CN103043702A - Method for grinding and preparing nano-cuprous oxide - Google Patents
Method for grinding and preparing nano-cuprous oxide Download PDFInfo
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- CN103043702A CN103043702A CN2012105361577A CN201210536157A CN103043702A CN 103043702 A CN103043702 A CN 103043702A CN 2012105361577 A CN2012105361577 A CN 2012105361577A CN 201210536157 A CN201210536157 A CN 201210536157A CN 103043702 A CN103043702 A CN 103043702A
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- cuprous oxide
- nano cuprous
- mantoquita
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Abstract
The invention relates to a grinding and preparing nano-cuprous oxide, comprising the following steps: (1) uniformly stirring a copper salt, a reducing agent and dimethyl sulfoxide in a temperature range of 10-70 DEG C, and grinding for 0.2-0.6h; and (2) repeatedly washing the ground mixture with deionized water, ethanol and acetone for several times, to obtain stabilized nano-cuprous oxide. The beneficial effects of the method are that: (1) purer nan0-cuprous oxide particles can be prepared; (2) the copper salt amount in each reaction process is not limited without solubility, (3) the method has the advantages of simple technology, simple operation, mild reaction, short reaction time, high efficiency and large scale production; the product has good performances, the particle size particle size of the prepared nano-cuprous oxide is less than 20nm, and the nano-cuprous oxide has good secondary dispersibility in various oils; and the method is low in preparation cost and energy consumption, generates no harmful waste, and accords with the production requirement of green production, environmental protection and energy saving.
Description
Technical field
The present invention relates to the Inorganic Chemicals production field, especially a kind of grinding production method of nano cuprous oxide.
Background technology
Red copper oxide (Cu
2O) be the p-type semiconductor material, of many uses.Except in organic synthesis, can be used as the catalyzer use, also can be used as boats and ships protective system and sterilant, more be applied to pottery and electron device aspect.Because quantum size effect, grade cuprous oxide has special optics, electricity and PhotoelectrochemicalProperties Properties, at aspects such as solar cell, sensor, superconductor, hydrogen manufacturing and electrochromism potential application is arranged, nano cuprous oxide also can be processed organic pollutant in environment, therefore studying the method for preparing nano cuprous oxide just becomes one of current study hotspot.
Disclose a kind of preparation method of nano cuprous oxide among Chinese patent CN 1693204 A, step is as follows: 1) add mantoquita, polyvinylpyrrolidone and sodium lauryl sulphate in deionized water; 2) add hydrazine hydrate aqueous solution, regulate pH value, add simultaneously paraffin or lubricating oil, stir ageing; 3) centrifugation; 4) clean.Its shortcoming is: contained prescription is more in the system, need to add organic protective agent, thereby the purity of final nano cuprous oxide particle is not high.
Disclose a kind of preparation method of nano cuprous oxide among Chinese patent CN 102167388 A, step is as follows: 1) mantoquita and organic protective agent are dissolved in the solvent, are warming up to gradually 70 ℃ of 20 –; 2) behind the temperature-stable reductive agent is added in the reaction system, continue afterwards after stirring reaction 20-30 minute, gradually cooling; 3) centrifugation; 4) clean.Its shortcoming is: the amount of the mantoquita that adds is subjected to its solubility limit in employed solvent.
Summary of the invention
The present invention will solve the shortcoming of above-mentioned prior art, provides that a kind of technique is simple, the grinding production method of energy-conserving and environment-protective, nano cuprous oxide that gained nano cuprous oxide particle purity is higher.
The present invention solves the technical scheme that its technical problem adopts: a kind of grinding production method of nano cuprous oxide may further comprise the steps: 1) mantoquita, reductive agent and dimethyl sulfoxide (DMSO) are stirred under 10-70 ℃ temperature, and the 0.2-6h that mills;
2) mixture after will milling is used deionized water, ethanol and acetone repetitive scrubbing several times successively, can obtain stable nano cuprous oxide.
As preferably, reductive agent is one or more in formaldehyde, V-Brite B, hydroborate and the hydrazine hydrate.
As preferably, the mol ratio of reductive agent and mantoquita is 1-10:1, and the ratio of dimethyl sulfoxide (DMSO) and mantoquita is 1-100ml:10g.
As preferably, mantoquita is one or several of the title complex of copper sulfate, cupric nitrate, cupric chloride, neutralized verdigris, copper and the organic copper that comprises long-chain, and wherein the carbon chain lengths of organic copper is 8-16.
As preferably, the technique of milling of step 1) is mechanical disruption or manual milling.
The grinding production method of another kind of nano cuprous oxide may further comprise the steps: 1) mantoquita, reductive agent, acid and dimethyl sulfoxide (DMSO) stirred under 10-70 ℃ temperature, and the 0.2-6h that mills;
2) mixture after will milling is used deionized water, ethanol and acetone repetitive scrubbing several times successively, can obtain stable nano cuprous oxide.
