic materials 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 5
- 238000001994 activation Methods 0.000 description 4
- 230000004913 activation Effects 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000002689 soil Substances 0.000 description 4
- 150000002500 ions Chemical class 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004088 simulation Methods 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 239000002734 clay mineral Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 238000004042 decolorization Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000010842 industrial wastewater Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 2
- 229940012189 methyl orange Drugs 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- JAUGGEIKQIHSMF-UHFFFAOYSA-N dialuminum;dimagnesium;dioxido(oxo)silane;oxygen(2-);hydrate Chemical class O.[O-2].[O-2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O JAUGGEIKQIHSMF-UHFFFAOYSA-N 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000007725 thermal activation Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
Classifications
-
- 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
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/16—Clays or other mineral silicates
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
-
- B01J35/33—
Abstract
The invention discloses the preparation method of the magnetic attapulgite clay of a kind of loaded composite photocatalysis agent, step: attapulgite clay powder body is mixed by (a) with water, stirring is dried, and obtains purifying attapulgite clay；B () joins hydrochloric acid solution, by pure water rinsing, add silver nitrate, heating, drying, sieves, and obtains acid attapulgite modified；C () joins FeCl3Solution soaks, ultrasonic disperse；Add FeCl3Solution, ultrasonic disperse, drip ammonia, ultrasonic, centrifugal, washing, to neutral, obtains magnetic attapulgite；D () joins ethanol solution, ultrasonic cleaning, add zinc nitrate hexahydrate and ferric chloride (FeCl36H2O), be sufficiently stirred for, and drips NaOH, regulates pH value；It is centrifuged again, washs, is dried, then mix with cetyl trimethylammonium bromide, distilled water, dehydrated alcohol, with distilled water and the washing of dehydrated alcohol alternating centrifugal, sucking filtration, be dried, prepare the magnetic attapulgite clay of loaded composite photocatalysis agent.It has the strongest absorption property and carrier property.
Description
Technical field
The present invention relates to the preparation method of the magnetic attapulgite clay of a kind of loaded composite photocatalysis agent, belong to sewage disposal
Technical field.
Background technology
In recent years, about attapulgite as sorbent treatment industrial wastewater research oneself have been reported that.Attapulgite is one
Kind have the absorption property of excellence and certain ion-exchange capacity containing Shuifu County town silicate clay mineral.Concavo-convex after activation
The features such as rod soil heavy metal ion has good adsorption cleaning effect, has treatment effeciency high, absorption low cost.
It is applied to water body at attapulgite clay as adsorbent and goes in heavy metal pollution removing, typically attapulgite clay is carried out
Acid activation, alkali activation, salt activation and thermal activation etc..The cutting mechanisms of this method is usually Electrostatic Absorption, ion exchange etc. and makees
With.Although there being certain effect, but during removing removing heavy metals, be easily subject to Na+, Ca2+etc. the competition of cation
Adsorption Effect.Research organically-modified for attapulgite clay, is concentrated mainly on some coupling agents of application or some cation forms
Face activating agent is modified, and by organic group grafting on the surface of attapulgite, and then strengthens its hydrophobicity, forms heavy metal
The adsorption activity center of ion and organic pollution, improves organic pollution and the Adsorption of heavy metal, and can use up
Possible neglects interionic competitive Adsorption.
Nano-ZnO is the photocatalyst of a kind of function admirable, can effectively the harmful organic substance in degradation water the most organic
Chloride, activating agent, pesticide, pigment etc., the response speed of nanometer particle is 100-1000 times of ordinary particle, and with general
Logical particle is compared, and it is substantially without causing scattering of light, and its specific surface area is very big and energy band is the widest, so it is considered
It it is one of the photocatalyst of great application prospect.The ZnO particle of nanorize hexagonal crystal system wurtzite structure, it is optical, electrical, sensitive
Nano effect out of the ordinary and the high Photocatalytic activity to organic pollution is shown so that it is processing organic contamination in field
Aspect has potential application economic worth.But, there is the problem reclaiming difficulty in the nano-ZnO for photocatalyst, these
Photocatalyst can disperse to exist in aqueous, is therefore reclaiming and there is disadvantage in recycling.And attapulgite glues
Soil is a kind of porous type chain layered hydrous richness magnesium alumino metasilicate salt clay mineral, in recent years, about attapulgite as adsorbent
Process industrial wastewater research oneself have been reported that, attapulgite clay has the strongest absorption property and carrier property, also has prosperity
Duct, bigger specific surface area, modified attapulgite heavy metal ion has good adsorption cleaning effect, and price
Cheap, adsorb the features such as low cost.
