CN101654278A - Method for synthesizing indium hydroxide nano block - Google Patents
Method for synthesizing indium hydroxide nano block Download PDFInfo
- Publication number
- CN101654278A CN101654278A CN200910091566A CN200910091566A CN101654278A CN 101654278 A CN101654278 A CN 101654278A CN 200910091566 A CN200910091566 A CN 200910091566A CN 200910091566 A CN200910091566 A CN 200910091566A CN 101654278 A CN101654278 A CN 101654278A
- Authority
- CN
- China
- Prior art keywords
- proline
- indium
- indium hydroxide
- nano block
- milliliter
- 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.)
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Links
- IGUXCTSQIGAGSV-UHFFFAOYSA-K indium(iii) hydroxide Chemical compound [OH-].[OH-].[OH-].[In+3] IGUXCTSQIGAGSV-UHFFFAOYSA-K 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 8
- 230000002194 synthesizing effect Effects 0.000 title abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 126
- ONIBWKKTOPOVIA-UHFFFAOYSA-N Proline Natural products OC(=O)C1CCCN1 ONIBWKKTOPOVIA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 21
- 239000000243 solution Substances 0.000 claims abstract description 18
- XURCIPRUUASYLR-UHFFFAOYSA-N Omeprazole sulfide Chemical compound N=1C2=CC(OC)=CC=C2NC=1SCC1=NC=C(C)C(OC)=C1C XURCIPRUUASYLR-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000007864 aqueous solution Substances 0.000 claims abstract description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 9
- 239000010935 stainless steel Substances 0.000 claims abstract description 9
- 238000010189 synthetic method Methods 0.000 claims abstract description 8
- ONIBWKKTOPOVIA-BYPYZUCNSA-N L-Proline Chemical compound OC(=O)[C@@H]1CCCN1 ONIBWKKTOPOVIA-BYPYZUCNSA-N 0.000 claims description 38
- 239000007788 liquid Substances 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- UVLYPUPIDJLUCM-UHFFFAOYSA-N indium;hydrate Chemical compound O.[In] UVLYPUPIDJLUCM-UHFFFAOYSA-N 0.000 claims description 8
- 239000000463 material Substances 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract 2
- 238000003786 synthesis reaction Methods 0.000 abstract 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract 1
- 229910002651 NO3 Inorganic materials 0.000 abstract 1
- 238000005260 corrosion Methods 0.000 abstract 1
- 230000007797 corrosion Effects 0.000 abstract 1
- 230000002401 inhibitory effect Effects 0.000 abstract 1
- 229910052748 manganese Inorganic materials 0.000 abstract 1
- 239000011572 manganese Substances 0.000 abstract 1
- -1 polytetrafluoroethylene Polymers 0.000 abstract 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 abstract 1
- 239000004810 polytetrafluoroethylene Substances 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 description 12
- 230000005540 biological transmission Effects 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 6
- 229940105847 calamine Drugs 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 229910052864 hemimorphite Inorganic materials 0.000 description 2
- 230000005764 inhibitory process Effects 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 235000014692 zinc oxide Nutrition 0.000 description 2
- 239000011787 zinc oxide Substances 0.000 description 2
- CPYIZQLXMGRKSW-UHFFFAOYSA-N zinc;iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Fe+3].[Fe+3].[Zn+2] CPYIZQLXMGRKSW-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- AMGQUBHHOARCQH-UHFFFAOYSA-N indium;oxotin Chemical compound [In].[Sn]=O AMGQUBHHOARCQH-UHFFFAOYSA-N 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011236 particulate material Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
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Abstract
The invention relates to a method for synthesizing an indium hydroxide nano block, belonging to the technical field of mercury-substituting corrosion-inhibiting materials for alkaline manganese batteries. The method takes hydrated indium nitrate [In(NO3)3.4.5H2O], proline (1-proline, C5H9NO2) and sodium hydroxide (NaOH) as raw materials and prepares aqueous solution containing the three raw materials as initial reaction solution at room temperature, placing the initial reaction solution in a stainless steel reaction kettle with a polytetrafluoroethylene liner to be heated at 180-240 DEG C for24-96h, thus obtaining the indium hydroxide nano block. Synthesis of the indium hydroxide nano block by the method is realized by employing the proline, a biomolecule, as one of the raw materials to participate in the reaction. The method provides a new synthetic method and a new material for researching the properties and practical purposes of the indium hydroxide nanocrystalline. Synthesis of the indium hydroxide nano block has great significance in both academic research and application.
Description
Technical field
The present invention relates to a kind of synthetic method of indium hydroxide nano block, belong to alkaline Mn cell for mercury inhibition material technology field.
Background technology
Indium hydroxide is to be widely used in tinted shade, pottery, alkaline Mn cell for traditional field such as mercury inhibition Liu, chemical reagent.Be widely used in high-technology field and military fields such as photoelectricity industry in recent years, be specially adapted to be processed as indium tin oxide (ITO) target, make transparency electrode and transparent heat reflection body material, being used for production flat liquid crystal display and demist ice device, is one of research focus of current information high-tech area.Therefore, no matter synthesize indium hydroxide nano block in academic research or in application facet, all significant.
By retrieval, 1 patent report about indium hydroxide is arranged in the prior art:
(1) " the nanometer indium hydroxide is used to produce the technology of alkaline cell " (applicant: Wuhan Dagong High-Energy Power Supply Co. Ltd., contriver: Jin Baitao; Qi Lin; Application number: 01133675.7), a kind of technology that the nanometer indium hydroxide is used to produce alkaline cell of this invention report mainly is over-all properties and the period of storage in order to improve alkaline cell.It mainly is when making the negative material calamine cream, and the nanometer indium hydroxide is added in it as additive.Because the nanometer indium hydroxide is a kind of ultrafine particulate material, makes its calamine cream morphology of particles that variation take place, the electrochemical reaction in it is more abundant, thereby has improved the over-all properties and the period of storage of alkaline cell.
Its crystal shape, size, pattern, degree of crystallinity, thermostability, solvability are depended in the application of indium hydroxide, and these all depend on the selection of its synthetic method.The synthetic biomolecules of utilizing---amino acid---proline(Pro) of the indium hydroxide nano block of this patent report is that one of raw material participates in the reaction realization.This character and practical use for the research indium hydroxide nano block provides new synthetic method and novel material.No matter in academic research still in application facet, all have great importance.
Summary of the invention
The object of the present invention is to provide a kind of hydrothermal synthesis method of easy preparation indium hydroxide nano block.Raw materials used being easy to get in the synthetic method of the present invention, technology is easy.
The synthetic method of a kind of indium hydroxide nano block that the present invention proposes is characterized in that this method carries out as follows:
(1) with nitric hydrate indium [In (NO
3)
34.5H
2O], proline(Pro) (l-Proline, C
5H
9NO
2), sodium hydroxide (NaOH) is raw material, at room temperature, preparation comprises indium nitrate [In (NO
3)
34.5H
2O], proline(Pro) (l-Proline, C
5H
9NO
2), the aqueous solution of sodium hydroxide (NaOH), as reaction starting liquid, wherein the indium nitrate concentration range is 1～2 mmole/40 milliliter, the concentration of proline scope is 2～8 mmoles/40 milliliter, reaches 40 milliliters and make the pH value of solution reach 8 with the sodium hydroxide x milliliter regulator solution volume of dropper Dropwise 5 M or 10M;
(2) this reaction starting liquid is placed in the teflon-lined stainless steel cauldron, under 180-240 ℃ of temperature, heated 24～96 hours;
(3) give a baby a bath on the third day after its birth time with dehydrated alcohol again after the throw out that obtains after will reacting is washed once with deionized water, put into loft drier (60 ℃) then and carried out drying 7 hours, promptly obtain indium hydroxide nano block.
Description of drawings
Fig. 1 (a) is the transmission electron microscope photo of embodiment 1, and Fig. 1 (b) is the x-ray diffraction pattern of embodiment 1.
Fig. 2 (a) is the transmission electron microscope photo of embodiment 2, and Fig. 2 (b) is the x-ray diffraction pattern of embodiment 2.
Fig. 3 (a) is the transmission electron microscope photo of embodiment 3, and Fig. 3 (b) is the x-ray diffraction pattern of embodiment 3.
Fig. 4 (a) is the transmission electron microscope photo of embodiment 4, and Fig. 4 (b) is the x-ray diffraction pattern of embodiment 4.
Fig. 5 (a) is the transmission electron microscope photo of embodiment 5, and Fig. 5 (b) is the x-ray diffraction pattern of embodiment 5.
Fig. 6 (a) is the transmission electron microscope photo of embodiment 6, and Fig. 6 (b) is the x-ray diffraction pattern of embodiment 6.
Embodiment
Below by specific embodiment the present invention further is illustrated.
Embodiment 1:
---with nitric hydrate indium [In (NO
3)
34.5H
2O], proline(Pro) (l-Proline, C
5H
9NO
2), sodium hydroxide (NaOH) is raw material, at room temperature, preparation comprises indium nitrate [In (NO
3)
34.5H
2O], proline(Pro) (l-Proline, C
5H
9NO
2), the aqueous solution of sodium hydroxide (NaOH), as reaction starting liquid, wherein indium nitrate is 1 mmole/40 milliliter, and concentration of proline is 2 mmoles/40 milliliter, reaches 40 milliliters and make the pH value of solution reach 8 with 0.6 milliliter of regulator solution volume of sodium hydroxide of dropper Dropwise 5 M.
---this reaction starting liquid is placed in the teflon-lined stainless steel cauldron, and heating is 24 hours under 180 ℃ of temperature.
---give a baby a bath on the third day after its birth time with dehydrated alcohol again after the throw out that obtain after will reacting is washed once with deionized water, put into loft drier (60 ℃) then and carried out drying 7 hours, promptly obtain indium hydroxide nano block.Fig. 1 (a) is the transmission electron microscope photo of embodiment 1, by visible its nanometer piece of Fig. 1 (a).Fig. 1 (b) is an x-ray diffraction pattern, determines that product is an indium hydroxide.
Embodiment 2:
---with nitric hydrate indium [In (NO
3)
34.5H
2O], proline(Pro) (l-Proline, C
5H
9NO
2), sodium hydroxide (NaOH) is raw material, at room temperature, preparation comprises indium nitrate [In (NO
3)
34.5H
2O], proline(Pro) (l-Proline, C
5H
9NO
2), the aqueous solution of sodium hydroxide (NaOH), as reaction starting liquid, wherein indium nitrate is 1 mmole/40 milliliter, and concentration of proline is 2 mmoles/40 milliliter, reaches 40 milliliters and make the pH value of solution reach 8 with 0.6 milliliter of regulator solution volume of sodium hydroxide of dropper Dropwise 5 M.
---this reaction starting liquid is placed in the teflon-lined stainless steel cauldron, and heating is 24 hours under 210 ℃ of temperature.
---give a baby a bath on the third day after its birth time with dehydrated alcohol again after the throw out that obtain after will reacting is washed once with deionized water, put into loft drier (60 ℃) then and carried out drying 7 hours, promptly obtain indium hydroxide nano block.Fig. 2 (a) is the transmission electron microscope photo of embodiment 2, by visible its nanometer piece of Fig. 2 (a).Fig. 2 (b) is an x-ray diffraction pattern, determines that product is an indium hydroxide.
Embodiment 3:
---with nitric hydrate indium [In (NO
3)
34.5H
2O], proline(Pro) (l-Proline, C
5H
9NO
2), sodium hydroxide (NaOH) is raw material, at room temperature, preparation comprises indium nitrate [In (NO
3)
34.5H
2O], proline(Pro) (l-Proline, C
5H
9NO
2), the aqueous solution of sodium hydroxide (NaOH), as reaction starting liquid, wherein indium nitrate is 1 mmole/40 milliliter, and concentration of proline is 2 mmoles/40 milliliter, reaches 40 milliliters and make the pH value of solution reach 8 with 0.6 milliliter of regulator solution volume of sodium hydroxide of dropper Dropwise 5 M.
---this reaction starting liquid is placed in the teflon-lined stainless steel cauldron, and heating is 48 hours under 210 ℃ of temperature.
---give a baby a bath on the third day after its birth time with dehydrated alcohol again after the throw out that obtain after will reacting is washed once with deionized water, put into loft drier (60 ℃) then and carried out drying 7 hours, promptly obtain indium hydroxide nano block.Fig. 3 (a) is the transmission electron microscope photo of embodiment 3, by visible its nanometer piece of Fig. 3 (a).Fig. 3 (b) is an x-ray diffraction pattern, determines that product is an indium hydroxide.
Embodiment 4:10#
---with nitric hydrate indium [In (NO
3)
34.5H
2O], proline(Pro) (l-Proline, C
5H
9NO
2), sodium hydroxide (NaOH) is raw material, at room temperature, preparation comprises indium nitrate [In (NO
3)
34.5H
2O], proline(Pro) (l-Proline, C
5H
9NO
2), the aqueous solution of sodium hydroxide (NaOH), as reaction starting liquid, wherein indium nitrate is 1 mmole/40 milliliter, and concentration of proline is 2 mmoles/40 milliliter, reaches 40 milliliters and make the pH value of solution reach 8 with 0.6 milliliter of regulator solution volume of sodium hydroxide of dropper Dropwise 5 M.
---this reaction starting liquid is placed in the teflon-lined stainless steel cauldron, and heating is 96 hours under 210 ℃ of temperature.
---give a baby a bath on the third day after its birth time with dehydrated alcohol again after the throw out that obtain after will reacting is washed once with deionized water, put into loft drier (60 ℃) then and carried out drying 7 hours, promptly obtain indium hydroxide nano block.Fig. 4 (a) is the transmission electron microscope photo of embodiment 4, by visible its nanometer piece of Fig. 4 (a).Fig. 4 (b) is an x-ray diffraction pattern, determines that product is an indium hydroxide.
Embodiment 5:
---with nitric hydrate indium [In (NO
3)
34.5H
2O], proline(Pro) (l-Proline, C
5H
9NO
2), sodium hydroxide (NaOH) is raw material, at room temperature, preparation comprises indium nitrate [In (NO
3)
34.5H
2O], proline(Pro) (l-Proline, C
5H
9NO
2), the aqueous solution of sodium hydroxide (NaOH), as reaction starting liquid, wherein indium nitrate is 1 mmole/40 milliliter, and concentration of proline is 8 mmoles/40 milliliter, and the 0.35 milliliter of regulator solution volume of sodium hydroxide that drips 10M with dropper reaches 40 milliliters and make the pH value of solution reach 8.
---this reaction starting liquid is placed in the teflon-lined stainless steel cauldron, and heating is 24 hours under 210 ℃ of temperature.
---give a baby a bath on the third day after its birth time with dehydrated alcohol again after the throw out that obtain after will reacting is washed once with deionized water, put into loft drier (60 ℃) then and carried out drying 7 hours, promptly obtain indium hydroxide nano block.Fig. 5 (a) is the transmission electron microscope photo of embodiment 5, by visible its nanometer piece of Fig. 5 (a).Fig. 5 (b) is an x-ray diffraction pattern, determines that product is an indium hydroxide.
Embodiment 6:12#
---with nitric hydrate indium [In (NO
3)
34.5H
2O], proline(Pro) (l-Proline, C
5H
9NO
2), sodium hydroxide (NaOH) is raw material, at room temperature, preparation comprises indium nitrate [In (NO
3)
34.5H
2O], proline(Pro) (l-Proline, C
5H
9NO
2), the aqueous solution of sodium hydroxide (NaOH), as reaction starting liquid, wherein indium nitrate is 1 mmole/40 milliliter, and concentration of proline is 4 mmoles/40 milliliter, and the 0.35 milliliter of regulator solution volume of sodium hydroxide that drips 10M with dropper reaches 40 milliliters and make the pH value of solution reach 8.
---this reaction starting liquid is placed in the teflon-lined stainless steel cauldron, and heating is 24 hours under 240 ℃ of temperature.
---give a baby a bath on the third day after its birth time with dehydrated alcohol again after the throw out that obtain after will reacting is washed once with deionized water, put into loft drier (60 ℃) then and carried out drying 7 hours, promptly obtain indium hydroxide nano block.Fig. 6 (a) is the transmission electron microscope photo of embodiment 6, by visible its nanometer piece of Fig. 6 (a).Fig. 6 (b) is an x-ray diffraction pattern, determines that product is an indium hydroxide.
Claims (1)
1, a kind of synthetic method of indium hydroxide nano block is characterized in that this method carries out as follows:
(1) with nitric hydrate indium [In (NO
3)
34.5H
2O], proline(Pro) (1-Proline, C
5H
9NO
2), sodium hydroxide (NaOH) is raw material, at room temperature, preparation comprises indium nitrate [In (NO
3)
34.5H
2O], proline(Pro) (1-Proline, C
5H
9NO
2), the aqueous solution of sodium hydroxide (NaOH), as reaction starting liquid, wherein the indium nitrate concentration range is 1～2 mmole/40 milliliter, the concentration of proline scope is 2～8 mmoles/40 milliliter, reaches 40 milliliters and make the pH value of solution reach 8 with the sodium hydroxide x milliliter regulator solution volume of dropper Dropwise 5 M or 10M;
(2) this reaction starting liquid is placed in the teflon-lined stainless steel cauldron, under 180-240 ℃ of temperature, heated 24～96 hours;
(3) give a baby a bath on the third day after its birth time with dehydrated alcohol again after the throw out that obtains after will reacting is washed once with deionized water, put into loft drier (60 ℃) then and carried out drying 7 hours, promptly obtain indium hydroxide nano block.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100915669A CN101654278B (en) | 2009-08-28 | 2009-08-28 | Method for synthesizing indium hydroxide nano block |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100915669A CN101654278B (en) | 2009-08-28 | 2009-08-28 | Method for synthesizing indium hydroxide nano block |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101654278A true CN101654278A (en) | 2010-02-24 |
| CN101654278B CN101654278B (en) | 2011-08-17 |
Family
ID=41708773
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100915669A Expired - Fee Related CN101654278B (en) | 2009-08-28 | 2009-08-28 | Method for synthesizing indium hydroxide nano block |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101654278B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807250A (en) * | 2012-07-26 | 2012-12-05 | 荣成百合生物技术有限公司 | Method for synthesizing indium hydroxide millimeter or submillimeter block |
| CN106732517A (en) * | 2016-11-28 | 2017-05-31 | 青岛科技大学 | A kind of preparation method of the indium hydroxide photochemical catalyst with regular cube structure |
| CN110952107A (en) * | 2019-12-19 | 2020-04-03 | 西南科技大学 | Method for extracting uranium from seawater by using metal oxide containing oxygen vacancy |
| CN111004934A (en) * | 2019-12-19 | 2020-04-14 | 西南科技大学 | Method for extracting uranium by using coupling device of wind power generation and uranium extraction from seawater |
-
2009
- 2009-08-28 CN CN2009100915669A patent/CN101654278B/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102807250A (en) * | 2012-07-26 | 2012-12-05 | 荣成百合生物技术有限公司 | Method for synthesizing indium hydroxide millimeter or submillimeter block |
| CN106732517A (en) * | 2016-11-28 | 2017-05-31 | 青岛科技大学 | A kind of preparation method of the indium hydroxide photochemical catalyst with regular cube structure |
| CN110952107A (en) * | 2019-12-19 | 2020-04-03 | 西南科技大学 | Method for extracting uranium from seawater by using metal oxide containing oxygen vacancy |
| CN111004934A (en) * | 2019-12-19 | 2020-04-14 | 西南科技大学 | Method for extracting uranium by using coupling device of wind power generation and uranium extraction from seawater |
| CN111004934B (en) * | 2019-12-19 | 2021-03-23 | 西南科技大学 | Method for extracting uranium by using coupling device of wind power generation and uranium extraction from seawater |
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| Publication number | Publication date |
|---|---|
| CN101654278B (en) | 2011-08-17 |
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