As preferably, reductive agent is one or several in hypophosphite, xitix, glucose, S-WAT, formic acid, trolamine, ethylene glycol, sorbyl alcohol, Xylitol and the oxammonium hydrochloride.
As preferably, the mol ratio of reductive agent and mantoquita is 1-10:1, and the ratio of acid and mantoquita is 1-20ml:100g, and the ratio of dimethyl sulfoxide (DMSO) and mantoquita is 1-100ml:10g.
As preferably, mantoquita is one or several of the title complex of copper sulfate, cupric nitrate, cupric chloride, neutralized verdigris, copper and the organic copper that comprises long-chain, and wherein the carbon chain lengths of organic copper is 8-16.
As preferably, acid is one or more in sulfuric acid, hydrochloric acid, nitric acid, acetic acid, phosphoric acid, formic acid and the oxalic acid; The technique of milling of step 1) can be mechanical disruption, also can be manual milling.
The effect that the present invention is useful is: (reductive agent is one or more in formaldehyde, V-Brite B, hydroborate and the hydrazine hydrate one, only to adopt mantoquita, reductive agent, acid in the preparation process, then need not acid adding) and four kinds of prescriptions of dimethyl sulfoxide (DMSO), wherein acid plays katalysis, can reduce temperature of reaction, can also suppress in addition the generation of copper hydroxide, to make the higher nano cuprous oxide particle of purity; Two, dimethyl sulfoxide (DMSO) (DMSO) is as protective material, and consumption seldom only needs get final product the particle of reductive agent and mantoquita is moistening, and do not require that mantoquita is dissolved among the DMSO, so the amount of every secondary response mantoquita that can hold is not subjected to the restriction of solubleness; Three, technique of the present invention is simple, and is easy and simple to handle, reaction temperature and, the reaction times is short, efficient is high, is fit to scale operation; Product performance are good, and the particle diameter of the nano cuprous oxide for preparing has good twice dispersing less than 20nm in all kinds of finishes; Preparation cost is low, and energy consumption is low, does not have bazardous waste to produce, and meets the modern production requirement of " green production, environmental protection and energy saving ".
Embodiment
Embodiment 1: 20g cupric sulfate pentahydrate, 80g inferior sodium phosphate, 20ml dimethyl sulfoxide (DMSO) and 2ml sulfuric acid are joined in the mortar, under 10 ℃ temperature, stir, and hand lapping 50 minutes, then use deionized water, ethanol and acetone repetitive scrubbing are more than three times, namely obtain the purity height, good stability, the nano cuprous oxide that oil soluble is good.
Embodiment 2: 15g cupric chloride, 8g sodium borohydride and 20ml dimethyl sulfoxide (DMSO) are joined in the mortar, under 70 ℃ temperature, stir, and employing mechanical mill 20min, then use deionized water, ethanol and acetone repetitive scrubbing are more than three times, namely obtain the purity height, good stability, the nano cuprous oxide that oil soluble is good.
Embodiment 3: 30g cupric sulfate pentahydrate, 100g xitix, 30ml dimethyl sulfoxide (DMSO) and 2ml formic acid are joined in the mortar, under 40 ℃ temperature, stir, and employing mechanical mill 50min, then use deionized water, ethanol and acetone repetitive scrubbing are more than three times, namely obtain the purity height, good stability, the nano cuprous oxide that oil soluble is good.
Embodiment 4: 12g cupric nitrate, 25g S-WAT (seven water), 10ml dimethyl sulfoxide (DMSO) and 2ml nitric acid are joined in the mortar, under 50 ℃ temperature, stir, and employing mechanical mill 30min, then use deionized water, ethanol and acetone repetitive scrubbing are more than three times, namely obtain the purity height, good stability, the nano cuprous oxide that oil soluble is good.
Embodiment 5: 16g cupric sulfate pentahydrate, 15g formic acid, 20ml dimethyl sulfoxide (DMSO) and 2ml formic acid are joined in the mortar, under 30 ℃ temperature, stir, and employing mechanical mill 40min, then use deionized water, ethanol and acetone repetitive scrubbing are more than three times, namely obtain the purity height, good stability, the nano cuprous oxide that oil soluble is good.
Embodiment 6: 12g neutralized verdigris (water), 10g trolamine, 20ml dimethyl sulfoxide (DMSO) and 2ml acetic acid are joined in the mortar, under 35 ℃ temperature, stir, and ground 6 hours, then use deionized water, ethanol and acetone repetitive scrubbing are more than three times, namely obtain the purity height, good stability, the nano cuprous oxide that oil soluble is good.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.
Claims (10)
1. the grinding production method of a nano cuprous oxide is characterized in that:
1) mantoquita, reductive agent and dimethyl sulfoxide (DMSO) are stirred under 10-70 ℃ temperature, and the 0.2-6h that mills;
2) mixture after will milling is used deionized water, ethanol and acetone repetitive scrubbing several times successively, can obtain stable nano cuprous oxide.
2. the grinding production method of nano cuprous oxide according to claim 1, it is characterized in that: described reductive agent is one or more in formaldehyde, V-Brite B, hydroborate and the hydrazine hydrate.
