CN101962211A - Method for preparing nano nickel bicarbonate - Google Patents
Method for preparing nano nickel bicarbonate Download PDFInfo
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- CN101962211A CN101962211A CN201010518911.5A CN201010518911A CN101962211A CN 101962211 A CN101962211 A CN 101962211A CN 201010518911 A CN201010518911 A CN 201010518911A CN 101962211 A CN101962211 A CN 101962211A
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- nickel
- urotropine
- nickel salt
- urea
- calcium carbonate
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 107
- 238000000034 method Methods 0.000 title claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000012153 distilled water Substances 0.000 claims abstract description 37
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 34
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000004202 carbamide Substances 0.000 claims abstract description 25
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 150000002815 nickel Chemical class 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000001291 vacuum drying Methods 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 13
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 34
- 239000001257 hydrogen Substances 0.000 claims description 30
- 229910052739 hydrogen Inorganic materials 0.000 claims description 30
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 29
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 29
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims description 29
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 18
- 238000001556 precipitation Methods 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 10
- 239000012266 salt solution Substances 0.000 claims description 6
- -1 stirs Chemical compound 0.000 claims description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 2
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 2
- IYFXESRMJKRSNZ-UHFFFAOYSA-L hydrogen carbonate;nickel(2+) Chemical compound [Ni+2].OC([O-])=O.OC([O-])=O IYFXESRMJKRSNZ-UHFFFAOYSA-L 0.000 claims description 2
- 239000011541 reaction mixture Substances 0.000 claims description 2
- 238000001816 cooling Methods 0.000 abstract description 17
- 239000002159 nanocrystal Substances 0.000 abstract description 2
- 239000012716 precipitator Substances 0.000 abstract 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 16
- 238000002360 preparation method Methods 0.000 description 6
- 238000012916 structural analysis Methods 0.000 description 4
- 241000080590 Niso Species 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000006183 anode active material Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000012018 catalyst precursor Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 1
- 125000000449 nitro group Chemical group [O-][N+](*)=O 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
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- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method for preparing nano nickel bicarbonate, which comprises the following steps of: adding water into urea or urotropine for dissolving, adding nickel salt or nickel hydroxide and stirring, wherein the mole ratio of the urea or the urotropine to nickel is 1:1-16:1, and the concentration of the nickel salt in solution is 0.1-1.0mol/L; shifting the obtained solution into a hydrothermal reactor; after reacting at 90-240 DEG C for 1-96 hours, cooling; and filtering obtained reaction mixed liquid, washing with distilled water and anhydrous ethanol and placing in a vacuum drying box at 60 DEG C for drying to obtain a cubic phase nano nickel bicarbonate square block with the size of 100nm or so. The invention uses the urotropine or the urea as a precipitator, NH3 and CO2 generated by the precipitator dissolve nickel hydroxide, and the pure cubic phase Ni(HCO3)2 nano crystal is prepared finally.
Description
Technical field
The present invention relates to a kind of preparation method of mineral compound, specifically, is the method for Hydrothermal Preparation nano-calcium carbonate hydrogen nickel.
Background technology
At present, because Ni (OH)
2Be the battery anode active material of generally acknowledging, in recent years for Ni (OH)
2Research emerge in an endless stream, and to Ni (HCO
3)
2Research, bibliographical information gets seldom.What finding was mentioned is the mixed phase that is produced in the process of preparation nickel-containing catalyst, when preparing the silicoaluminate nickel catalyzator as human sol-gel methodes such as K. J.Ciufi, Ni (HCO is arranged in the mixed phase of appearance
3)
2Peter Birke etc. produce by Ni (HCO in the catalyst precursor preparation when preparation makes the nitro hydrogenation of nitryl aromatic thing generate the catalyzer of corresponding amine
3)
2And Ni
3(OH)
4(NO
3)
2The mixture of forming.