Summary of the invention
The invention aims to solve defect present in prior art, it is provided that a kind of loaded composite photocatalysis agent
The preparation method of magnetic attapulgite clay, magnetic attapulgite clay prepared by the method can realize magnetic at the dyeing waste water that degraded is difficult
Control separates, and reaches cycling and reutilization.
In order to achieve the above object, the invention provides the system of the magnetic attapulgite clay of a kind of loaded composite photocatalysis agent
Preparation Method, comprises the following steps:
(a) purification attapulgite clay:
First, attapulgite clay is pulverized and sieved, obtain the attapulgite clay powder body that granular size is 100 mesh, attapulgite is glued
Soil powder body and water with weight ratio as 1:(8～10) ratio mix, be that 200～300 r/min stir 2 h with rotary speed, stir
After refilter, be dried, obtain attapulgite clay after purifying clay；
(b) preparation acid modified attapulgite clay
Above-mentioned attapulgite clay after purifying clay is joined in the hydrochloric acid solution that concentration is 5%, be 250～300 with rotary speed
R/min is stirred acidified modified 2～3 h；It is neutral by pure water rinsing to pH value again after stirring, adds silver nitrate, until
Precipitation disappears；It is then heated at 105～110 DEG C dry, crosses 200 mesh sieves, obtain the modified attapulgite powder of acid and preserve
In drying baker standby；
C () prepares magnetic modified attapulgite clay
The concentration taking the 1.0g attapulgite modified 50mL of joining of acid is 0.15～0.2mol L-1FeCl3Solution soaks, super
Sound dispersion 3h, obtain ultrasonic after the first dispersion soln a；The concentration adding 50mL is 0.4～0.45mol L-1FeCl3Molten
Liquid, continues ultrasonic disperse 2 h, passs dropping concentration 8mol L-1Ammonia spirit be 10.5～11.5 to pH value, continue ultrasonic 1～2
H, obtain ultrasonic after the second dispersion soln b；Being centrifuged, the distilled water solution of the precipitate after being centrifuged washs to pH value again
For neutrality, it is dried after being centrifuged, obtains magnetic attapulgite, be stored in drying baker standby；
D () prepares the loaded optic catalyst of the attapulgite clay of loaded composite photocatalysis agent
After step (c), taking the attapulgite clay after purifying clay 3g that above-mentioned steps (a) obtains, to join 50mL dehydrated alcohol molten
In liquid so that it is full and uniform mixing, using ultrasonic washing unit ultrasonic cleaning 15min, stand 10～12 h, adding concentration is
6mmol L-1Zinc nitrate hexahydrate Zn (N03)2·6H20 and ferric chloride (FeCl36H2O) (FeCl that concentration is 4mmol3·6H2O), fill
Divide stirring, be 0.10 mol L to mixed solution and dripping concentration-1NaOH, regulation pH value be 7～8, stir 15min；Again will
Mixed liquor is centrifuged under 3500r/min rotating speed, is washed out, is dried, then with the cetyl trimethylammonium bromide of 0.lg,
The distilled water of 30mL, the dehydrated alcohol mixing of 15mL, put into after mixing in hydrothermal reaction kettle, heat 180～200 DEG C, and hydro-thermal is anti-
Answer 24h, with distilled water and the washing of dehydrated alcohol alternating centrifugal, decompression sucking filtration after reaction, be again heated at 350 DEG C be dried 2h, warp
Grind, cross 200 mesh sieves, prepare the magnetic attapulgite clay of loaded composite photocatalysis agent.
The present invention compared with prior art has the advantage that the recessed of the magnetic carrying composite photo-catalyst prepared by the method
Convex rod clay is that load two kinds exists complementary composite photo-catalyst, has the strongest absorption property and carrier property, in degraded
Difficult dyeing waste water realizes magnetic control and separates, it is achieved cycling and reutilization.
Detailed description of the invention
Below, in conjunction with instantiation, the present invention is further described.
