CN107555490A - A kind of quick method for preparing chlorion intercalation cobalt aluminium houghite - Google Patents
A kind of quick method for preparing chlorion intercalation cobalt aluminium houghite Download PDFInfo
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Abstract
The invention discloses a kind of quick method for preparing chlorion intercalation cobalt aluminium houghite.The present invention uses acetic acid sodium acetate buffer, the pH stable of preparation system is controlled 4.00~5.00, using cobalt chloride hexahydrate, Aluminium chloride hexahydrate as raw material, using sodium hydroxide as precipitating reagent, using deionized water as solvent, detergent, formulated solution, titration co-precipitation, hydro-thermal process, washing, suction filtration, drying steps, are made chlorion intercalation cobalt aluminium houghite.This preparation method can effectively avoid CO in environment2Dissolve and form CO3 2‑The influence of ion, it is the fast preparation method of pure phase chlorion intercalation cobalt aluminium houghite.
Description
Technical field
The invention belongs to novel inorganic stratified material field, and in particular to one kind is quickly had based on control synthetic system pH
The method that effect prepares chlorion intercalation cobalt aluminium houghite.
Background technology
Houghite（Layered Double Hydroxides, abbreviation LDHs）For layered double hydroxide, have
Layered crystal structure, it is made up of the hydroxide of divalence and trivalent metallic element, anion should be filled between structure sheaf.Co-precipitation
Main preparation methods of the method as LDHs, because its preparation process is generally carried out under the system of opening wide, the CO of environmental system2Often can not
Ground pass into solution system can be avoided to be converted into the stronger carbonate of laminate adhesion and preferentially enter hydrotalcite-like compound interlayer, therefore
And carbonic acid intercalation hydrotalcite-like is generally preferentially prepared in traditional co-precipitation method；And effective system of chlorion intercalation houghite
It is standby then generally require to exchange carbonic acid intercalation hydrotalcite-like by chlorion and realize.
Although largely there is new main body, the hydrotalcite-like materials of the Nomenclature Composition and Structure of Complexes constantly to be synthesized and studied, surround
The research enthusiasm of classical member's cobalt aluminium houghite but never disappears, as cobalt aluminium houghite is in fields such as catalysis, absorption
Deeply, the regulation and control design of different anions intercalation cobalt aluminium hydrotalcite-like materials increasingly receives the favor of researcher for research.Chlorine
Ion insertion cobalt aluminium houghite（It is designated as CoAl-Cl-LDH）Due to acceptant object anion, can often be used as from
Sub- exchange adsorbing substance, its excellent ion-exchange performance can not only compare anion exchange resin, and possess and handed over than anion
The bigger ion exchange capacity of resin is changed, the excellent characteristics such as its high temperature resistant, radiation hardness, not aging, the big, small volume of density make in addition
It has a wide range of applications in printing and dyeing, papermaking, plating and nuclear waste water processing etc..With the application field research not
It is disconnected to go deep into, prepare the tradition side that cumbersome and inefficient interlayer anion exchange process prepares chlorion intercalation cobalt aluminium houghite
Method has obviously been unable to meet demand.On the basis of cobalt aluminium houghite application of function is paid close attention to, traditional co-precipitation method synthesis is focused on
The deficiency of chlorion intercalation cobalt aluminium houghite, exploitation is a kind of to be met actual rapid and effective method and prepares chlorion intercalation cobalt aluminium
Houghite is significant.
The content of the invention
The problem of can not efficiently preparing chlorion intercalation cobalt aluminium houghite for traditional co-precipitation method, the present invention is based on altogether
The precipitation method provide a kind of fast and effective method for preparing chlorion intercalation cobalt aluminium houghite；Concrete principle be using acetic acid-
The cushioning effect of sodium acetate buffer, by the control of the pH stable of preparation system 4.00~5.00, effectively avoiding environment
Middle CO2An efficient step prepares CoAl-Cl-LDH on the basis of dissolving the influence to prepared product.