Summary of the invention
The purpose of this invention is to provide a kind of economical and practical, the method for preparing nano-calcium carbonate hydrogen nickel of efficient and environmental protection.The present invention transforms synthesis of cubic phase Ni (HCO by urotropine or urea with non-crystalline state or the dissolving of crystalline state nickel hydroxide under the condition of high pressure hydro-thermal
3)
2The nanometer square can be a precipitation agent by urotropine or urea also, at Ni
2+-NH
3-CO
2-H
2Directly synthetic pure phase Ni (HCO in the O reaction system
3)
2Nano particle.Technical scheme of the present invention is as follows:
A kind of method for preparing nano-calcium carbonate hydrogen nickel, it comprises the steps:
Step 1. is dissolved in water urea or urotropine, adds nickel salt or nickel hydroxide, stirs, and urea or urotropine are 1:1 ~ 16:1 with the ratio of the amount of substance of nickel, and the concentration of nickel salt is 0.1 ~ 1.0mol/L in the solution;
The solution that step 2. obtains step 1 is transferred in the hydrothermal reaction kettle,, cools off after 1 ~ 96 hour in reaction under 90 ~ 240 ℃;
The reaction mixture that step 3. obtains step 2 filters, the product that filters out with distilled water and absolute ethanol washing again, and place 60 ℃ vacuum drying oven drying, make the cubic-phase nano hydrogen-carbonate nickel square about 100nm.
The above-mentioned method for preparing nano-calcium carbonate hydrogen nickel, described nickel hydroxide can be commercially available nickel hydroxides, also can following method prepare:
Nickel salt and sodium hydroxide or potassium hydroxide is dissolved in generates amorphous Ni (OH) in the distilled water
2Precipitation suspension, nickel salt is 1:1.2 ~ 1:2.0 with the ratio of the amount of substance of sodium hydroxide or potassium hydroxide, and the concentration of nickel salt solution is 0.1 ~ 1.0mol/L, and so, in the step 1, described urea or urotropine are 1:1 ~ 8:1 with the ratio of the amount of substance of nickel salt.
The above-mentioned method for preparing nano-calcium carbonate hydrogen nickel, in the step 1, the ratio of the preferred amount of substance of described urea and nickel salt is 4:1 ~ 16:1, the concentration of nickel salt solution is 0.1 ~ 2.0mol/L.
The above-mentioned method for preparing nano-calcium carbonate hydrogen nickel, in the step 1, the ratio of the preferred amount of substance of described urotropine and nickel salt is 1:1 ~ 16:1, and preferred hydrothermal temperature is 170 ~ 240 ℃, and the concentration of nickel salt solution is 0.1 ~ 2.0mol/L.
The above-mentioned method for preparing nano-calcium carbonate hydrogen nickel, described nickel salt can be hydrochloride, vitriol, nitrate, acetate and oxalate.
The present invention is a precipitation agent with urotropine or urea, the NH of its generation
3And CO
2With the dissolved hydrogen nickel oxide, finally prepare pure cube phase Ni (HCO
3)
2Nanocrystal.
Ni (the HCO that the present invention makes
3)
2Can be used for catalyzer and experiment reagent, thermal degradation can prepare highly purified nano NiO, also can be used for catalyzer and lab analysis titration etc.
Description of drawings
Fig. 1 is that the direct hydro-thermal reaction product when not adding urea in the step 1 is sheet β-Ni (OH)
2
Fig. 2 is by the synthetic Ni (HCO of urea conversion method
3)
2XRD(a), SEM(b) and TEM(c) photo;
Fig. 3 is by the synthetic Ni (HCO of urotropine conversion method
3)
2XRD(a), SEM(b) and TEM(c) photo;
Fig. 4 is by urea direct method synthetic Ni (HCO
3)
2XRD(a), SEM(b) photo;
Fig. 5 is by the direct synthetic Ni of urotropine (HCO
3)
2XRD(a), SEM(b) photo.
Embodiment
Embodiment 1
With 1.523 g (0.0064 mol) NiCl
26H
2O and 0.341 g (0.0085 mol) NaOH is dissolved in the 40 mL distilled water, generates amorphous Ni (OH)
2Precipitation suspension is transferred to precipitation in the 50 mL teflon-lined hydrothermal reaction kettles, and at above-mentioned neutral amorphous Ni (OH)
2Add 1.536g (0.0256 mol) urea in the precipitation suspension, 180 ℃ of reaction 4h.After hydro-thermal reaction finished, two sample throw outs were filtered in cooling, and it is inferior respectively to give a baby a bath on the third day after its birth with distilled water and dehydrated alcohol successively, and dry 4 h in 60 ℃ vacuum drying oven obtain nano-calcium carbonate hydrogen nickel then.Its structural analysis and Photomicrograph are seen Fig. 4.
