CN103043702B - Method for grinding and preparing nano-cuprous oxide - Google Patents
Method for grinding and preparing nano-cuprous oxide Download PDFInfo
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- CN103043702B CN103043702B CN201210536157.7A CN201210536157A CN103043702B CN 103043702 B CN103043702 B CN 103043702B CN 201210536157 A CN201210536157 A CN 201210536157A CN 103043702 B CN103043702 B CN 103043702B
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- cuprous oxide
- mantoquita
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- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 229940112669 cuprous oxide Drugs 0.000 title claims abstract description 38
- 238000000227 grinding Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 12
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 70
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 238000004519 manufacturing process Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 5
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims description 32
- 230000002829 reductive effect Effects 0.000 claims description 17
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 15
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 14
- 239000010949 copper Substances 0.000 claims description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 12
- 229910052802 copper Inorganic materials 0.000 claims description 12
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims description 10
- 230000003252 repetitive effect Effects 0.000 claims description 10
- 238000005201 scrubbing Methods 0.000 claims description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
- 239000002253 acid Substances 0.000 claims description 9
- 238000003801 milling Methods 0.000 claims description 9
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 7
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 7
- 235000019253 formic acid Nutrition 0.000 claims description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- NWFNSTOSIVLCJA-UHFFFAOYSA-L copper;diacetate;hydrate Chemical compound O.[Cu+2].CC([O-])=O.CC([O-])=O NWFNSTOSIVLCJA-UHFFFAOYSA-L 0.000 claims description 5
- 229960003280 cupric chloride Drugs 0.000 claims description 5
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 4
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 235000011054 acetic acid Nutrition 0.000 claims description 3
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 claims description 3
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 3
- 229960004418 trolamine Drugs 0.000 claims description 3
- MEIRRNXMZYDVDW-MQQKCMAXSA-N (2E,4E)-2,4-hexadien-1-ol Chemical compound C\C=C\C=C\CO MEIRRNXMZYDVDW-MQQKCMAXSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 claims description 2
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 claims description 2
- 235000011007 phosphoric acid Nutrition 0.000 claims description 2
- 239000000811 xylitol Substances 0.000 claims description 2
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 claims description 2
- 229960002675 xylitol Drugs 0.000 claims description 2
- 235000010447 xylitol Nutrition 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 8
- 238000003756 stirring Methods 0.000 abstract description 8
- 239000003921 oil Substances 0.000 abstract description 7
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 150000001879 copper Chemical class 0.000 abstract 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000003638 chemical reducing agent Substances 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 229910000366 copper(II) sulfate Inorganic materials 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000003223 protective agent Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- JJLJMEJHUUYSSY-UHFFFAOYSA-L Copper hydroxide Chemical compound [OH-].[OH-].[Cu+2] JJLJMEJHUUYSSY-UHFFFAOYSA-L 0.000 description 1
- 239000005750 Copper hydroxide Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000005662 Paraffin oil Substances 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 239000004141 Sodium laurylsulphate Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910001956 copper hydroxide Inorganic materials 0.000 description 1
- LBJNMUFDOHXDFG-UHFFFAOYSA-N copper;hydrate Chemical compound O.[Cu].[Cu] LBJNMUFDOHXDFG-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002887 superconductor Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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 Inorganic Chemicals production field, especially a kind of grinding production method of nano cuprous oxide.
Background technology
Red copper oxide (Cu
2o) be p-type semiconductor material, of many uses.Except can be used as catalyzer and use in organic synthesis, also can be used as boats and ships protective system and sterilant, be more applied to pottery and electron device aspect.Due to quantum size effect, grade cuprous oxide has special optics, electricity and PhotoelectrochemicalProperties Properties, potential application is had in solar cell, sensor, superconductor, hydrogen manufacturing and electrochromism etc., nano cuprous oxide also can process organic pollutant in the environment, and the method that therefore nano cuprous oxide is prepared in research just becomes one of current study hotspot.
Disclose a kind of preparation method of nano cuprous oxide in Chinese patent CN 1693204 A, step is as follows: 1) add mantoquita in deionized water, polyvinylpyrrolidone and sodium lauryl sulphate; 2) add hydrazine hydrate aqueous solution, regulate pH value, add paraffin or lubricating oil simultaneously, stir ageing; 3) centrifugation; 4) clean.Its shortcoming is: in system, contained formula is more, needs to add organic protective agent, and thus the purity of final nano cuprous oxide particle is not high.
