CN107555465A - A kind of fast preparation method of nitrate anion intercalation copper aluminium houghite - Google Patents
A kind of fast preparation method of nitrate anion intercalation copper aluminium houghite Download PDFInfo
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- CN107555465A CN107555465A CN201710821939.8A CN201710821939A CN107555465A CN 107555465 A CN107555465 A CN 107555465A CN 201710821939 A CN201710821939 A CN 201710821939A CN 107555465 A CN107555465 A CN 107555465A
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Abstract
The invention discloses a kind of fast preparation method of nitrate anion intercalation copper aluminium houghite.The present invention uses acetic acid sodium acetate buffer, the pH stable of preparation system is controlled 4.00~5.00, using Gerhardite, ANN aluminium nitrate nonahydrate 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 nitrate anion intercalation copper aluminium houghite.This preparation method can effectively avoid CO in environment2Dissolve and form CO3 2‑The influence of ion, it is the effective ways of the quick preparation of pure phase nitrate anion intercalation copper 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 nitrate anion intercalation copper 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 nitric acid intercalation hydrotalcite-like
It is standby then generally require to exchange carbonic acid intercalation hydrotalcite-like by nitrate ion 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,
The research history of houghite compound is looked back, it can be found that copper aluminium houghite is as important a member in such material, it
Synthesis and application study always by extensive concern, as research of the copper aluminium houghite in fields such as catalysis, absorption is goed deep into, enclose
Regulation and control design around copper aluminium hydrotalcite-like materials still enjoys researcher to favor, in recent years, in order to preferably design copper aluminium class water
Talc materials, copper aluminium houghite need to often be peeled off；Carbonate intercalation copper aluminium houghite（It is designated as CuAl-CO3-LDH）
It is constrained because of the high forces between carbonate and laminate efficiently to peel off.Regulate and control to prepare easily peelable nitrate anion according to demand
Intercalation copper aluminium houghite（It is designated as CuAl-NO3-LDH）It is very necessary.And prepare cumbersome and inefficient through nitrate ion
The conventional method for exchanging carbanion and preparing nitrate anion intercalation copper aluminium houghite is obviously outdated.In concern copper
On the basis of aluminium houghite peels off assembling and application of function, exploitation meets actual straightforward procedure fast and effective to prepare nitrate anion
Intercalation copper aluminium houghite is significant.
The content of the invention
The problem of can not efficiently preparing nitrate anion intercalation copper aluminium houghite for traditional co-precipitation method, the present invention is based on altogether
The precipitation method, which provide, a kind of fast and effective prepares nitrate anion intercalation copper aluminium houghite method；Concrete principle is to utilize acetic acid-vinegar
The cushioning effect of sour sodium cushioning liquid, by the pH stability contortings of preparation system 4.00~5.00, in effective CO in avoiding environment2
Fast and effective preparation CuAl-NO on the basis of influence of the dissolving to prepared product3-LDH。
The invention provides a kind of fast preparation method of nitrate anion intercalation copper aluminium houghite, with Gerhardite,
ANN aluminium nitrate nonahydrate 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, nitrate anion intercalation copper 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 corresponding acetic acid is 0.060~0.164 mol L-1, it is made into NaAc_HAc buffer solution；
（2）Prepare mixing salt solution
Gerhardite and ANN aluminium nitrate nonahydrate 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 nitrate anion intercalation copper 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；Nitrate anion intercalation copper aluminium houghite is made.
In the above method, the step（2）In, willc(Cu2+): c(Al3+) control 2:1~4:1.Whereinc(Cu2+) be
Refer to copper nitrate substance withdrawl syndrome in mixing salt solution,c(Al3+) refer to aluminum nitrate substance withdrawl syndrome in mixing salt solution.
In the above method, the step（2）In, the substance withdrawl syndrome of aluminum nitrate 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, by the control of preparation system pH stable 4.00 ~
5.00, the preparation system can effectively avoid CO in environment2Dissolve and form CO3 2-The influence of ion, be it is simple and quick prepare it is pure
The effective ways of phase nitrate anion intercalation copper aluminium houghite；
（2）Due to NO3 -Different from CO3 2-Radius and its acid-base property, NO3 -Instead of CO3 2-, will into copper aluminium houghite interlayer
Inner layer space and soda acid performance that nitrate anion intercalation copper aluminium houghite is different from carbonate intercalation copper aluminium houghite can be assigned,
The change of these performances can influence its catalytic applications to a certain extent；
（3）Due to NO3 -It is weaker than CO3 2-With the adhesion of laminate, nitrate anion intercalation copper aluminium houghite generally has preferably stripping
From performance, it will be that effectively assembling provides safeguard using copper aluminium hydrotalcite-like materials.
Brief description of the drawings
Fig. 1 is the X ray diffracting spectrum that gained sample is prepared in embodiment 1 ~ 3（XRD）.Wherein A：c(Cu2+): c(Al3 +)=2:1, pH=4.81；B：c(Cu2+): c(Al3+)=3:1, pH=4.23；C：c(Cu2+): c (Al3+)=4:1, pH=4.44；A、
B, C corresponds to embodiment 1 ~ 3 respectively.
Fig. 2 is in embodiment 4 and 5c(Cu2+): 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=4.58；E：pH=4.97.D, E 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 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 Gerhardite 8.70 ± 0.01 is weighed, the g of ANN aluminium nitrate nonahydrate 6.75 ± 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(Cu2+)=0.40 mol▪L-1, c (Al3+)=0.20 mol▪L-1）It is transferred in 250 mL hanging bottle type transfusion devices
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, is used in combination
The min of magnetic stirrer 10 is allowed to be completely dissolved, and 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=4.80±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 4.81 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, 80 ± 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 preparing crystal fines product, its diffraction spectrogram as shown in Figure 1, shows in spectrogram
CuAl-NO is shown3The distinctive diffraction maximum of-LDH compounds, crystalline phase is single, and crystallinity is higher.
Embodiment 2：
（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 Gerhardite 21.74 ± 0.01, the g of ANN aluminium nitrate nonahydrate 11.25 ± 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(Cu2+)=0.90 mol▪L-1, c (Al3+)=0.30 mol▪L-1）It is transferred to the transfusion of 250 mL hanging bottle types
It is stand-by in 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 60 ± 1 mL to prepare（pH=4.20±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 4.23, 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, 90 ± 2 DEG C of 24 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 preparing crystal fines product, its diffraction spectrogram as shown in Figure 1, shows in spectrogram
CuAl-NO is shown3The distinctive diffraction maximum of-LDH compounds, crystalline phase is single, and crystallinity is higher.
Embodiment 3：
（1）The mol L of 37.00 ± 0.01 mL 0.2 are pipetted with pipette-1Sodium acetate solution into 100 mL volumetric flasks, then
The mol L of 63.00 ± 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=4.40 ± 0.01.
（2）The g of Gerhardite 28.99 ± 0.01, the g of ANN aluminium nitrate nonahydrate 11.25 ± 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（(Cu2+)=1.00 mol▪L-1, c (Al3+)=0.25 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, 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=4.40±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, in whole course of reaction, the pH value of system is maintained at 4.44, continues to stir 30 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, is sieved after taking-up through grinding, produces into the production of crystal fine powder
Thing.
（6）To the present invention powdery product carry out X-ray diffraction analysis, its diffraction spectrogram as shown in Figure 1, in spectrogram
Show CuAl-NO3The distinctive diffraction maximum of-LDH compounds, crystalline phase is single, and crystallinity is higher.
Embodiment 4：
（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 Gerhardite 24.16 ± 0.01, the g of ANN aluminium nitrate nonahydrate 18.76 ± 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(Cu2+)=1.00 mol▪L-1, c (Al3+)=0.50 mol▪L-1）It is transferred to the transfusion of 250 mL hanging bottle types
It is stand-by in 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）Take acetic acid-sodium acetate buffer that 100 ± 1 mL are prepared（pH=4.60±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 4.58, continues to stir 30 min after dripping, then will
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, is sieved after taking-up through grinding, produces into the production of crystal fine powder
Thing.
（6）To the present invention powdery product carry out X-ray diffraction analysis, its diffraction spectrogram as shown in Figure 2, in spectrogram
Show CuAl-NO3The distinctive diffraction maximum of-LDH compounds, crystalline phase is single, and crystallinity is higher.
Embodiment 5：
（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 Gerhardite 28.99 ± 0.01, the g of ANN aluminium nitrate nonahydrate 22.51 ± 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(Cu2+)=1.20 mol▪L-1, c (Al3+)=0.60 mol▪L-1）It is transferred to the transfusion of 250 mL hanging bottle types
It is stand-by in 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=5.00±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, in whole course of reaction, the pH value of system is maintained at 4.97, continues to stir 20 min after dripping, then will
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
Show CuAl-NO3The distinctive diffraction maximum of-LDH compounds, crystalline phase is single, and crystallinity is higher.
Claims (5)
- A kind of 1. fast preparation method of nitrate anion intercalation copper aluminium houghite, it is characterised in that：With Gerhardite and nine Nitric hydrate aluminium 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, nitrate anion intercalation copper aluminium houghite is made.
- A kind of 2. fast preparation method of nitrate anion intercalation copper 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 solutionGerhardite and ANN aluminium nitrate nonahydrate 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 nitrate anion intercalation copper 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, nitrate anion intercalation copper aluminium houghite is made.
- A kind of 3. fast preparation method of nitrate anion intercalation copper aluminium houghite according to claim 2, it is characterised in that： The step（2）In, willc(Cu2+): c(Al3+) control 2:1~4:1；Whereinc(Cu2+) refer to nitric acid in mixing salt solution The amount concentration of copper material,c(Al3+) refer to aluminum nitrate substance withdrawl syndrome in mixing salt solution.
- A kind of 4. fast preparation method of nitrate anion intercalation copper aluminium houghite according to claim 2, it is characterised in that： The step（2）In, by aluminum nitrate substance withdrawl syndrome control in mixing salt solution in 0.10~1.00 mol L-1。
- A kind of 5. fast preparation method of nitrate anion intercalation copper 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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| CN114314686A (en) * | 2022-01-14 | 2022-04-12 | 青岛理工大学 | One-pot preparation method of LDH micro-nano colloidal coating liquid |
| CN115007205A (en) * | 2022-06-24 | 2022-09-06 | 湘潭大学 | Methyl isothiocyanate intercalated hydrotalcite and preparation method and application thereof |
| CN116196222A (en) * | 2023-02-28 | 2023-06-02 | 上海沐良医疗器械有限公司 | Caries preventing additive, caries preventing material, dental diaphragm and invisible appliance |
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| CN115007205A (en) * | 2022-06-24 | 2022-09-06 | 湘潭大学 | Methyl isothiocyanate intercalated hydrotalcite and preparation method and application thereof |
| CN115007205B (en) * | 2022-06-24 | 2023-08-08 | 湘潭大学 | Methyl isothiocyanate intercalated hydrotalcite-like compound as well as preparation method and application thereof |
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