CN107555490B - A method of quickly preparing chloride ion intercalation cobalt aluminium houghite - Google Patents
A method of quickly preparing chloride ion intercalation cobalt aluminium houghite Download PDFInfo
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Abstract
The invention discloses a kind of methods for quickly preparing chloride ion intercalation cobalt aluminium houghite.The present invention uses NaAc_HAc buffer solution, 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 chloride ion intercalation cobalt aluminium houghite.This preparation method can effectively avoid CO in environment2It dissolves and forms CO3 2‑The influence of ion is the fast preparation method of pure phase chloride ion intercalation cobalt aluminium houghite.
Description
Technical field
The invention belongs to novel inorganic stratified material fields, and in particular to one kind is quickly had based on control synthetic system pH
The method that effect prepares chloride ion intercalation cobalt aluminium houghite.
Background technique
Houghite (Layered Double Hydroxides, abbreviation LDHs) is layered double hydroxide, is had
Layered crystal structure is made of the hydroxide of divalent and trivalent metallic element, and anion should be filled between structure sheaf.Co-precipitation
Main preparation methods of the method as LDHs, because its preparation process usually carries out under the system of opening wide, the CO of environmental system2Often can not
It can avoid ground pass into solution system to be converted into the stronger carbonate of laminate binding force and preferentially enter hydrotalcite-like compound interlayer, therefore
And carbonic acid intercalation hydrotalcite-like is usually preferentially prepared in traditional co-precipitation method；And effective system of chloride ion intercalation houghite
It is standby then generally require by chloride ion exchange carbonic acid intercalation hydrotalcite-like realize.
Although the hydrotalcite-like materials largely with new main body, the Nomenclature Composition and Structure of Complexes are constantly synthesized and studied, surround
The research enthusiasm of classical member's cobalt aluminium houghite but never subsides, as cobalt aluminium houghite is in fields such as catalysis, absorption
Deeply, the regulation design of different anions intercalation cobalt aluminium hydrotalcite-like materials increasingly receives the favor of researcher for research.Chlorine
Ion insertion cobalt aluminium houghite (being denoted as CoAl-Cl-LDH) due to acceptant object anion, can often be used as from
Sub- exchange adsorbing substance, excellent ion-exchange performance can not only compare anion exchange resin, and possess and hand over than anion
The bigger ion exchange capacity of resin is changed, its high temperature resistant, radiation hardness, not aging, density is big in addition, the excellent characteristics such as small in size make
It has a wide range of applications in terms of printing and dyeing, papermaking, plating and nuclear waste water.Not with the application field research
It is disconnected to go deep into, prepare the tradition side that cumbersome and inefficient interlayer anion exchange process prepares chloride ion intercalation cobalt aluminium houghite
Method is obviously no longer satisfied demand.On the basis of paying close attention to cobalt aluminium houghite functional application, traditional co-precipitation method synthesis is focused
The deficiency of chloride ion intercalation cobalt aluminium houghite, develops one kind and meets actual rapid and effective method and prepare chloride ion intercalation cobalt aluminium
Houghite is significant.
Summary of the invention
Aiming at the problem that traditional co-precipitation method cannot efficiently prepare chloride ion intercalation cobalt aluminium houghite, the present invention is based on altogether
The precipitation method provide a kind of method for quickly and effectively preparing chloride ion intercalation cobalt aluminium houghite；Concrete principle is to utilize acetic acid-
The buffer function of sodium acetate buffer is effectively avoiding environment by the pH stable control of preparation system 4.00~5.00
Middle CO2An efficient step prepares CoAl-Cl-LDH on the basis of dissolving the influence to prepared product.
The present invention provides a kind of method for quickly preparing chloride ion 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,
Chloride ion intercalation cobalt aluminium houghite is made in hydro-thermal process, washing, suction filtration, drying steps.