Disclose a kind of preparation method of nano cuprous oxide in Chinese patent CN 102167388 A, step is as follows: 1) be dissolved in solvent by mantoquita and organic protective agent, is warming up to 20 – 70 DEG C gradually; 2) add in reaction system by reductive agent after temperature-stable, Keep agitation reaction afterwards, after 20-30 minute, cools gradually; 3) centrifugation; 4) clean.Its shortcoming is: the amount of the mantoquita added limits by its solubleness in used solvent.
Summary of the invention
The present invention will solve the shortcoming of above-mentioned prior art, provide that a kind of technique is simple, energy-conserving and environment-protective, nano cuprous oxide that gained nano cuprous oxide particle purity is higher grinding production method.
The present invention solves the technical scheme that its technical problem adopts: a kind of grinding production method of nano cuprous oxide comprises the following steps: 1) mantoquita, reductive agent and dimethyl sulfoxide (DMSO) are stirred at the temperature of 10-70 DEG C, and the 0.2-6h that mills;
2) mixture after milling is used deionized water, ethanol and acetone repetitive scrubbing several times successively, stable nano cuprous oxide can be obtained.
As preferably, reductive agent is one or more in formaldehyde, V-Brite B, hydroborate and 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 copper sulfate, the title complex of cupric nitrate, cupric chloride, neutralized verdigris, copper and comprise one or several of organic copper of 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 mills by hand.
The grinding production method of another kind of nano cuprous oxide comprises the following steps: 1) mantoquita, reductive agent, acid and dimethyl sulfoxide (DMSO) are stirred at the temperature of 10-70 DEG C, and the 0.2-6h that mills;
2) mixture after milling is used deionized water, ethanol and acetone repetitive scrubbing several times successively, stable nano cuprous oxide can be obtained.
As preferably, reductive agent is one or several in hypophosphite, xitix, glucose, S-WAT, formic acid, trolamine, ethylene glycol, sorbyl alcohol, Xylitol and 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 copper sulfate, the title complex of cupric nitrate, cupric chloride, neutralized verdigris, copper and comprise one or several of organic copper of 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 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: one, only adopt mantoquita, reductive agent in preparation process, (reductive agent is one or more in formaldehyde, V-Brite B, hydroborate and hydrazine hydrate in acid, then without the need to acid adding) and dimethyl sulfoxide (DMSO) four kinds formula, wherein acid plays katalysis, temperature of reaction can be reduced, the generation of copper hydroxide can also be suppressed in addition, with the nano cuprous oxide particle that obtained purity is higher; Two, dimethyl sulfoxide (DMSO) (DMSO) is as protective material, and consumption is little, only needs moistening for the particle of reductive agent and mantoquita, and does not require that mantoquita is dissolved in DMSO, and the amount of mantoquita that therefore every secondary response can hold is not subject to the restriction of solubleness; Three, present invention process is simple, easy and simple to handle, reaction temperature and, the reaction times is short, and efficiency is high, is applicable to scale operation; Product performance are good, and the particle diameter of the nano cuprous oxide prepared is less than 20nm, in all kinds of finish, have good twice dispersing; The modern production requirement that preparation cost is low, and energy consumption is low, does not have bazardous waste to produce, meets " 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 mortar, stir at the temperature of 10 DEG C, and hand lapping 50 minutes, then deionized water is used, ethanol and acetone repetitive scrubbing more than three times, namely purity is obtained high, the nano cuprous oxide that good stability, oil soluble are good.
Embodiment 2: 15g cupric chloride, 8g sodium borohydride and 20ml dimethyl sulfoxide (DMSO) are joined in mortar, stir at the temperature of 70 DEG C, and adopt mechanical mill 20min, then deionized water is used, ethanol and acetone repetitive scrubbing more than three times, namely purity is obtained high, the nano cuprous oxide that good stability, oil soluble are good.