Embodiment 2
With 0.995 g (0.004 mol) Ni (CH
3COO)
24H
2O and 0.192 g (0.0048 mol) NaOH is dissolved in the 40 mL distilled water, generates amorphous Ni (OH)
2Precipitation suspension is transferred to precipitation in the 50 mL teflon-lined hydrothermal reaction kettles, adds 1.922g (0.032mol) urea, 240 ℃ of reaction 1h.After hydro-thermal reaction finished, the sample throw out was filtered in cooling, and it is inferior respectively to give a baby a bath on the third day after its birth with distilled water and dehydrated alcohol successively, and dry 4h makes nano-calcium carbonate hydrogen nickel in 60 ℃ vacuum drying oven then.
Embodiment 3
With 11.63 g (0.04 mol) Ni (NO
3)
26H
2O and 4.49 g (0.08 mol) KOH is dissolved in the 40 mL distilled water, generates amorphous Ni (OH)
2Precipitation suspension is transferred to precipitation in the 50mL teflon-lined hydrothermal reaction kettle, adds 2.401g (0.04mol) urea, 90 ℃ of reaction 96h.After hydro-thermal reaction finished, the sample throw out was filtered in cooling, and it is inferior respectively to give a baby a bath on the third day after its birth with distilled water and dehydrated alcohol successively, and dry 4h makes nano-calcium carbonate hydrogen nickel in 60 ℃ vacuum drying oven then.
Embodiment 4
1.536 g (0.0256 mol) urea is dissolved in the 40 mL distilled water, this solution is shifted in 50mL teflon-lined hydrothermal reaction kettle, in this solution, add 0.593g (0.0064mol) Ni (OH) again
2And stir, the fastening reactor is in 180 ℃ of reaction 4h.After hydro-thermal reaction finished, the sample throw out was filtered in cooling, and it is inferior respectively to give a baby a bath on the third day after its birth with distilled water and dehydrated alcohol successively, and dry 4 h make nano-calcium carbonate hydrogen nickel in 60 ℃ vacuum drying oven then.
Embodiment 5
With 1.19 g (0.005mol) NiCl
26H
2O and 0.267g (0.0067mol) NaOH is dissolved in the 40mL distilled water, generates amorphous Ni (OH)
2Precipitation suspension is at above-mentioned neutral amorphous Ni (OH)
2Add 2.8g (0.02mol) urotropine in the precipitation suspension, 180 ℃ of reaction 24h.After hydro-thermal reaction finished, two sample throw outs were filtered in cooling, and it is inferior respectively to give a baby a bath on the third day after its birth with distilled water and dehydrated alcohol successively, and dry 4h makes nano-calcium carbonate hydrogen nickel in 60 ℃ vacuum drying oven then.Its structural analysis and Photomicrograph are seen Fig. 5.
Embodiment 6
With 1.051g (0.004 mol) NiSO
46H
2O and 0.192g (0.0048 mol) NaOH is dissolved in the 40mL distilled water, generates amorphous Ni (OH)
2Precipitation suspension is transferred to precipitation in the 50mL teflon-lined hydrothermal reaction kettle, adds 4.49g (0.032mol) urotropine, 240 ℃ of reaction 12h.After hydro-thermal reaction finished, the sample throw out was filtered in cooling, and it is inferior respectively to give a baby a bath on the third day after its birth with distilled water and dehydrated alcohol successively, and dry 4h makes nano-calcium carbonate hydrogen nickel in 60 ℃ vacuum drying oven then.
Embodiment 7
With 11.63 g (0.04 mol) Ni (NO
3)
26H
2O and 4.49g (0.08 mol) KOH is dissolved in the 40mL distilled water, generates amorphous Ni (OH)
2Precipitation suspension is transferred to precipitation in the 50mL teflon-lined hydrothermal reaction kettle, adds 5.607g (0.04mol) urotropine, 90 ℃ of reaction 96h.After hydro-thermal reaction finished, the sample throw out was filtered in cooling, and it is inferior respectively to give a baby a bath on the third day after its birth with distilled water and dehydrated alcohol successively, and dry 4h makes nano-calcium carbonate hydrogen nickel in 60 ℃ vacuum drying oven then.
Embodiment 8
2.8g (0.02 mol) urotropine is dissolved in the 40mL distilled water, this solution is shifted in 50mL teflon-lined hydrothermal reaction kettle, in this solution, add 0.463g (0.005mol) Ni (OH) again
2And stir, the fastening reactor is in 180 ℃ of reaction 24 h.After hydro-thermal reaction finished, the sample throw out was filtered in cooling, and it is inferior respectively to give a baby a bath on the third day after its birth with distilled water and dehydrated alcohol successively, and dry 4h makes nano-calcium carbonate hydrogen nickel in 60 ℃ vacuum drying oven then.
With 1.523 g (0.0064mol) NiCl
26H
2O and 1.537 g (0.0256mol) urea are dissolved in the 40mL distilled water, stir 10 min and obtain green clear liquor, gained solution are transferred in the 50mL teflon-lined hydrothermal reaction kettle, at 160 ℃ of reaction 4h.After hydro-thermal reaction finished, throw out was filtered in cooling, and it is inferior respectively to give a baby a bath on the third day after its birth with distilled water and dehydrated alcohol successively, and dry 4h makes nano-calcium carbonate hydrogen nickel in 60 ℃ vacuum drying oven then, and its structural analysis and Photomicrograph are seen Fig. 6.
Embodiment 10
With 0.995g (0.004mol) Ni (CH
3COO)
24H
2O and 0.192g (0.0032mol) urea is dissolved in the 40mL distilled water, stirs 10min and obtains green clear liquor, gained solution is transferred in the 50mL teflon-lined hydrothermal reaction kettle, at 90 ℃ of reaction 96h.After hydro-thermal reaction finished, throw out was filtered in cooling, and it is inferior respectively to give a baby a bath on the third day after its birth with distilled water and dehydrated alcohol successively, and dry 4h makes nano-calcium carbonate hydrogen nickel in 60 ℃ vacuum drying oven then.
Embodiment 11
With 1.861g (0.0064mol) Ni (NO
3)
26H
2O and 6.149g (0.1024mol) urea is dissolved in the 40mL distilled water, stirs 10min and obtains green clear liquor, gained solution is transferred in the 50mL teflon-lined hydrothermal reaction kettle, at 240 ℃ of reaction 1h.After hydro-thermal reaction finished, throw out was filtered in cooling, and it is inferior respectively to give a baby a bath on the third day after its birth with distilled water and dehydrated alcohol successively, and dry 4h makes nano-calcium carbonate hydrogen nickel in 60 ℃ vacuum drying oven then.
Embodiment 12
With 21.02g (0.08mol) NiSO
46H
2O and 19.22 g (0.32mol) urea are dissolved in the 40mL distilled water, stir 10 min and obtain green clear liquor, gained solution are transferred in the 50mL teflon-lined hydrothermal reaction kettle, at 160 ℃ of reaction 12h.After hydro-thermal reaction finished, throw out was filtered in cooling, and it is inferior respectively to give a baby a bath on the third day after its birth with distilled water and dehydrated alcohol successively, and dry 4h makes nano-calcium carbonate hydrogen nickel in 60 ℃ vacuum drying oven then.
Embodiment 13
With 1.19 g (0.005mol) NiCl
26H
2O and 1.40g (0.01mol) urotropine is dissolved in the 40mL distilled water, stirs 10min and obtains green clear liquor, gained solution is transferred in the 50mL teflon-lined hydrothermal reaction kettle, at 180 ℃ of reaction 4h.After hydro-thermal reaction finished, throw out was filtered in cooling, and it is inferior respectively to give a baby a bath on the third day after its birth with distilled water and dehydrated alcohol successively, and dry 4h makes nano-calcium carbonate hydrogen nickel in 60 ℃ vacuum drying oven then, and its its structural analysis and Photomicrograph are seen Fig. 7.