Embodiment
The preparation method of the magnetic attapulgite clay of the present invention a kind of loaded composite photocatalysis agent, it is characterised in that the most such as
Under process and step:
(a) purification attapulgite clay:
First, attapulgite clay is pulverized and sieved, obtain the attapulgite clay powder body that granular size is 100 mesh, attapulgite is glued
Soil powder body mixes with the water ratio with weight ratio as 1:10, is that 200～300 r/min stir 2 h, after stirring again with rotary speed
Filter, be dried, obtain attapulgite clay after purifying clay；
(b) preparation acid modified attapulgite clay
Above-mentioned attapulgite clay after purifying clay is joined in the hydrochloric acid solution that concentration is 5%, be 250～300 with rotary speed
R/min is stirred acidified modified 3 h；It is neutral by pure water rinsing to pH value again after stirring, adds silver nitrate, until precipitation
Disappear；It is then heated at 110 DEG C dry, crosses 200 mesh sieves, obtain the modified attapulgite powder of acid and be stored in drying baker
Standby；
C () prepares magnetic modified attapulgite clay
The concentration taking the 1.0g attapulgite modified 50mL of joining of acid is 0.15～0.2mol L-1FeCl3Solution soaks, ultrasonic
Dispersion 3h, obtain ultrasonic after the first dispersion soln a；The concentration adding 50mL is 0.4～0.45mol L-1FeCl3Solution,
Continue ultrasonic disperse 2h, pass dropping concentration 8mol L-1Ammonia spirit be 10.5～11.5 to pH value, continue ultrasonic 1～2h,
To the second dispersion soln b after ultrasonic；It is centrifuged again, during the precipitate distilled water solution washing after being centrifuged to pH value is
Property, it is dried after being centrifuged, obtains magnetic attapulgite, be stored in drying baker standby；
D () prepares the loaded optic catalyst of the attapulgite clay of loaded composite photocatalysis agent
After step (c), taking the attapulgite clay after purifying clay 3g that above-mentioned steps (a) obtains, to join 50mL dehydrated alcohol molten
In liquid so that it is full and uniform mixing, using ultrasonic washing unit ultrasonic cleaning 15min, stand 10～12h, adding concentration is
6mmol L-1Zinc nitrate hexahydrate Zn (N03)2·6H20 and ferric chloride (FeCl36H2O) (FeCl that concentration is 4mmol3·6H2O), fill
Divide stirring, be 0.10 mol L to mixed solution and dripping concentration-1NaOH, regulation pH value be 7～8, stir 15min；Again will
Mixed liquor is centrifuged under 3500r/min rotating speed, is washed out, is dried, then with the cetyl trimethylammonium bromide of 0.lg,
The distilled water of 30mL, the dehydrated alcohol mixing of 15mL, put into after mixing in hydrothermal reaction kettle, be heated to 180～200 DEG C, hydro-thermal
Reaction 24h, with distilled water and the washing of dehydrated alcohol alternating centrifugal, decompression sucking filtration after reaction, is again heated at 350 DEG C be dried 2h,
Ground, 200 mesh sieves excessively, prepare the magnetic attapulgite clay of loaded composite photocatalysis agent.
In order to verify the magnetic attapulgite clay decolouring at dyeing waste water of loaded composite photocatalysis agent prepared by the present invention
Degradation effect, tests the most as follows:
Test case 1
The magnetic attapulgite clay of 100mg loaded composite photocatalysis agent is joined the simulation printing and dyeing that 50mL concentration is 100mg/L
In the methyl orange solution of waste water, temperature is adjusted to 25 DEG C, at the irradiation 5h of simulation nature light, and uses the vibration of 150 r/min
Device shakes, and the percent of decolourization recording methyl orange is 74.2%, and reuses after magnetic control recovery eluting, and it has the most again
Raw utility.
Test case 2
The magnetic attapulgite clay of 100mg loaded composite photocatalysis agent is joined 50mL dyeing waste water (extracting from printing and dyeing mill)
In tail water, temperature is adjusted to 25 DEG C, at the irradiation 5h of simulation nature light, and uses the agitator of 150 r/min constantly to shake, and surveys
The percent of decolourization obtaining methyl orange is 71.8%, and reuses after magnetic control recovery eluting, and it has preferable regeneration
Energy.
