CN107651712B - 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
- Publication number
- CN107651712B CN107651712B CN201710821940.0A CN201710821940A CN107651712B CN 107651712 B CN107651712 B CN 107651712B CN 201710821940 A CN201710821940 A CN 201710821940A CN 107651712 B CN107651712 B CN 107651712B
- Authority
- CN
- China
- Prior art keywords
- solution
- htlcs
- nitrate
- nial
- anion intercalation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Paper (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses the methods that a kind of one step of co-precipitation prepares nitrate anion intercalation NiAl-HTLcs.The present invention uses NaAc_HAc buffer solution, 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 environment2It dissolves and forms CO32‑The influence of ion is the fast preparation method of pure phase nitrate anion intercalation NiAl-HTLcs.
Description
Technical field
The invention belongs to novel inorganic stratified material fields, and in particular to one kind is by adjustment and control system pH value using co-precipitation
The method that one step prepares nitrate anion intercalation NiAl-HTLcs.
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 nitric acid intercalation hydrotalcite-like
It is standby then generally require by nitrate 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 are 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, the research with NiAl-HTLcs in fields such as catalysis, absorption is goed deep into, and encloses
Step design around NiAl-HTLcs material is still favored by researcher, in recent years, in order to preferably design nickel aluminium class water
Talc materials need to often remove NiAl-HTLcs；Carbonate intercalation NiAl-HTLcs (are denoted as NiAl-CO3- LDH)
It is constrained because of the high forces between carbonate and laminate efficiently to remove.Carry out a step according to demand and prepares easily peelable nitrate anion
Intercalation NiAl-HTLcs (are denoted as NiAl-NO3- LDH) it is very necessary.And it prepares 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 removing assembling and functional application, exploitation meets actual straightforward procedure quickly and effectively to prepare nitrate anion
Intercalation NiAl-HTLcs are significant.
Summary of the invention
Traditional co-precipitation method cannot a step prepare nitrate anion intercalation NiAl-HTLcs aiming at the problem that, the present invention provides
A kind of one step of application co-precipitation prepares nitrate anion intercalation NiAl-HTLcs method；Concrete principle is slow using Acetic acid-sodium acetate
The buffer function for rushing solution is effectively avoiding CO in environment by the pH stability contorting of preparation system 4.00~5.002Dissolution pair
An efficient step prepares NiAl-NO on the basis of the influence of prepared product3-LDH。
The present invention provides the methods that a kind of one step of co-precipitation prepares 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
Nitrate anion intercalation NiAl-HTLcs are made in precipitating, 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 corresponding acetic acid is 0.060~0.164mol L-1, it is molten to be made into Acetic acid-sodium acetate buffering
Liquid；
(2) mixing salt solution is prepared
It weighs Nickelous nitrate hexahydrate and ANN aluminium nitrate nonahydrate 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) nitrate anion intercalation NiAl-HTLcs are 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；Nitrate anion intercalation NiAl-HTLcs are made.
It, will in the step (2) in the above methodc(Ni2+): c(Al3+) control in 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, in the step (2), the substance withdrawl syndrome of aluminum nitrate 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 control of preparation system pH stable is existed
4.00 ~ 5.00, which can effectively avoid CO in environment2It dissolves and forms CO3 2-The influence of ion is simple and quick
Prepare the effective ways of pure 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-Into NiAl-HTLcs layer
Between, it will assign inner layer space and soda acid that nitrate anion intercalation NiAl-HTLcs are different from carbonate intercalation NiAl-HTLcs
Performance, the change of these performances will affect its catalytic applications to a certain extent；
(3) due to NO3 -It is weaker than CO3 2-With the binding force of laminate, nitrate anion intercalation NiAl-HTLcs usually have preferably
Stripping performance will provide safeguard for effectively assembling using NiAl-HTLcs material.
Detailed description of the invention
Fig. 1 is that different nickel 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(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 respectively correspond embodiment 1 ~ 3.
Fig. 2 is the X ray diffracting spectrum (XRD) of preparation gained sample in embodiment 4 and 5.D:c(Ni2+) : c(Al3+)
=3:1, pH=4.77；E:c(Ni2+) : c(Al3+)=3:1, pH=4.25；D, E 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) 31.41 ± 0.01 g of Nickelous nitrate hexahydrate, 20.26 ± 0.01 g of ANN aluminium nitrate nonahydrate are weighed, is mixed and adds
Enter in beaker, 90 ± 1 mL deionized waters is added in beaker, and be allowed to be completely dissolved with 10 min of magnetic stirrer, it will
Prepared solution (c (Ni2+The mol L of)=1.20-1, c (Al3+)=0.60 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, 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=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 4.02 in entire reaction process, continues 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, 90 ± 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) to crystal fines product progress X-ray diffraction analysis is prepared, diffraction spectrogram is as shown in Fig. 1, shows in spectrogram
NiAl-NO is shown3The distinctive diffraction maximum of-LDH compound, 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 to 100 mL volumetric flasks
In, then 51.00 ± 0.01 mL 0.2mol L are added thereto-1Acetum, shaking by swirling is allowed to uniformly mixed, and constant volume is made into
The NaAc_HAc buffer solution of 100 pH=4.60 ± 0.01 mL.