Embodiment 14
With 0.995g (0.004mol) Ni (CH
3COO)
24H
2O and 2.80g (0.02mol) urotropine is dissolved in the 40mL distilled water, stirs 10min and obtains green clear liquor, gained solution is transferred in the 50mL teflon-lined hydrothermal reaction kettle, at 170 ℃ of reaction 96h.After hydro-thermal reaction finished, throw out was filtered in cooling, and it is inferior respectively to give a baby a bath on the third day after its birth with distilled water and dehydrated alcohol successively, and dry 4h makes nano-calcium carbonate hydrogen nickel in 60 ℃ vacuum drying oven then.
Embodiment 15
With 21.02g (0.08mol) NiSO
46H
2O and 11.21g (0.08mol) urotropine is dissolved in the 40mL distilled water, stirs 10min and obtains green clear liquor, gained solution is transferred in the 50mL teflon-lined hydrothermal reaction kettle, at 220 ℃ of reaction 2h.After hydro-thermal reaction finished, throw out was filtered in cooling, and it is inferior respectively to give a baby a bath on the third day after its birth with distilled water and dehydrated alcohol successively, and dry 4h makes nano-calcium carbonate hydrogen nickel in 60 ℃ vacuum drying oven then.
Embodiment 16
With 1.454g (0.005mol) Ni (NO
3)
26H
2O and 11.21g (0.08mol) urotropine is dissolved in the 40mL distilled water, stirs 10min and obtains green clear liquor, gained solution is transferred in the 50mL teflon-lined hydrothermal reaction kettle, at 240 ℃ of reaction 1h.After hydro-thermal reaction finished, throw out was filtered in cooling, and it is inferior respectively to give a baby a bath on the third day after its birth with distilled water and dehydrated alcohol successively, and dry 4h makes nano-calcium carbonate hydrogen nickel in 60 ℃ vacuum drying oven then.
Claims (5)
1. a method for preparing nano-calcium carbonate hydrogen nickel is characterized in that it comprises the steps:
Step 1. is dissolved in water urea or urotropine, adds nickel salt or nickel hydroxide, stirs, and urea or urotropine are 1:1 ~ 16:1 with the ratio of the amount of substance of nickel, and the concentration of nickel salt is 0.1 ~ 1.0mol/L in the solution;
The solution that step 2. obtains step 1 is transferred in the hydrothermal reaction kettle,, cools off after 1 ~ 6 hour in reaction under 90 ~ 240 ℃;
Step 3. is filtered the reaction mixture that step 2 obtains, and uses distilled water and absolute ethanol washing again, and places 60 ℃ vacuum drying oven dry, makes the cubic-phase nano hydrogen-carbonate nickel square about 100nm.
2. the method for preparing nano-calcium carbonate hydrogen nickel according to claim 1 is characterized in that: described nickel hydroxide is prepared as follows:
Nickel salt and sodium hydroxide or potassium hydroxide is dissolved in generates amorphous Ni (OH) in the distilled water
2Precipitation suspension, nickel salt is 1:1.2 ~ 1:2.0 with the ratio of the amount of substance of sodium hydroxide or potassium hydroxide, and the concentration of nickel salt solution is 0.1 ~ 1.0mol/L, and so, in the step 1, described urea or urotropine are 1:1 ~ 8:1 with the ratio of the amount of substance of nickel salt.
3. according to the described method for preparing nano-calcium carbonate hydrogen nickel of claim 1, it is characterized in that: in the step 1, the ratio of the amount of substance of described urea and nickel salt is 4:1 ~ 16:1, and the concentration of nickel salt solution is 0.1 ~ 2.0mol/L.
4. according to the above-mentioned method for preparing nano-calcium carbonate hydrogen nickel of claim, in the step 1, the ratio of the amount of substance of described urotropine and nickel salt is 1:1 ~ 16:1, and the concentration of nickel salt solution is 0.1 ~ 2.0mol/L.
5. according to claim 1 or the 2 described methods that prepare nano-calcium carbonate hydrogen nickel, described nickel salt can be hydrochloride, vitriol, nitrate, acetate and oxalate.
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|---|---|---|---|
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102423708A (en) * | 2011-08-12 | 2012-04-25 | 南京大学 | Nickel-based composite nanomaterial and preparation method thereof as well as porous nickel nanomaterial and preparation method and application thereof |
| CN103647072A (en) * | 2013-12-25 | 2014-03-19 | 南京师范大学 | Preparation method of nitrogen-doped carbon wrapping layer with adjustable carbon/nitrogen content ratio on surface of nickel oxide |
| CN103880093A (en) * | 2014-04-15 | 2014-06-25 | 山东大学 | Hollow spherical nickel bicarbonate aggregate |
| CN105481026A (en) * | 2015-12-17 | 2016-04-13 | 宁波繁盛商业管理有限公司 | Preparation method of nickel bicarbonate |
| CN107331538A (en) * | 2017-08-07 | 2017-11-07 | 云南大学 | A kind of preparation method of nano nickel bicarbonate composite carbon electrode material |
| CN107394177A (en) * | 2017-08-02 | 2017-11-24 | 中国石油大学(华东) | A kind of sodium-ion battery negative pole bicarbonate nickel/graphene composite material and preparation method and application |
| CN107622876A (en) * | 2017-08-01 | 2018-01-23 | 大连理工大学 | A kind of bicarbonate nickel copper nickel oxide electrode material and preparation method thereof |
| CN107640761A (en) * | 2017-10-13 | 2018-01-30 | 郑州大学 | The preparation method and stored energy application of graphene/carbon acid hydrogen nickel nanocube three-dimensional composite material |
| CN108364798A (en) * | 2018-01-04 | 2018-08-03 | 同济大学 | Spongy C/Ni (the HCO in sea3)2- Ni composite material and preparation methods |
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-
2010
- 2010-10-26 CN CN201010518911.5A patent/CN101962211B/en not_active Expired - Fee Related
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102423708A (en) * | 2011-08-12 | 2012-04-25 | 南京大学 | Nickel-based composite nanomaterial and preparation method thereof as well as porous nickel nanomaterial and preparation method and application thereof |
| CN103647072A (en) * | 2013-12-25 | 2014-03-19 | 南京师范大学 | Preparation method of nitrogen-doped carbon wrapping layer with adjustable carbon/nitrogen content ratio on surface of nickel oxide |
| CN103647072B (en) * | 2013-12-25 | 2015-12-30 | 南京师范大学 | A kind of nickel oxide surfaces carbon/nitrogen content is than the preparation method of adjustable nitrogen-doped carbon integument |
| CN103880093A (en) * | 2014-04-15 | 2014-06-25 | 山东大学 | Hollow spherical nickel bicarbonate aggregate |
| CN103880093B (en) * | 2014-04-15 | 2015-03-11 | 山东大学 | Hollow spherical nickel bicarbonate aggregate |
| CN105481026A (en) * | 2015-12-17 | 2016-04-13 | 宁波繁盛商业管理有限公司 | Preparation method of nickel bicarbonate |
| CN107622876A (en) * | 2017-08-01 | 2018-01-23 | 大连理工大学 | A kind of bicarbonate nickel copper nickel oxide electrode material and preparation method thereof |
| CN107394177A (en) * | 2017-08-02 | 2017-11-24 | 中国石油大学(华东) | A kind of sodium-ion battery negative pole bicarbonate nickel/graphene composite material and preparation method and application |
| CN107331538A (en) * | 2017-08-07 | 2017-11-07 | 云南大学 | A kind of preparation method of nano nickel bicarbonate composite carbon electrode material |
| CN107640761A (en) * | 2017-10-13 | 2018-01-30 | 郑州大学 | The preparation method and stored energy application of graphene/carbon acid hydrogen nickel nanocube three-dimensional composite material |
| CN107640761B (en) * | 2017-10-13 | 2019-11-29 | 郑州大学 | The preparation method and stored energy application of graphene/carbon acid hydrogen nickel nanocube three-dimensional composite material |
| CN108364798A (en) * | 2018-01-04 | 2018-08-03 | 同济大学 | Spongy C/Ni (the HCO in sea3)2- Ni composite material and preparation methods |
| CN115970698A (en) * | 2022-06-15 | 2023-04-18 | 湘潭大学 | Preparation of nickel-iron-calcium catalyst for treating wastewater containing metal complex |
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