Specifically comprise the following steps:
(1) NaAc_HAc buffer solution, pH=4.00~5.00 of buffer solution are prepared
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) mixing salt solution is prepared
It weighs cobalt chloride hexahydrate and Aluminium chloride hexahydrate and deionized water is added in beaker into beaker, and use magnetic force
Blender stirs 5~15 min and is allowed to be completely dissolved, and prepared solution is transferred in hanging bottle type infusion apparatus for use；
(3) sodium hydrate aqueous solution is prepared
Sodium hydrate solid is weighed, being configured to concentration is 1.00 mol L-1Sodium hydrate aqueous solution, shifted
It is stand-by into hanging bottle type infusion apparatus；
(4) chloride ion intercalation cobalt aluminium houghite is prepared
Prepared NaAc_HAc buffer solution is placed in reactor, reactor is placed in 30~60 DEG C of thermostatted waters
In bath, and it is stirred continuously；The mixing salt solution of preparation and sodium hydrate aqueous solution are instilled above-mentioned anti-equipped with buffer solution
It answers in device, and with the pH value in acidometer real-time monitoring titration process, controlling rate of titration makes system pH in entire reaction process
Value is fixed；Continue 20~30 min of stirring after dripping, then obtained precipitating and mother liquor sealing are placed in polytetrafluoroethylene (PTFE)
In the stainless steel cauldron of lining, 3~48 h are heated in 90~150 DEG C of baking ovens；
(5) it filters
After turbid solution after reaction is cooled to room temperature, it is placed in the Buchner funnel on bottle,suction top and filters, on filter paper
Remaining product filter cake, solution are evacuated in filter flask；
(6) deionized water washing, suction filtration
Product cake is placed in a beaker, 100~200 mL of deionized water, 5~10 min of agitator treating is added, then will
Cleaning solution is placed in Buchner funnel and filters again, and remaining product filter cake on filter paper, solution is evacuated in filter flask；Deionized water washing,
Suction filtration repeats, until filtrate is in neutrality；
(7) dry
Washing, filtered product are placed in surface plate, is put into 80~100 DEG C of baking oven and is dried together, is done
The dry time is 12~24 h；Chloride ion intercalation cobalt aluminium houghite is made.
It, will in the step (2) in the above methodc(Co2+): c(Al3+) control in 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, in the step (2), the substance withdrawl syndrome of aluminium chloride in mixing salt solution is controlled 0.10
~1.00 mol L-1。
In the above method, in the step (3), sodium hydrate aqueous solution substance withdrawl syndrome is 1.00 mol L-1。
In the above method, in step (4), system pH control is 4.00~5.00 in reaction process.
Product of the present invention is further in application, need to be by the process that is ground up, sieved: the crystalline product particle after drying is existed
It grinds in mortar, is then sieved with 100 mesh screens, screen the product at crystal fine powder.
The present invention has carried out phenetic analysis to the crystal structure for preparing product by x-ray diffractometer.
Beneficial effects of the present invention:
(1) present invention utilizes the buffer function of NaAc_HAc buffer solution, and the pH stable control of preparation system is existed
4.00~5.00, which can effectively avoid CO in environment2It dissolves and forms CO3 2-The influence of ion is a kind of simple
The quickly effective ways of preparation pure phase chloride ion 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,
Inner layer space and acid-base property that chloride ion intercalation cobalt aluminium houghite is different from carbonate intercalation cobalt aluminium houghite will be assigned
Can, the change of these performances will affect its catalytic applications to a certain extent；
(3) due to Cl-It is weaker than CO3 2-With the binding force of laminate, chloride ion intercalation cobalt aluminium houghite usually has preferably
Ion-exchange performance, quickly and effectively it is useless in printing and dyeing, papermaking, plating and core to will further speed up cobalt aluminium hydrotalcite-like materials for preparation
The application of water process etc..
Detailed description of the invention
Fig. 1 is that different cobalt aluminium ratios are in different pH environmental systems in embodiment 1 ~ 3, the X-ray diffraction intensity map 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 respectively correspond embodiment 1 ~ 3.
Fig. 2 is in embodiment 4 and 5c(Co2+): c(Al3+)=2:1 X-ray of sample in different pH environmental systems is spread out
Intensity map (XRD) is penetrated, D:pH=4.77 are followed successively by；E:pH=4.25.DE respectively corresponds embodiment 4 and 5.
Specific embodiment
The present invention is further illustrated below by embodiment, but is not limited to following embodiment.
Embodiment 1:
(1) 18.00 ± 0.01 mL, 0.2 mol L is pipetted with pipette-1Sodium acetate solution into 100 mL volumetric flasks,
82.00 ± 0.01 mL, 0.2 mol L is added thereto again-1Acetum, shaking by swirling is allowed to uniformly mixed, and constant volume is made into 100
The NaAc_HAc buffer solution of pH=4.00 ± 0.01 mL.
(2) 8.57 ± 0.01 g of cobalt chloride hexahydrate is weighed, 4.35 ± 0.01 g of Aluminium chloride hexahydrate is mixed addition
In beaker, 90 ± 1 mL deionized waters is added in beaker, and be allowed to be completely dissolved with 10 min of magnetic stirrer, will match
Make solution (c (Co2+)=0.40 mol▪L-1, c (Al3+)=0.20 mol▪L-1) it is transferred to 250 mL hanging bottle type infusion apparatuses
In it is stand-by.
