CN107651712A - It is co-precipitated the method that a step prepares nitrate anion intercalation NiAl-HTLcs - Google Patents
It is co-precipitated the method that a step prepares nitrate anion intercalation NiAl-HTLcs Download PDFInfo
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- CN107651712A CN107651712A CN201710821940.0A CN201710821940A CN107651712A CN 107651712 A CN107651712 A CN 107651712A CN 201710821940 A CN201710821940 A CN 201710821940A CN 107651712 A CN107651712 A CN 107651712A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
Abstract
The invention discloses a kind of method for being co-precipitated a step and preparing nitrate anion intercalation NiAl-HTLcs.The present invention uses acetic acid sodium acetate buffer, the pH stable of preparation system is controlled 4.00~5.00, using Nickelous nitrate hexahydrate, 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 NiAl-HTLcs.This preparation method can effectively avoid CO in environment2Dissolve and form CO32‑The influence of ion, it is the fast preparation method of pure phase nitrate anion intercalation NiAl-HTLcs.
Description
Technical field
The invention belongs to novel inorganic stratified material field, and in particular to a kind of used by adjustment and control system pH value is co-precipitated
The method that one step prepares nitrate anion intercalation NiAl-HTLcs.
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 NiAl-HTLcs are as important a member in such material, it
Synthesis and application study always by extensive concern, as research of the NiAl-HTLcs in fields such as catalysis, absorption is goed deep into, enclose
Step design around NiAl-HTLcs material still enjoys researcher to favor, in recent years, in order to preferably design nickel aluminium class water
Talc materials, NiAl-HTLcs need to often be peeled off；Carbonate intercalation NiAl-HTLcs（It is designated as NiAl-CO3-LDH）
It is constrained because of the high forces between carbonate and laminate efficiently to peel off.Carry out a step according to demand and prepare easily peelable nitrate anion
Intercalation NiAl-HTLcs（It is designated as NiAl-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 NiAl-HTLcs is obviously outdated.In concern nickel
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 NiAl-HTLcs are significant.
The content of the invention
For traditional co-precipitation method can not a step prepare nitrate anion intercalation NiAl-HTLcs the problem of, the invention provides
One kind application one step of co-precipitation prepares nitrate anion intercalation NiAl-HTLcs method；Concrete principle is delayed using Acetic acid-sodium acetate
The cushioning effect of solution is rushed, by the pH stability contortings of preparation system 4.00~5.00, in effective CO in avoiding environment2Dissolving pair
An efficient step prepares NiAl-NO on the basis of the influence of prepared product3-LDH。
The invention provides a kind of method for being co-precipitated a step and preparing nitrate anion intercalation NiAl-HTLcs, with six hydration nitre
Sour nickel, ANN aluminium nitrate nonahydrate are raw material, and using sodium hydroxide as precipitating reagent, deionized water is as solvent, and formulated solution, titration are altogether
Precipitation, hydro-thermal process, washing, suction filtration, drying steps, nitrate anion intercalation NiAl-HTLcs are 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 0.060~0.164mol L-1, it is made into NaAc_HAc buffer solution；
（2）Prepare mixing salt solution
Nickelous nitrate hexahydrate 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 NiAl-HTLcs
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 NiAl-HTLcs are made.
In the above method, the step（2）In, willc(Ni2+): c(Al3+) control 2:1~4:1.Whereinc(Ni2+) be
Refer to nickel 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 NiAl-HTLcs；
（2）Due to NO3 -Different from CO3 2-Radius and its acid-base property, NO3 -Instead of CO3 2-, will into NiAl-HTLcs interlayer
Inner layer space and soda acid performance that nitrate anion intercalation NiAl-HTLcs are different from carbonate intercalation NiAl-HTLcs 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 NiAl-HTLcs generally have preferably stripping
From performance, it will be that effectively assembling provides safeguard using NiAl-HTLcs material.
Brief description of the drawings
Fig. 1 is that different nickel 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(Ni2+): c(Al3+)=2:1, pH=4.02；B:c(Ni2+): c(Al3+)=3:1, pH=4.57；C:c
(Ni2+): c(Al3+)=4:1, pH=4.98.A, B, C correspond to embodiment 1 ~ 3 respectively.