(2) 43.62 ± 0.01 g of Nickelous nitrate hexahydrate, 18.76 ± 0.01 g of ANN aluminium nitrate nonahydrate 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 (Ni2+The mol L of)=1.50-1, c (Al3+)=0.50 mol▪L-1) it is transferred to the infusion of 250 mL hanging bottle types
It is stand-by in 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 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, the pH value of system is maintained at 4.57 in entire reaction process, continues to stir 25 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
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, 85 ± 2 DEG C of 24 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) to crystal fines product progress X-ray diffraction analysis is prepared, diffraction spectrogram is as shown in Fig. 1, shows in spectrogram
NiAl-NO is shown3The distinctive diffraction maximum of-LDH compound, 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 to 100 mL volumetric flasks
In, then 30.00 ± 0.01 mL, 0.2 mol L is added thereto-1Acetum, shaking by swirling is allowed to uniformly mixed, and constant volume is made into
The NaAc_HAc buffer solution of 100 pH=5.00 ± 0.01 mL.
(2) 34.89 ± 0.01 g of Nickelous nitrate hexahydrate, 11.25 ± 0.01 g of ANN aluminium nitrate nonahydrate 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 (Ni2+The mol L of)=1.00-1, c (Al3+)=0.25 mol▪L-1) it is transferred to the infusion of 250 mL hanging bottle types
It is stand-by in 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 4.98 in entire reaction process, continues 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, 85 ± 2 DEG C of 24 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. 1, in spectrogram
Show NiAl-NO3The distinctive diffraction maximum of-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 to 100 mL volumetric flasks
In, then 41.00 ± 0.01 mL, 0.2 mol L is added thereto-1Acetum, shaking by swirling is allowed to uniformly mixed, and constant volume is made into
The NaAc_HAc buffer solution of 100 pH=4.80 ± 0.01 mL.
(2) 26.17 ± 0.01 g of Nickelous nitrate hexahydrate, 11.25 ± 0.01 g of ANN aluminium nitrate nonahydrate 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 (Ni2+The mol L of)=0.90-1, c (Al3+)=0.30 mol▪L-1) it is transferred to the infusion of 250 mL hanging bottle types
It is stand-by in 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=4.80 ± 0.01) 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, the pH value of system is maintained at 4.77 in entire reaction process, continues to stir 20 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 110 ± 2 DEG C of baking ovens
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, 98 ± 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 NiAl-NO3The distinctive diffraction maximum of-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) 26.17 ± 0.01 g of Nickelous nitrate hexahydrate, 11.25 ± 0.01 g of ANN aluminium nitrate nonahydrate 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 (Ni2+The mol L of)=0.75-1, c (Al3+)=0.25 mol▪L-1) it is transferred to the infusion of 250 mL hanging bottle types
It is stand-by in 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, the pH value of system is maintained at 4.25 in entire reaction process, continues to stir 20 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 110 ± 2 DEG C of baking ovens
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, 90 ± 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 NiAl-NO3The distinctive diffraction maximum of-LDH compound, crystal phase is single, and crystallinity is higher.
Claims (4)
1. one step of the co-precipitation method for preparing 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,
Nitrate anion intercalation NiAl-HTLcs are 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, 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 Nickelous nitrate hexahydrate and ANN aluminium nitrate nonahydrate 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) nitrate anion intercalation NiAl-HTLcs are 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 hydroxide solution of preparation and mixing salt solution are instilled in the above-mentioned reactor equipped with buffer solution,
And with the pH value in acidometer real-time monitoring titration process, controlling rate of titration fixes system pH in entire reaction process；
Continue 20~30 min of stirring after dripping, obtained precipitating and mother liquor sealing are then placed in the stainless of polytetrafluoroethyllining lining
In steel reaction kettle, 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 nitrate anion intercalation NiAl-HTLcs.
2. the method that one step of co-precipitation according to claim 1 prepares nitrate anion intercalation NiAl-HTLcs, feature exist
In: it, will in the step (2)c(Ni2+): c(Al3+) control in 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.