(3) it weighs 4.00 ± 0.01 g of sodium hydroxide to be placed in a beaker, a small amount of deionized water is added in beaker, and use magnetic
Power blender 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 in 250 mL hanging bottle type infusion apparatuses stand-by.
(4) take the prepared NaAc_HAc buffer solution of 90 ± 1 mL (pH=4.00 ± 0.01) in 500 mL beakers
In, and place the beaker in 60 DEG C of thermostat water baths.In the case where being constantly vigorously stirred, by above-mentioned mixing salt solution and hydroxide
Sodium water solution (1.00 mol L-1) instill in the beaker equipped with buffer solution simultaneously, and with acidometer real-time monitoring titration process
In pH value, the pH value of system is maintained at 3.99 in entire reaction process.Continue to stir 30 min after dripping, will then obtain
Precipitating 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 reaction kettle natural cooling, the solution after reaction is filtered to obtain sediment, repeatedly uses deionized water
After washing to neutrality, it is put into 85 ± 2 DEG C of 12 h of drying in baking oven.Through being ground up, sieved to get at the production of crystal fine powder after taking-up
Object.
(6) to crystal fines product progress X-ray diffraction analysis is prepared, diffraction spectrogram is as shown in Fig. 1.It is shown in spectrogram
The distinctive diffraction maximum of CoAl-Cl-LDH compound is shown, crystal phase is single, and crystallinity is higher.
Embodiment 2:
(1) 49.00 ± 0.01 mL, 0.2 mol L is pipetted with pipette-1Sodium acetate solution into 100 mL volumetric flasks,
51.00 ± 0.01 mL 0.2mol L are added thereto again-1Acetum, shaking by swirling is allowed to uniformly mixed, and constant volume is made into 100
The NaAc_HAc buffer solution of pH=4.60 ± 0.01 mL.
(2) 21.41 ± 0.01 g of cobalt chloride hexahydrate, 7.24 ± 0.01 g of Aluminium chloride hexahydrate are weighed, is mixed and adds
Enter in beaker, 100 ± 1 mL deionized waters be added in beaker, and be allowed to be completely dissolved with 10 min of magnetic stirrer,
By prepared solution (c (Co2+)=0.90 mol▪L-1, c (Al3+)=0.30 mol▪L-1) to be transferred to 250 mL hanging bottle types defeated
It is stand-by in liquid device.
(3) it weighs 4.00 ± 0.01 g of sodium hydroxide to be placed in a beaker, a small amount of deionized water is added in beaker, and use magnetic
Power blender 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 in 250 mL hanging bottle type infusion apparatuses stand-by.
(4) take the prepared NaAc_HAc buffer solution of 60 ± 1 mL (pH=4.60 ± 0.01) in 500 mL beakers
In, and place the beaker in 30 DEG C of thermostat water baths.In the case where being constantly vigorously stirred, by above-mentioned mixing salt solution and hydroxide
Sodium water solution (1.00 mol L-1) instill in the beaker equipped with buffer solution simultaneously, and with acidometer real-time monitoring titration process
In pH value, in entire reaction process, the pH value of system is maintained at 4.63, continue to stir 25 min after dripping, then will
To precipitating and mother liquor sealing be placed in polytetrafluoroethyllining lining stainless steel cauldron in, in 120 ± 2 DEG C of baking ovens at hydro-thermal
Manage 15 h.
(5) after reaction kettle natural cooling, the solution after reaction is filtered to obtain sediment, repeatedly uses deionized water
After washing to neutrality, it is put into 83 ± 2 DEG C of 24 h of drying in baking oven.Through being ground up, sieved to get at the production of crystal fine powder after taking-up
Object.
(6) to crystal fines product progress X-ray diffraction analysis is prepared, diffraction spectrogram is as shown in Fig. 1.It is shown in spectrogram
The distinctive diffraction maximum of CoAl-Cl-LDH compound is shown, crystal phase is single, and crystallinity is higher.
Embodiment 3:
(1) 70.00 ± 0.01 mL, 0.2 mol L is pipetted with pipette-1Sodium acetate solution into 100 mL volumetric flasks,
30.00 ± 0.01 mL, 0.2 mol L is added thereto again-1Acetum, shaking by swirling is allowed to uniformly mixed, and constant volume is made into 100
The NaAc_HAc buffer solution of pH=5.00 ± 0.01 mL.