The invention provides a kind of quick method for preparing chlorion intercalation cobalt aluminium houghite, with cobalt chloride hexahydrate,
Aluminium chloride hexahydrate is raw material, using sodium hydroxide as precipitating reagent, deionized water as solvent, formulated solution, titration co-precipitation,
Hydro-thermal process, washing, suction filtration, drying steps, chlorion intercalation cobalt aluminium houghite is made.
Specifically comprise the following steps：
（1）Prepare NaAc_HAc buffer solution, pH=4.00~5.00 of cushioning liquid
Sodium acetate solution and acetum are mixed, the substance withdrawl syndrome for controlling sodium acetate is 0.036~0.140 mol L-1, the substance withdrawl syndrome of acetic acid is 0.060~0.164 mol L-1, it is made into NaAc_HAc buffer solution；
（2）Prepare mixing salt solution
Cobalt chloride hexahydrate and Aluminium chloride hexahydrate are weighed into beaker, deionized water is added in beaker, and use magnetic agitation
Device stirs 5~15 min and is allowed to be completely dissolved, and the solution prepared is transferred to stand-by in hanging bottle type transfusion device；
（3）Prepare sodium hydrate aqueous solution
Sodium hydrate solid is weighed, it is 1.00 mol L to be configured to concentration-1Sodium hydrate aqueous solution, transfer them to
It is stand-by in hanging bottle type transfusion device；
（4）Prepare chlorion intercalation cobalt aluminium houghite
The NaAc_HAc buffer solution prepared is placed in reactor, reactor is placed in 30~60 DEG C of thermostat water baths
In, and be stirred continuously；The mixing salt solution of preparation and sodium hydrate aqueous solution are instilled into the above-mentioned reactor equipped with cushioning liquid
In, and consolidate system pH in whole course of reaction with the pH value during the real-time monitoring titration of acidometer, control rate of titration
It is fixed；Continue the min of stirring 20~30 after dripping, obtained precipitation and mother liquor sealing are then placed in polytetrafluoroethyllining lining
In stainless steel cauldron, 3~48 h are heated in 90~150 DEG C of baking ovens；
（5）Filter
After reacted turbid solution is cooled into room temperature, it is placed in the Buchner funnel on bottle,suction top and filters, retained on filter paper
Product cake, solution are evacuated in filter flask；
（6）Deionized water washing, filter
Product cake is placed in beaker, adds the mL of deionized water 100~200, the min of agitator treating 5~10, then will washing
Liquid is placed in Buchner funnel and filtered again, and remaining product filter cake on filter paper, solution is evacuated in filter flask；Deionized water washing, filter
Repeat, until filtrate is in neutrality；
（7）Dry
Washing, filtered product are placed in surface plate, is together put into 80~100 DEG C of baking oven and is dried, when drying
Between be 12~24 h；Chlorion intercalation cobalt aluminium houghite is made.
In the above method, the step（2）In, willc(Co2+): c(Al3+) control 2:1~4:1.Whereinc(Co2+) be
Refer to cobalt chloride substance withdrawl syndrome in mixing salt solution,c(Al3+) refer to aluminium chloride substance withdrawl syndrome in mixing salt solution.
In the above method, the step（2）In, the substance withdrawl syndrome of aluminium chloride in mixing salt solution is controlled 0.10
~1.00 mol L-1。
In the above method, the step（3）In, sodium hydrate aqueous solution substance withdrawl syndrome is 1.00 mol L-1。
In the above method, step（4）In, system pH control is 4.00~5.00 in course of reaction.
When product of the present invention is further applied, grinding, the process of sieving need to be passed through：Dried crystalline product particle is existed
Grind in mortar, then sieved with 100 eye mesh screens, screen into the product of crystal fine powder.
The present invention has carried out phenetic analysis by x-ray diffractometer to the crystal structure for preparing product.
Beneficial effects of the present invention：
（1）The present invention utilizes the cushioning effect of NaAc_HAc buffer solution, and the pH stable of preparation system is controlled 4.00
~5.00, the preparation system can effectively avoid CO in environment2Dissolve and form CO3 2-The influence of ion, it is a kind of simple and quick
Prepare the effective ways of pure phase chlorion intercalation cobalt aluminium houghite；
（2）Due to Cl-Different from CO3 2-Radius and its acid-base property, Cl-Instead of CO3 2-Into cobalt aluminium houghite interlayer, it will
Inner layer space and soda acid performance that chlorion intercalation cobalt aluminium houghite is different from carbonate intercalation cobalt aluminium houghite are assigned, this
The change of a little performances can influence its catalytic applications to a certain extent；
（3）Due to Cl-It is weaker than CO3 2-With the adhesion of laminate, chlorion intercalation cobalt aluminium houghite generally has more preferable ion
Switching performance, its fast and effective preparation will further speed up cobalt aluminium hydrotalcite-like materials at printing and dyeing, papermaking, plating and nuclear waste water
The application of reason etc..
Brief description of the drawings
Fig. 1 is that different cobalt aluminum ratios are in different pH environmental systems in embodiment 1 ~ 3, the X-ray diffraction intensity collection of illustrative plates of sample
（XRD）, it is followed successively by A：c(Co2+): c(Al3+)=2:1, pH=3.99；B：c(Co2+): c(Al3+)=3:1, pH=4.63；C：c
(Co2+): c(Al3+)=4:1, pH=4.95.A, B, C correspond to embodiment 1 ~ 3 respectively.
Fig. 2 is in embodiment 4 and 5c(Co2+): c(Al3+) =2:1 in different pH environmental systems the X ray of sample spread out
Penetrate intensity collection of illustrative plates（XRD）, it is followed successively by D：pH=4.77；E：pH=4.25.DE corresponds to embodiment 4 and 5 respectively.
Embodiment
The present invention is further illustrated below by embodiment, but is not limited to following examples.
Embodiment 1：
（1）The mol L of 18.00 ± 0.01 mL 0.2 are pipetted with pipette-1Sodium acetate solution into 100 mL volumetric flasks, then
The mol L of 82.00 ± 0.01 mL 0.2 are added thereto-1Acetum, shaking by swirling is allowed to well mixed, and constant volume is made into 100 mL
The NaAc_HAc buffer solution of pH=4.00 ± 0.01.
（2）The g of cobalt chloride hexahydrate 8.57 ± 0.01 is weighed, the g of Aluminium chloride hexahydrate 4.35 ± 0.01, is mixed addition
In beaker, 90 ± 1 mL deionized waters are added in beaker, and are allowed to be completely dissolved with the min of magnetic stirrer 10, will be matched somebody with somebody
The solution made（c (Co2+)=0.40 mol▪L-1, c (Al3+)=0.20 mol▪L-1）It is transferred to 250 mL hanging bottle type transfusion devices
In it is stand-by.
（3）Weigh the g of sodium hydroxide 4.00 ± 0.01 to be placed in beaker, a small amount of deionized water is added in beaker, and use magnetic
Power agitator stirs 10 min and is allowed to be completely dissolved.The solution dissolved is transferred in 100 mL volumetric flasks, is made into 1.00
mol▪L-1Sodium hydrate aqueous solution, then transfer them to stand-by in 250 mL hanging bottle type transfusion devices.
（4）The NaAc_HAc buffer solution for taking 90 ± 1 mL to prepare（pH=4.00±0.01）In 500 mL beakers
In, and beaker is placed in 60 DEG C of thermostat water baths.In the case where being constantly stirred vigorously, by above-mentioned mixing salt solution and hydroxide
Sodium water solution（1.00 mol▪L-1）Instill simultaneously in the beaker equipped with cushioning liquid, and with the real-time monitoring titration process of acidometer
In pH value, the pH value of system is maintained at 3.99 in whole course of reaction.Continue to stir 30 min after dripping, will then obtain
Precipitation and mother liquor sealing be placed in the stainless steel cauldron of polytetrafluoroethyllining lining, the hydro-thermal process in 100 ± 2 DEG C of baking ovens
15 h。
（5）After question response kettle natural cooling, reacted solution is filtered to obtain sediment, repeatedly uses deionized water
After washing to neutrality, 85 ± 2 DEG C of 12 h of drying in baking oven are put into.Sieved after taking-up through grinding, produce into the production of crystal fine powder
Thing.