3. the grinding production method of nano cuprous oxide according to claim 1 and 2, it is characterized in that: the mol ratio of described reductive agent and mantoquita is 1-10:1, the ratio of dimethyl sulfoxide (DMSO) and mantoquita is 1-100ml:10g.
4. the grinding production method of nano cuprous oxide according to claim 1 and 2, it is characterized in that: described mantoquita is one or several of the title complex of copper sulfate, cupric nitrate, cupric chloride, neutralized verdigris, copper and the organic copper that comprises long-chain, and wherein the carbon chain lengths of organic copper is 8-16.
5. the grinding production method of nano cuprous oxide according to claim 1 and 2 is characterized in that: the technique of milling of described step 1) is mechanical disruption or manual milling.
6. the grinding production method of a nano cuprous oxide is characterized in that:
1) mantoquita, reductive agent, acid and dimethyl sulfoxide (DMSO) are stirred under 10-70 ℃ temperature, and the 0.2-6h that mills;
2) mixture after will milling is used deionized water, ethanol and acetone repetitive scrubbing several times successively, can obtain stable nano cuprous oxide.
7. the grinding production method of nano cuprous oxide according to claim 6, it is characterized in that: described reductive agent is one or several in hypophosphite, xitix, glucose, S-WAT, formic acid, trolamine, ethylene glycol, sorbyl alcohol, Xylitol and the oxammonium hydrochloride.
8. according to claim 6 or the grinding production method of 7 described nano cuprous oxides, it is characterized in that: the mol ratio of described reductive agent and mantoquita is 1-10:1, and the ratio of acid and mantoquita is 1-20ml:100g, and the ratio of dimethyl sulfoxide (DMSO) and mantoquita is 1-100ml:10g.
9. according to claim 6 or the grinding production method of 7 described nano cuprous oxides, it is characterized in that: described mantoquita is one or several of the title complex of copper sulfate, cupric nitrate, cupric chloride, neutralized verdigris, copper and the organic copper that comprises long-chain, and wherein the carbon chain lengths of organic copper is 8-16.
10. according to claim 6 or the grinding production method of 7 described nano cuprous oxides, it is characterized in that: described acid is one or more in sulfuric acid, hydrochloric acid, nitric acid, acetic acid, phosphoric acid, formic acid and the oxalic acid; The technique of milling of step 1) is mechanical disruption or manual milling.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210536157.7A CN103043702B (en) | 2012-12-10 | 2012-12-10 | Method for grinding and preparing nano-cuprous oxide |
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| CN201210536157.7A CN103043702B (en) | 2012-12-10 | 2012-12-10 | Method for grinding and preparing nano-cuprous oxide |
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| CN103043702A true CN103043702A (en) | 2013-04-17 |
| CN103043702B CN103043702B (en) | 2015-01-21 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435090A (en) * | 2013-08-02 | 2013-12-11 | 浙江理工大学 | Grinding production method of nano cuprous chloride |
| CN105776310A (en) * | 2016-02-03 | 2016-07-20 | 常州市好利莱光电科技有限公司 | Method for preparing cuprous oxide |
| CN106115764A (en) * | 2016-06-23 | 2016-11-16 | 淮北师范大学 | The method that one pot of ball milling solid phase method prepares CuI nano-powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101778799A (en) * | 2007-07-25 | 2010-07-14 | Lg化学株式会社 | Spherical assembly particle composition of cuprous oxide and preparation method thereof |
| CN102167388A (en) * | 2010-02-26 | 2011-08-31 | 上海亿金纳米科技有限公司 | Novel and large-scale preparation method of nano-cuprous oxide |
| CN102390861A (en) * | 2011-08-17 | 2012-03-28 | 金川集团有限公司 | Method for preparing cuprous oxide powder |
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2012
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101778799A (en) * | 2007-07-25 | 2010-07-14 | Lg化学株式会社 | Spherical assembly particle composition of cuprous oxide and preparation method thereof |
| CN102167388A (en) * | 2010-02-26 | 2011-08-31 | 上海亿金纳米科技有限公司 | Novel and large-scale preparation method of nano-cuprous oxide |
| CN102390861A (en) * | 2011-08-17 | 2012-03-28 | 金川集团有限公司 | Method for preparing cuprous oxide powder |
Non-Patent Citations (1)
| Title |
|---|
| 钱红梅等: "纳米Cu2O粉体的室温固相合成及其光催化性能", 《半导体光电》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103435090A (en) * | 2013-08-02 | 2013-12-11 | 浙江理工大学 | Grinding production method of nano cuprous chloride |
| CN105776310A (en) * | 2016-02-03 | 2016-07-20 | 常州市好利莱光电科技有限公司 | Method for preparing cuprous oxide |
| CN106115764A (en) * | 2016-06-23 | 2016-11-16 | 淮北师范大学 | The method that one pot of ball milling solid phase method prepares CuI nano-powder |
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| CN103043702B (en) | 2015-01-21 |
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