(2) 28.55 ± 0.01 g of cobalt chloride hexahydrate, 7.24 ± 0.01 g of Aluminium chloride hexahydrate are weighed, is mixed and adds
Enter in beaker, 120 ± 5 mL deionized waters be added in beaker, and be allowed to be completely dissolved with 10 min of magnetic stirrer,
By prepared solution (c (Co2+)=1.00 mol▪L-1, c (Al3+)=0.25 mol▪L-1) to be transferred to 250 mL hanging bottle types defeated
It is stand-by in liquid device.
(3) it weighs 4.00 ± 0.01 g of sodium hydroxide to be placed in a beaker, a small amount of deionized water is added in beaker, is used in combination
10 min of magnetic stirrer 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 in 250 mL hanging bottle type infusion apparatuses stand-by.
(4) take the prepared NaAc_HAc buffer solution of 90 ± 1 mL (pH=5.00 ± 0.01) in 500 mL beakers
In, and place the beaker in 50 DEG C of thermostat water baths.In the case where being constantly vigorously stirred, by above-mentioned mixing salt solution and hydroxide
Sodium water solution (1.00 mol L-1) instill in the beaker equipped with buffer solution simultaneously, and with acidometer real-time monitoring titration process
In pH value, the pH value of system is maintained at 4.95 in entire reaction process.Continue to stir 30 min after dripping, will then obtain
Precipitating 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 reaction kettle natural cooling, the solution after reaction is filtered to obtain sediment, repeatedly uses deionized water
After washing to neutrality, it is put into 88 ± 2 DEG C of 24 h of drying in baking oven.Through being ground up, sieved to get at the production of crystal fine powder after taking-up
Object.
(6) X-ray diffraction analysis is carried out to powdery product of the invention, diffraction spectrogram is as shown in Fig. 1.In spectrogram
Show the distinctive diffraction maximum of CoAl-Cl-LDH compound, crystal phase is single, and crystallinity is higher.
Embodiment 4:
(1) 59.00 ± 0.01 mL, 0.2 mol L is pipetted with pipette-1Sodium acetate solution into 100 mL volumetric flasks,
41.00 ± 0.01 mL, 0.2 mol L is added thereto again-1Acetum, shaking by swirling is allowed to uniformly mixed, and constant volume is made into 100
The NaAc_HAc buffer solution of pH=4.80 ± 0.01 mL.
(2) 23.79 ± 0.01 g of cobalt chloride hexahydrate, 12.07 ± 0.01 g of Aluminium chloride hexahydrate are weighed, is mixed and adds
Enter in beaker, 100 ± 1 mL deionized waters be added in beaker, and be allowed to be completely dissolved with 10 min of magnetic stirrer,
By prepared solution (c (Co2+)=1.00 mol▪L-1, c (Al3+)=0.50 mol▪L-1) to be transferred to 250 mL hanging bottle types defeated
It is stand-by in liquid device.
(3) it weighs 4.00 ± 0.01 g of sodium hydroxide to be placed in a beaker, a small amount of deionized water is added in beaker, and use magnetic
Power blender 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 in 250 mL hanging bottle type infusion apparatuses stand-by.
(4) take the prepared acetic acid-sodium acetate buffer (pH=4.80 ± 0.01) of 100 ± 1 mL in 500 mL beakers
In, and place the beaker in 40 DEG C of thermostat water baths.In the case where being constantly vigorously stirred, by above-mentioned mixing salt solution and hydroxide
Sodium water solution (1.00 mol L-1) instill in the beaker equipped with buffer solution simultaneously, and with acidometer real-time monitoring titration process
In pH value, in entire reaction process, the pH value of system is maintained at 4.77.Continue to stir 30 min after dripping, then incite somebody to action
To precipitating and mother liquor sealing be placed in polytetrafluoroethyllining lining stainless steel cauldron in, in 140 ± 2 DEG C of baking ovens at hydro-thermal
Manage 12 h.
(5) after reaction kettle natural cooling, the solution after reaction is filtered to obtain sediment, repeatedly uses deionized water
After washing to neutrality, it is put into 90 ± 2 DEG C of 12 h of drying in baking oven.Through being ground up, sieved to get at the production of crystal fine powder after taking-up
Object.
(6) X-ray diffraction analysis is carried out to powdery product of the invention, diffraction spectrogram is as shown in Fig. 2.In spectrogram
Show the distinctive diffraction maximum of CoAl-Cl-LDH compound, crystal phase is single, and crystallinity is higher.
Embodiment 5:
(1) 26.50 ± 0.01 mL, 0.2 mol L is pipetted with pipette-1Sodium acetate solution into 100 mL volumetric flasks,
73.50 ± 0.01 mL, 0.2 mol L is added thereto again-1Acetum, shaking by swirling is allowed to uniformly mixed, and constant volume is made into 100
The NaAc_HAc buffer solution of pH=4.20 ± 0.01 mL.
(2) 28.55 ± 0.01 g of cobalt chloride hexahydrate, 14.49 ± 0.01 g of Aluminium chloride hexahydrate are weighed, is mixed and adds
Enter in beaker, 100 ± 1 mL deionized waters be added in beaker, and be allowed to be completely dissolved with 10 min of magnetic stirrer,
By prepared solution (c (Co2+)=1.20 mol▪L-1, c (Al3+)=0.60 mol▪L-1) to be transferred to 250 mL hanging bottle types defeated
It is stand-by in liquid device.
(3) it weighs 4.00 ± 0.01 g of sodium hydroxide to be placed in a beaker, a small amount of deionized water is added in beaker, is used in combination
10 min of magnetic stirrer 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 in 250 mL hanging bottle type infusion apparatuses stand-by.
(4) take the prepared NaAc_HAc buffer solution of 100 ± 1 mL (pH=4.20 ± 0.01) in 500 mL beakers
In, and place the beaker in 60 DEG C of thermostat water baths.In the case where being constantly vigorously stirred, by above-mentioned mixing salt solution and hydroxide
Sodium water solution (1.00 mol L-1) instill in the beaker equipped with buffer solution simultaneously, and with acidometer real-time monitoring titration process
In pH value, in entire reaction process, the pH value of system is maintained at 4.25.Continue to stir 20 min after dripping, then incite somebody to action
To precipitating and mother liquor sealing be placed in polytetrafluoroethyllining lining stainless steel cauldron in, in 110 ± 2 DEG C of baking ovens at hydro-thermal
Manage 12 h.
(5) after reaction kettle natural cooling, the solution after reaction 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, through being ground up, sieved to get at the production of crystal fine powder after taking-up
Object.
(6) X-ray diffraction analysis is carried out to powdery product of the invention, diffraction spectrogram is as shown in Fig. 2.In spectrogram
Show the distinctive diffraction maximum of CoAl-Cl-LDH compound, crystal phase is single, and crystallinity is higher.
Claims (4)
1. a kind of method for quickly preparing chloride ion 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, filters, drying steps washing, and chloride ion intercalation cobalt aluminium houghite is made；Specifically comprise the following steps:
(1) NaAc_HAc buffer solution, pH=4.00~5.00 of buffer solution are prepared
Sodium acetate solution and acetum are mixed, control sodium acetate substance withdrawl syndrome is 0.036~0.140 mol L-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) mixing salt solution is prepared
It weighs cobalt chloride hexahydrate and Aluminium chloride hexahydrate and deionized water is added in beaker into beaker, and use magnetic agitation
Device stirs 5~15 min and is allowed to be completely dissolved, and prepared solution is transferred in hanging bottle type infusion apparatus for use；
(3) sodium hydrate aqueous solution is prepared
Sodium hydrate solid is weighed, being configured to concentration is 1.00 mol L-1Sodium hydrate aqueous solution, transfer them to and hang
It is stand-by in bottle type infusion device；
(4) chloride ion intercalation cobalt aluminium houghite is prepared
Prepared NaAc_HAc buffer solution 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 buffer solution
In, and with the pH value in acidometer real-time monitoring titration process, controlling rate of titration keeps system pH in entire reaction process solid
It is fixed；Continue 20~30 min of stirring after dripping, obtained precipitating 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) it filters
After turbid solution after reaction is cooled to 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, suction filtration
Product cake is placed in a beaker, 100~200 mL of deionized water, 5~10 min of agitator treating is added, it then will washing
Liquid is placed in Buchner funnel and filters again, and remaining product filter cake on filter paper, solution is evacuated in filter flask；Deionized water washing filters
Repeat, until filtrate is in neutrality；
(7) dry
Washing, filtered product are placed in surface plate, is put into 80~100 DEG C of baking oven and is dried together, when dry
Between be 12~24 h, be made chloride ion intercalation cobalt aluminium houghite.
2. a kind of method for quickly preparing chloride ion intercalation cobalt aluminium houghite according to claim 1, it is characterised in that:
It, will in the step (2)c(Co2+): c(Al3+) control in 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.
3. a kind of method for quickly preparing chloride ion intercalation cobalt aluminium houghite according to claim 1, it is characterised in that:
In the step (2), the substance withdrawl syndrome of aluminium chloride is 0.10~1.00 mol L in mixing salt solution-1。
4. a kind of method for quickly preparing chloride ion intercalation cobalt aluminium houghite according to claim 1, it is characterised in that:
In step (4), system pH control is 4.00~5.00 in reaction process.
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