（6）X-ray diffraction analysis are carried out to preparing crystal fines product, its diffraction spectrogram is as shown in Figure 1.Show in spectrogram
The distinctive diffraction maximum of CoAl-Cl-LDH compounds is shown, crystalline phase is single, and crystallinity is higher.
Embodiment 2：
（1）The mol L of 49.00 ± 0.01 mL 0.2 are pipetted with pipette-1Sodium acetate solution into 100 mL volumetric flasks, then
51.00 ± 0.01 mL 0.2mol L are added thereto-1Acetum, shaking by swirling is allowed to well mixed, and constant volume is made into 100 mL
The NaAc_HAc buffer solution of pH=4.60 ± 0.01.
（2）The g of cobalt chloride hexahydrate 21.41 ± 0.01, the g of Aluminium chloride hexahydrate 7.24 ± 0.01 are weighed, is mixed and adds
Enter in beaker, 100 ± 1 mL deionized waters added in beaker, and be allowed to be completely dissolved with the min of magnetic stirrer 10,
The solution that will be prepared（c (Co2+)=0.90 mol▪L-1, c (Al3+)=0.30 mol▪L-1）It is defeated to be transferred to 250 mL hanging bottle types
It is stand-by in liquid device.
（3）Weigh the g of sodium hydroxide 4.00 ± 0.01 to be placed in beaker, a small amount of deionized water is added in beaker, and use magnetic
Power agitator stirs 10 min and is allowed to be completely dissolved.The solution dissolved is transferred in 100 mL volumetric flasks, is made into 1.00
mol▪L-1Sodium hydrate aqueous solution, then transfer them to stand-by in 250 mL hanging bottle type transfusion devices.
（4）The NaAc_HAc buffer solution for taking 60 ± 1 mL to prepare（pH=4.60±0.01）In 500 mL beakers
In, and beaker is placed in 30 DEG C of thermostat water baths.In the case where being constantly stirred vigorously, by above-mentioned mixing salt solution and hydroxide
Sodium water solution（1.00 mol▪L-1）Instill simultaneously in the beaker equipped with cushioning liquid, and with the real-time monitoring titration process of acidometer
In pH value, in whole course of reaction, the pH value of system is maintained at 4.63, continues to stir 25 min after dripping, then will
To precipitation and mother liquor sealing be placed in the stainless steel cauldron of polytetrafluoroethyllining lining, in 120 ± 2 DEG C of baking ovens at hydro-thermal
Manage 15 h.
（5）After question response kettle natural cooling, reacted solution is filtered to obtain sediment, repeatedly uses deionized water
After washing to neutrality, 83 ± 2 DEG C of 24 h of drying in baking oven are put into.Sieved after taking-up through grinding, produce into the production of crystal fine powder
Thing.
（6）X-ray diffraction analysis are carried out to preparing crystal fines product, its diffraction spectrogram is as shown in Figure 1.Show in spectrogram
The distinctive diffraction maximum of CoAl-Cl-LDH compounds is shown, crystalline phase is single, and crystallinity is higher.
Embodiment 3：
（1）The mol L of 70.00 ± 0.01 mL 0.2 are pipetted with pipette-1Sodium acetate solution into 100 mL volumetric flasks, then
The mol L of 30.00 ± 0.01 mL 0.2 are added thereto-1Acetum, shaking by swirling is allowed to well mixed, and constant volume is made into 100 mL
The NaAc_HAc buffer solution of pH=5.00 ± 0.01.
（2）The g of cobalt chloride hexahydrate 28.55 ± 0.01, the g of Aluminium chloride hexahydrate 7.24 ± 0.01 are weighed, is mixed and adds
Enter in beaker, 120 ± 5 mL deionized waters added in beaker, and be allowed to be completely dissolved with the min of magnetic stirrer 10,
The solution that will be prepared（c (Co2+)=1.00 mol▪L-1, c (Al3+)=0.25 mol▪L-1）It is defeated to be transferred to 250 mL hanging bottle types
It is stand-by in liquid device.
（3）Weigh the g of sodium hydroxide 4.00 ± 0.01 to be placed in beaker, a small amount of deionized water is added in beaker, is used in combination
The min of magnetic stirrer 10 is allowed to be completely dissolved.The solution dissolved is transferred in 100 mL volumetric flasks, is made into 1.00
mol▪L-1Sodium hydrate aqueous solution, then transfer them to stand-by in 250 mL hanging bottle type transfusion devices.
（4）The NaAc_HAc buffer solution for taking 90 ± 1 mL to prepare（pH=5.00±0.01）In 500 mL beakers
In, and beaker is placed in 50 DEG C of thermostat water baths.In the case where being constantly stirred vigorously, by above-mentioned mixing salt solution and hydroxide
Sodium water solution（1.00 mol▪L-1）Instill simultaneously in the beaker equipped with cushioning liquid, and with the real-time monitoring titration process of acidometer
In pH value, the pH value of system is maintained at 4.95 in whole course of reaction.Continue to stir 30 min after dripping, will then obtain
Precipitation and mother liquor sealing be placed in the stainless steel cauldron of polytetrafluoroethyllining lining, the hydro-thermal process in 120 ± 2 DEG C of baking ovens
15 h。
（5）After question response kettle natural cooling, reacted solution is filtered to obtain sediment, repeatedly uses deionized water
After washing to neutrality, 88 ± 2 DEG C of 24 h of drying in baking oven are put into.Sieved after taking-up through grinding, produce into the production of crystal fine powder
Thing.
（6）X-ray diffraction analysis are carried out to the powdery product of the present invention, its diffraction spectrogram is as shown in Figure 1.In spectrogram
The distinctive diffraction maximum of CoAl-Cl-LDH compounds is shown, crystalline phase is single, and crystallinity is higher.
Embodiment 4：
（1）The mol L of 59.00 ± 0.01 mL 0.2 are pipetted with pipette-1Sodium acetate solution into 100 mL volumetric flasks, then
The mol L of 41.00 ± 0.01 mL 0.2 are added thereto-1Acetum, shaking by swirling is allowed to well mixed, and constant volume is made into 100 mL
The NaAc_HAc buffer solution of pH=4.80 ± 0.01.
（2）The g of cobalt chloride hexahydrate 23.79 ± 0.01, the g of Aluminium chloride hexahydrate 12.07 ± 0.01 are weighed, is mixed and adds
Enter in beaker, 100 ± 1 mL deionized waters added in beaker, and be allowed to be completely dissolved with the min of magnetic stirrer 10,
The solution that will be prepared（c (Co2+)=1.00 mol▪L-1, c (Al3+)=0.50 mol▪L-1）It is defeated to be transferred to 250 mL hanging bottle types
It is stand-by in liquid device.
（3）Weigh the g of sodium hydroxide 4.00 ± 0.01 to be placed in beaker, a small amount of deionized water is added in beaker, and use magnetic
Power agitator stirs 10 min and is allowed to be completely dissolved.The solution dissolved is transferred in 100 mL volumetric flasks, is made into 1.00
mol▪L-1Sodium hydrate aqueous solution, then transfer them to stand-by in 250 mL hanging bottle type transfusion devices.
（4）Take acetic acid-sodium acetate buffer that 100 ± 1 mL are prepared（pH=4.80±0.01）In 500 mL beakers
In, and beaker is placed in 40 DEG C of thermostat water baths.In the case where being constantly stirred vigorously, by above-mentioned mixing salt solution and hydroxide
Sodium water solution（1.00 mol▪L-1）Instill simultaneously in the beaker equipped with cushioning liquid, and with the real-time monitoring titration process of acidometer
In pH value, in whole course of reaction, the pH value of system is maintained at 4.77.Continue to stir 30 min after dripping, then incite somebody to action
To precipitation and mother liquor sealing be placed in the stainless steel cauldron of polytetrafluoroethyllining lining, in 140 ± 2 DEG C of baking ovens at hydro-thermal
Manage 12 h.
（5）After question response kettle natural cooling, reacted solution is filtered to obtain sediment, repeatedly uses deionized water
After washing to neutrality, 90 ± 2 DEG C of 12 h of drying in baking oven are put into.Sieved after taking-up through grinding, produce into the production of crystal fine powder
Thing.
（6）X-ray diffraction analysis are carried out to the powdery product of the present invention, its diffraction spectrogram is as shown in Figure 2.In spectrogram
The distinctive diffraction maximum of CoAl-Cl-LDH compounds is shown, crystalline phase is single, and crystallinity is higher.
Embodiment 5：
（1）The mol L of 26.50 ± 0.01 mL 0.2 are pipetted with pipette-1Sodium acetate solution into 100 mL volumetric flasks, then
The mol L of 73.50 ± 0.01 mL 0.2 are added thereto-1Acetum, shaking by swirling is allowed to well mixed, and constant volume is made into 100 mL
The NaAc_HAc buffer solution of pH=4.20 ± 0.01.
（2）The g of cobalt chloride hexahydrate 28.55 ± 0.01, the g of Aluminium chloride hexahydrate 14.49 ± 0.01 are weighed, is mixed and adds
Enter in beaker, 100 ± 1 mL deionized waters added in beaker, and be allowed to be completely dissolved with the min of magnetic stirrer 10,
The solution that will be prepared（c (Co2+)=1.20 mol▪L-1, c (Al3+)=0.60 mol▪L-1）It is defeated to be transferred to 250 mL hanging bottle types
It is stand-by in liquid device.
（3）Weigh the g of sodium hydroxide 4.00 ± 0.01 to be placed in beaker, a small amount of deionized water is added in beaker, is used in combination
The min of magnetic stirrer 10 is allowed to be completely dissolved.The solution dissolved is transferred in 100 mL volumetric flasks, is made into 1.00
mol▪L-1Sodium hydrate aqueous solution, then transfer them to stand-by in 250 mL hanging bottle type transfusion devices.
（4）The NaAc_HAc buffer solution for taking 100 ± 1 mL to prepare（pH=4.20±0.01）In 500 mL beakers
In, and beaker is placed in 60 DEG C of thermostat water baths.In the case where being constantly stirred vigorously, by above-mentioned mixing salt solution and hydroxide
Sodium water solution（1.00 mol▪L-1）Instill simultaneously in the beaker equipped with cushioning liquid, and with the real-time monitoring titration process of acidometer
In pH value, in whole course of reaction, the pH value of system is maintained at 4.25.Continue to stir 20 min after dripping, then incite somebody to action
To precipitation and mother liquor sealing be placed in the stainless steel cauldron of polytetrafluoroethyllining lining, in 110 ± 2 DEG C of baking ovens at hydro-thermal
Manage 12 h.
（5）After question response kettle natural cooling, reacted solution is filtered to obtain sediment, repeatedly uses deionized water
After washing to neutrality, 95 ± 2 DEG C of 12 h of drying in baking oven are put into, is sieved after taking-up through grinding, produces into the production of crystal fine powder
Thing.
（6）X-ray diffraction analysis are carried out to the powdery product of the present invention, its diffraction spectrogram is as shown in Figure 2.In spectrogram
The distinctive diffraction maximum of CoAl-Cl-LDH compounds is shown, crystalline phase is single, and crystallinity is higher.
Claims (5)
- A kind of 1. quick method for preparing chlorion intercalation cobalt aluminium houghite, it is characterised in that：With Aluminium chloride hexahydrate and six Hydrated cobalt chloride is raw material, and using sodium hydroxide as precipitating reagent, deionized water is as solvent, formulated solution, titration co-precipitation, water Heat treatment, washing, filter, drying steps, chlorion intercalation cobalt aluminium houghite is made.