Embodiment 3: 30g cupric sulfate pentahydrate, 100g xitix, 30ml dimethyl sulfoxide (DMSO) and 2ml formic acid are joined in mortar, stir at the temperature of 40 DEG C, and adopt mechanical mill 50min, then deionized water is used, ethanol and acetone repetitive scrubbing more than three times, namely purity is obtained high, the nano cuprous oxide that good stability, oil soluble are good.
Embodiment 4: 12g cupric nitrate, 25g S-WAT (seven water), 10ml dimethyl sulfoxide (DMSO) and 2ml nitric acid are joined in mortar, stir at the temperature of 50 DEG C, and adopt mechanical mill 30min, then deionized water is used, ethanol and acetone repetitive scrubbing more than three times, namely purity is obtained high, the nano cuprous oxide that good stability, oil soluble are good.
Embodiment 5: 16g cupric sulfate pentahydrate, 15g formic acid, 20ml dimethyl sulfoxide (DMSO) and 2ml formic acid are joined in mortar, stir at the temperature of 30 DEG C, and adopt mechanical mill 40min, then deionized water is used, ethanol and acetone repetitive scrubbing more than three times, namely purity is obtained high, the nano cuprous oxide that good stability, oil soluble are good.
Embodiment 6: 12g neutralized verdigris (water), 10g trolamine, 20ml dimethyl sulfoxide (DMSO) and 2ml acetic acid are joined in mortar, stir at the temperature of 35 DEG C, and grind 6 hours, then deionized water is used, ethanol and acetone repetitive scrubbing more than three times, namely purity is obtained high, the nano cuprous oxide that good stability, oil soluble are 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 application claims.
Claims (8)
1. a grinding production method for nano cuprous oxide, is characterized in that:
1) mantoquita, reductive agent and dimethyl sulfoxide (DMSO) are stirred at the temperature of 10-70 DEG C, and the 0.2-6h that mills;
2) mixture after milling is used deionized water, ethanol and acetone repetitive scrubbing several times successively, stable nano cuprous oxide can be obtained;
The mol ratio of described reductive agent and mantoquita is 1-10:1, and the ratio of dimethyl sulfoxide (DMSO) and mantoquita is 1-100ml:10g.
2. the grinding production method of nano cuprous oxide according to claim 1, is characterized in that: described reductive agent is one or more in formaldehyde, V-Brite B, hydroborate and hydrazine hydrate.
3. the grinding production method of nano cuprous oxide according to claim 1 and 2, it is characterized in that: described mantoquita is copper sulfate, the title complex of cupric nitrate, cupric chloride, neutralized verdigris, copper and comprise one or several of organic copper of long-chain, and wherein the carbon chain lengths of organic copper is 8-16.
4. the grinding production method of nano cuprous oxide according to claim 1 and 2, is characterized in that: described step 1) technique of milling be mechanical disruption or manual mill.
5. a grinding production method for nano cuprous oxide, is characterized in that:
1) mantoquita, reductive agent, acid and dimethyl sulfoxide (DMSO) are stirred at the temperature of 10-70 DEG C, and the 0.2-6h that mills;
2) mixture after milling is used deionized water, ethanol and acetone repetitive scrubbing several times successively, stable nano cuprous oxide can be obtained;
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.
6. the grinding production method of nano cuprous oxide according to claim 5, 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 oxammonium hydrochloride.
7. the grinding production method of the nano cuprous oxide according to claim 5 or 6, it is characterized in that: described mantoquita is copper sulfate, the title complex of cupric nitrate, cupric chloride, neutralized verdigris, copper and comprise one or several of organic copper of long-chain, and wherein the carbon chain lengths of organic copper is 8-16.
8. the grinding production method of the nano cuprous oxide according to claim 5 or 6, is characterized in that: described acid is one or more in sulfuric acid, hydrochloric acid, nitric acid, acetic acid, phosphoric acid, formic acid and oxalic acid; Step 1) technique of milling be mechanical disruption or manual mill.
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CN103435090B (en) * | 2013-08-02 | 2015-06-10 | 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 |
CN106115764B (en) * | 2016-06-23 | 2017-12-12 | 淮北师范大学 | The method that one pot of ball milling solid phase method prepares CuI nano-powders |
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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 |
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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 |
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