Claims (1)
1. the preparation method of the magnetic attapulgite clay of a loaded composite photocatalysis agent, it is characterised in that the method include with
Lower step:
(a). purify attapulgite clay: first, pulverized and sieved by attapulgite clay, obtain the attapulgite that granular size is 100 mesh
Clay powder body, by attapulgite clay powder body and water with weight ratio as 1:(8～10) ratio mix, with rotary speed be 200～
300 r/min stir 2 h, refilter, be dried, obtain attapulgite clay after purifying clay after stirring；
(b). preparation acid modified attapulgite clay: above-mentioned attapulgite clay after purifying clay is joined the hydrochloric acid that concentration is 5%
In solution, it is that 250～300 r/min are stirred acidified modified 2～3 h with rotary speed；Again by pure water rinsing to pH after stirring
Value is neutrality, adds silver nitrate, until precipitation disappears；It is then heated at 105～110 DEG C dry, crosses 200 mesh sieves, obtain
The modified attapulgite powder of acid is stored in drying baker standby；
(c). prepare magnetic modified attapulgite clay: take the concentration of the 1.0g attapulgite modified 50mL of joining of acid be 0.15～
0.2mol L-1FeCl3In solution soak, ultrasonic disperse 3h, obtain ultrasonic after the first dispersion soln a；Add the dense of 50mL
Degree is 0.4～0.45mol L-1FeCl3Solution, continues ultrasonic disperse 2 h, passs dropping concentration 8mol L-1Ammonia spirit to pH
Value is 10.5～11.5, continues ultrasonic 1～2 h, obtain ultrasonic after the second dispersion soln b；It is centrifuged again, after being centrifuged
Precipitate distilled water solution washing to pH value is neutral, is dried, obtains magnetic attapulgite, be stored in dry after being centrifuged
In case standby；
(d). prepare the loaded optic catalyst of the attapulgite clay of loaded composite photocatalysis agent: after step (c), take above-mentioned
The attapulgite clay after purifying clay 3g that step (a) obtains joins in 50mL ethanol solution so that it is full and uniform mixing, adopts
With ultrasonic washing unit ultrasonic cleaning 15min, standing 10～12 h, adding concentration is 6mmol L-1Zinc nitrate hexahydrate Zn
(N03)2·6H20 and ferric chloride (FeCl36H2O) (FeCl that concentration is 4mmol3·6H2O), it is sufficiently stirred for, to mixed solution and dripping
Concentration is 0.10 mol L-1NaOH, regulation pH value be 7～8, stir 15min；Again by mixed liquor under 3500r/min rotating speed
Be centrifuged, be washed out, be dried, then with the cetyl trimethylammonium bromide of 0.lg, the distilled water of 30mL, 15mL anhydrous
Ethanol mixes, and puts in hydrothermal reaction kettle, heat 180～200 DEG C after mixing, hydro-thermal reaction 24h, by distilled water and nothing after reaction
The washing of water-ethanol alternating centrifugal, decompression sucking filtration, be again heated at 350 DEG C be dried 2h, ground, cross 200 mesh sieves, prepares load multiple
Close the magnetic attapulgite clay of photocatalyst.
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| CN201610536347.7A CN106179521A (en) | 2016-07-10 | 2016-07-10 | A kind of preparation method of the magnetic attapulgite clay of loaded composite photocatalysis agent |
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Cited By (5)
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| CN106799201A (en) * | 2017-01-24 | 2017-06-06 | 西安理工大学 | A kind of preparation method of AlCe composite axis systems |
| CN107787966A (en) * | 2017-11-18 | 2018-03-13 | 明光市海港凹坭矿业有限公司 | A kind of preparation method of attapulgite clay particle for farm chemical carrier |
| CN108525640A (en) * | 2017-03-03 | 2018-09-14 | 沈金池 | A kind of modified technique improving attapulgite absorption property |
| CN116037210A (en) * | 2022-12-26 | 2023-05-02 | 安徽世倾环保科技有限公司 | Preparation method and application of attapulgite-based composite material loaded with cobalt oxime complex photocatalyst |
| CN116216931A (en) * | 2023-03-30 | 2023-06-06 | 中国科学院南京地理与湖泊研究所 | Preparation method and application of denitrification solid slow-release carbon source |
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