- A kind of 2. quick method for preparing chlorion intercalation cobalt aluminium houghite according to claim 1, it is characterised in that： Comprise the following steps：（1）Prepare NaAc_HAc buffer solution, pH=4.00~5.00 of cushioning liquidSodium acetate solution and acetum are mixed, it is 0.036~0.140 mol L to control sodium acetate substance withdrawl syndrome-1, vinegar The amount concentration of acid substance is 0.060~0.164 mol L-1, it is made into NaAc_HAc buffer solution；（2）Prepare mixing salt solutionCobalt chloride hexahydrate and Aluminium chloride hexahydrate are weighed into beaker, deionized water is added in beaker, and use magnetic agitation Device stirs 5~15 min and is allowed to be completely dissolved, and the solution prepared is transferred to stand-by in hanging bottle type transfusion device；（3）Prepare sodium hydrate aqueous solutionSodium hydrate solid is weighed, it is 1.00 mol L to be configured to concentration-1Sodium hydrate aqueous solution, transfer them to and hang It is stand-by in bottle type infusion device；（4）Prepare chlorion intercalation cobalt aluminium houghiteThe NaAc_HAc buffer solution prepared is placed in reactor, reactor is placed in 30~60 DEG C of thermostat water baths In, and be stirred continuously；The sodium hydrate aqueous solution of preparation and mixing salt solution are instilled into the above-mentioned reactor equipped with cushioning liquid In, and consolidate system pH in whole course of reaction with the pH value during the real-time monitoring titration of acidometer, control rate of titration It is fixed；Continue the min of stirring 20~30 after dripping, obtained precipitation and mother liquor sealing are then placed in polytetrafluoroethyllining lining In stainless steel cauldron, 3~48 h are heated in 90~150 DEG C of baking ovens；（5）FilterAfter reacted turbid solution is cooled into room temperature, it is placed in the Buchner funnel on bottle,suction top and filters, retained on filter paper Product cake, solution are evacuated in filter flask；（6）Deionized water washing, filterProduct cake is placed in beaker, adds the mL of deionized water 100~200, the min of agitator treating 5~10, then will washing Liquid is placed in Buchner funnel and filtered again, and remaining product filter cake on filter paper, solution is evacuated in filter flask；Deionized water washing, filter Repeat, until filtrate is in neutrality；（7）DryWashing, filtered product are placed in surface plate, is together put into 80~100 DEG C of baking oven and is dried, when drying Between be 12~24 h, chlorion intercalation cobalt aluminium houghite is made.
- A kind of 3. quick method for preparing chlorion intercalation cobalt aluminium houghite according to claim 2, it is characterised in that： The step（2）In, willc(Co2+): c(Al3+) control 2:1~4:1, whereinc(Co2+) refer to chlorination in mixing salt solution Cobalt substance withdrawl syndrome,c(Al3+) refer to aluminium chloride substance withdrawl syndrome in mixing salt solution.
- A kind of 4. quick method for preparing chlorion intercalation cobalt aluminium houghite according to claim 2, it is characterised in that： The step（2）In, the substance withdrawl syndrome of aluminium chloride is 0.10~1.00 mol L in mixing salt solution-1。
- A kind of 5. quick method for preparing chlorion intercalation cobalt aluminium houghite according to claim 2, it is characterised in that： Step（4）In, system pH control is 4.00~5.00 in course of reaction.
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| CN109502656A (en) * | 2018-11-29 | 2019-03-22 | 兰州金通储能动力新材料有限公司 | A kind of spherical Co (II) Co (III) hydrotalcite-like materials and preparation method thereof |
| CN115140779A (en) * | 2022-05-05 | 2022-10-04 | 中南大学 | Hexagonal chlorine intercalation cobalt-aluminum hydrotalcite-like defluorination material and preparation and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109502656A (en) * | 2018-11-29 | 2019-03-22 | 兰州金通储能动力新材料有限公司 | A kind of spherical Co (II) Co (III) hydrotalcite-like materials and preparation method thereof |
| CN115140779A (en) * | 2022-05-05 | 2022-10-04 | 中南大学 | Hexagonal chlorine intercalation cobalt-aluminum hydrotalcite-like defluorination material and preparation and application thereof |
| CN115140779B (en) * | 2022-05-05 | 2023-09-08 | 中南大学 | Hexagonal chlorine intercalation cobalt-aluminum hydrotalcite defluorination material and preparation and application thereof |
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