Fig. 2 is the X ray diffracting spectrum that gained sample is prepared in embodiment 4 and 5（XRD）.D：c(Ni2+) : c(Al3+)
=3:1, pH=4.77；E：c(Ni2+) : c(Al3+) =3:1, pH=4.25；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 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 Nickelous nitrate hexahydrate 31.41 ± 0.01, the g of ANN aluminium nitrate nonahydrate 20.26 ± 0.01 are weighed, is mixed and adds
Enter in beaker, 90 ± 1 mL deionized waters are added in beaker, and be allowed to be completely dissolved with the min of magnetic stirrer 10, will
The solution prepared（c(Ni2+）=1.20 mol▪L-1, c (Al3+)=0.60 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=4.00±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 4.02 in whole course of reaction, continues 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, 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）X-ray diffraction analysis are carried out to preparing crystal fines product, its diffraction spectrogram as shown in Figure 1, shows in spectrogram
NiAl-NO is shown3The distinctive diffraction maximum of-LDH compounds, 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 Nickelous nitrate hexahydrate 43.62 ± 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(Ni2+）=1.50 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）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, the pH value of system is maintained at 4.57 in whole course of reaction, continues to stir 25 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
12 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 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
NiAl-NO is shown3The distinctive diffraction maximum of-LDH compounds, 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 Nickelous nitrate hexahydrate 34.89 ± 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（c(Ni2+）=1.00 mol▪L-1, c (Al3+)=0.25 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 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 4.98 in whole course of reaction, continues 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, 85 ± 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 NiAl-NO3The distinctive diffraction maximum of-LDH compounds, 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 Nickelous nitrate hexahydrate 26.17 ± 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(Ni2+）=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 100 ± 1 mL to prepare（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, the pH value of system is maintained at 4.77 in whole course of reaction, continues to stir 20 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 110 ± 2 DEG C of baking ovens
12 h。
（5）After question response kettle natural cooling, reacted solution is filtered to obtain sediment, repeatedly uses deionized water
After washing to neutrality, 98 ± 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 NiAl-NO3The distinctive diffraction maximum of-LDH compounds, 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 Nickelous nitrate hexahydrate 26.17 ± 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（c(Ni2+）=0.75 mol▪L-1, c (Al3+)=0.25 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=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, the pH value of system is maintained at 4.25 in whole course of reaction, continues to stir 20 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 110 ± 2 DEG C of baking ovens
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 NiAl-NO3The distinctive diffraction maximum of-LDH compounds, crystalline phase is single, and crystallinity is higher.
Claims (5)
1. the method that one step of co-precipitation prepares nitrate anion intercalation NiAl-HTLcs, it is characterised in that：With ANN aluminium nitrate nonahydrate with
Nickelous nitrate 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, nitrate anion intercalation NiAl-HTLcs are made.
2. the method that one step of co-precipitation according to claim 1 prepares nitrate anion intercalation NiAl-HTLcs, its feature exist
In：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, 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 solution
Nickelous nitrate hexahydrate 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 and hang
It is stand-by in bottle type infusion device；
（4）Prepare nitrate anion intercalation NiAl-HTLcs
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 sodium hydroxide solution of preparation and mixing salt solution are instilled in the above-mentioned reactor equipped with cushioning liquid,
And fix system pH in whole course of reaction with the pH value during the real-time monitoring titration of acidometer, control rate of titration；
Continue the min of stirring 20~30 after dripping, obtained precipitation and mother liquor sealing are then placed in the stainless of polytetrafluoroethyllining lining
In steel reactor, 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 NiAl-HTLcs are made.
3. the method that one step of co-precipitation according to claim 2 prepares nitrate anion intercalation NiAl-HTLcs, its feature exist
In：The step（2）In, willc(Ni2+): c(Al3+) control 2:1~4:1, whereinc(Ni2+) refer to nitre in mixing salt solution
Sour nickel substance withdrawl syndrome,c(Al3+) refer to aluminum nitrate substance withdrawl syndrome in mixing salt solution.
4. the method that one step of co-precipitation according to claim 2 prepares nitrate anion intercalation NiAl-HTLcs, its feature exist
In：The step（2）In, by aluminum nitrate substance withdrawl syndrome control in mixing salt solution in 0.10~1.00 mol L-1。
5. the method that one step of co-precipitation according to claim 2 prepares nitrate anion intercalation NiAl-HTLcs, its feature exist
In：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 |
| CN110302789A (en) * | 2019-06-27 | 2019-10-08 | 中国科学院广州能源研究所 | A kind of Na-NiAl (O) catalyst and its application in the biological aviation fuel presoma of preparation |
| CN114247411A (en) * | 2021-12-23 | 2022-03-29 | 华北理工大学 | Device and method for preparing hydrotalcite-like compound by continuous flow coprecipitation |
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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 |
| CN110302789A (en) * | 2019-06-27 | 2019-10-08 | 中国科学院广州能源研究所 | A kind of Na-NiAl (O) catalyst and its application in the biological aviation fuel presoma of preparation |
| CN114247411A (en) * | 2021-12-23 | 2022-03-29 | 华北理工大学 | Device and method for preparing hydrotalcite-like compound by continuous flow coprecipitation |
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| CN107651712B (en) | 2019-06-18 |
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