3. the method that one step of co-precipitation according to claim 1 prepares nitrate anion intercalation NiAl-HTLcs, feature exist
In: in the step (2), by aluminum nitrate substance withdrawl syndrome control in mixing salt solution in 0.10~1.00 mol L-1。
4. the method that one step of co-precipitation according to claim 1 prepares nitrate anion intercalation NiAl-HTLcs, feature exist
In: in step (4), system pH control is 4.00~5.00 in reaction process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710821940.0A CN107651712B (en) | 2017-09-13 | 2017-09-13 | It is co-precipitated the method that a step prepares nitrate anion intercalation NiAl-HTLcs |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710821940.0A CN107651712B (en) | 2017-09-13 | 2017-09-13 | It is co-precipitated the method that a step prepares nitrate anion intercalation NiAl-HTLcs |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107651712A CN107651712A (en) | 2018-02-02 |
| CN107651712B true CN107651712B (en) | 2019-06-18 |
Family
ID=61129961
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710821940.0A Active CN107651712B (en) | 2017-09-13 | 2017-09-13 | It is co-precipitated the method that a step prepares nitrate anion intercalation NiAl-HTLcs |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107651712B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109502656B (en) * | 2018-11-29 | 2021-02-19 | 兰州金通储能动力新材料有限公司 | Spherical Co (II) Co (III) hydrotalcite-like material 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 |
| CN114247411B (en) * | 2021-12-23 | 2023-05-05 | 华北理工大学 | Device and method for preparing hydrotalcite-like compound by continuous flow coprecipitation |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1566260A (en) * | 2003-07-01 | 2005-01-19 | 北京化工大学 | Photochromic nitrate type hydrotalcite and method for producing the same |
| CN101140257A (en) * | 2007-10-18 | 2008-03-12 | 北京化工大学 | Biologic sensor enzyme functional susceptivity film containing nickel and aluminum hydrotalcite nano piece and method of producing the same |
| EP3015429A1 (en) * | 2014-10-30 | 2016-05-04 | Wintershall Holding GmbH | Monolayer from at least one layered double hydroxide (LDH) |
-
2017
- 2017-09-13 CN CN201710821940.0A patent/CN107651712B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1566260A (en) * | 2003-07-01 | 2005-01-19 | 北京化工大学 | Photochromic nitrate type hydrotalcite and method for producing the same |
| CN101140257A (en) * | 2007-10-18 | 2008-03-12 | 北京化工大学 | Biologic sensor enzyme functional susceptivity film containing nickel and aluminum hydrotalcite nano piece and method of producing the same |
| EP3015429A1 (en) * | 2014-10-30 | 2016-05-04 | Wintershall Holding GmbH | Monolayer from at least one layered double hydroxide (LDH) |
Non-Patent Citations (1)
| Title |
|---|
| "铜铝类水滑石催化合成安息香乙醚的研究";吴旭等;《太原理工大学学报》;20140930;第４５卷(第５期);第605页左栏第2段至第606页右栏第2段 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107651712A (en) | 2018-02-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107651712B (en) | It is co-precipitated the method that a step prepares nitrate anion intercalation NiAl-HTLcs | |
| CN101094810B (en) | Composite oxides or hydroxides comprising alumina, zirconia and optionally ceria and/or rare earth oxides for automotive catalyst applications and method of manufacturing | |
| CN107555491B (en) | It is co-precipitated the method that a step prepares nitrate anion intercalation cobalt aluminium houghite | |
| CN103818927B (en) | The method of the synthetic high hydrothermal stability cupric CHA type molecular sieve of one-step method | |
| CN109311687A (en) | The method of continuous synthetic zeolite material | |
| CN104692429B (en) | A kind of controllable method for preparing of bigger serface macropore volume boehmite | |
| CN107555465A (en) | A kind of fast preparation method of nitrate anion intercalation copper aluminium houghite | |
| CN102219245B (en) | Pseudoboehmite and aluminium oxide prepared from same | |
| CN110407221A (en) | A kind of preparation method of chabazite molecular sieve, the preparation method of SCR catalyst | |
| CN102674389B (en) | Preparation method of titanium-containing nano-mordenite molecular sieve | |
| CN107555490B (en) | A method of quickly preparing chloride ion intercalation cobalt aluminium houghite | |
| CN101962194B (en) | Method for preparing ZSM-34 and heteroatomic substitution molecular sieve thereof by direct synthesis method | |
| CN107446138B (en) | A kind of method and application preparing MIL-100 (Fe) using floride-free auxiliary agent sodium carbonate | |
| CN108217702A (en) | A kind of method that the synthesis and its pyrolysis of ultramicropore aluminum carbonate basic ammonium prepare aluminium oxide | |
| CN102850056A (en) | Preparation method of spherical ferrite | |
| CN107500367B (en) | A kind of preparation method of chloride ion intercalation NiAl-HTLcs | |
| CN106865565A (en) | A kind of flyash synthesizes the method for X-type zeolite | |
| CN107188207B (en) | A kind of preparation method for the magnesium oxide material being assembled into micron bar structure by nanometer sheet | |
| CN109775734A (en) | A kind of preparation method of low specific surface area basic magnesium carbonate | |
| CN102502812A (en) | Method for preparing octahedral nano titanium dioxide | |
| CN107115856A (en) | A kind of preparation method of sheet bismuth titanates chlorine oxygen bismuth composite | |
| CN107619063B (en) | A method of preparing chloride ion intercalation copper aluminium houghite | |
| CN102963925B (en) | Method for preparing nanometer n-zinc titanate spinel by virtue of taking zinc-titanium hydrotalcite as precursor | |
| CN101573297A (en) | Processes for the flux calcination production of titanium dioxide | |
| CN102294247B (en) | Visible light responsive composite photocatalyst and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |