CN102491403B - Method for preparing copper oxide powder by using complexed-precipitation method - Google Patents
Method for preparing copper oxide powder by using complexed-precipitation method Download PDFInfo
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- CN102491403B CN102491403B CN201110426617.6A CN201110426617A CN102491403B CN 102491403 B CN102491403 B CN 102491403B CN 201110426617 A CN201110426617 A CN 201110426617A CN 102491403 B CN102491403 B CN 102491403B
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- aqueous solution
- naoh
- powder
- copper sulfate
- koh
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- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000001556 precipitation Methods 0.000 title claims abstract description 25
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 54
- 239000007864 aqueous solution Substances 0.000 claims abstract description 44
- 239000000843 powder Substances 0.000 claims abstract description 38
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 24
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 239000008139 complexing agent Substances 0.000 claims abstract description 5
- 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 35
- NWFNSTOSIVLCJA-UHFFFAOYSA-L copper;diacetate;hydrate Chemical compound O.[Cu+2].CC([O-])=O.CC([O-])=O NWFNSTOSIVLCJA-UHFFFAOYSA-L 0.000 claims description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- 238000013016 damping Methods 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 9
- 238000003837 high-temperature calcination Methods 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 150000003863 ammonium salts Chemical class 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 14
- 239000000243 solution Substances 0.000 abstract description 13
- 239000002245 particle Substances 0.000 abstract description 8
- 238000001354 calcination Methods 0.000 abstract description 2
- 238000010899 nucleation Methods 0.000 abstract description 2
- 230000006911 nucleation Effects 0.000 abstract description 2
- 150000001879 copper Chemical class 0.000 abstract 3
- 230000003139 buffering effect Effects 0.000 abstract 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 abstract 1
- -1 amine salt Chemical class 0.000 abstract 1
- 235000011114 ammonium hydroxide Nutrition 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- 239000010949 copper Substances 0.000 description 8
- 229960004643 cupric oxide Drugs 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for preparing copper oxide powder by using a complexed-precipitation method. The concentration of an aqueous solution of water-soluble copper salt, such as copper sulfate is between 0.5mole/L and 3mole/L; and a 4-6mole/L NaOH or KOH aqueous solution is utilized as a neutralizer. The method comprises the following steps of: adding 1/10 of the copper salt aqueous solution and the NaOH or KOH aqueous solution into 5-15wt% ammonia water or an amine salt complexing agent to dissolve precipitates gradually, further controlling the pH to be 9-12, thus obtaining a buffering solution; and dropwise adding the residual copper salt aqueous solution and the residual NaOH or KOH aqueous solution into the buffering solution, controlling the pH value to be 9-12, controlling the reaction temperature at 80-90 DEG C, reacting for 4 hours, filtering, washing, drying at the temperature of over 100 DEG C, and calcining at high temperature to obtain high-compactness CuO powder with the apparent density of more than 1.5g/cm<3>. By utilizing the technical scheme, the CuO powder is subjected to processes of nucleation and gradual growth, so that the appearance of the CuO power is spherical, the particle size is uniformly distributed, and an aggregation-free product is obtained. The preparation process is simple and quick; and the particle size of the prepared CuO powder is controllable.
Description
Technical field
The invention belongs to mineral compound Preparation Technique of Powders field, particularly be that a kind of complex-precipitation legal system that adopts is for the method for high fine and close cupric oxide powder.
Background technology
CuO is as a kind of broad-spectrum multifunctional inorganic material, there is unique electricity, magnetic, catalysis characteristics, be widely used in the key areas such as glass, coating, inorganic adhesive, solder flux, catalyzer, gas sensor, magnetic storage medium, superconducting material and electrode active material.
At present, the preparation of cupric oxide powder comprises three kinds of methods, the one, and the method for mantoquita high-temperature calcination, adopts at high temperature calcining and decomposing of the inorganic salt such as copper sulfate, obtain cupric oxide powder, the method technique is simple, and cost is low, is the main production of domestic cupric oxide powder, but the particle diameter of the uncontrollable product of the method, be difficult to obtain particle diameter high fine and close cupric oxide powder uniformly, and relate to the discharge of sulfide, application is restricted day by day.Another kind is the cupric oxide powder technology of preparing that offshore company adopts, by spray method ejection under high temperature (approximately 1300 ℃) for the copper of melt and dissolved state, through being combined into cupric oxide powder with airborne oxygen, this kind of equipment and the technology more complicated that method needs, therefore, this method is only used in a few countries such as U.S., day, morals.
Having is exactly to utilize liquid-phase precipitation technology to prepare CuO powder again, and primitive reaction is as follows:
Cu
2+?+?OH
-?=?Cu(OH)
2↓→?CuO
Insoluble compound feature of crystallisation process in the aqueous solution is to be easy to nucleation and particle is difficult to grow up, for Cu (OH)
2precipitation is also like this.By mantoquita and alkali direct reaction, prepare Cu (OH)
2time, if reaction and crystallisation process are not effectively controlled to Cu (OH)
2degree of supersaturation in process of growth is enough to generate a large amount of nucleus, and the speed of growth of crystal is relatively very slow, the Cu (OH) therefore generating
2particle is very thin, is a kind of colloidal precipitation, the equal difficult of solid-liquid separation and washing operation, and after product is dry, caking is serious, need to grind and can obtain powder product, this Cu (OH)
2the tap density of product is very low.
Summary of the invention
The present situation that cannot prepare the controlled CuO powder of particle diameter for current liquid-phase precipitation technology, the present invention proposes a kind of method of utilizing complex-precipitation technology to prepare CuO powder.
Technical scheme of the present invention is: a kind of method of preparing copper oxide powder by using complexed-precipitation method, specifically comprises the following steps:
1) a certain amount of copper sulfate, cupric nitrate or neutralized verdigris are made into the aqueous solution that concentration is 0.5 ~ 3 mol/L, take with NaOH or the KOH of the quality such as described copper sulfate, cupric nitrate or neutralized verdigris and be made into the aqueous solution that concentration is 4～6 mol/L, standby;
2) get copper sulfate, cupric nitrate or the neutralized verdigris aqueous solution and NaOH or the KOH aqueous solution that 1/10th step 1 configurations obtain, produce a large amount of precipitations after mixing, adding concentration is the complexing agent of 5 ~ 15wt%, precipitation is dissolved gradually, control pH 9～12, obtain damping fluid, standby; Wherein, complexing agent is for adopting the aqueous solution of ammonia or ammonium salt;
3) aqueous solution of remaining copper sulfate, cupric nitrate or the neutralized verdigris aqueous solution and NaOH or KOH being added drop-wise to step 2 simultaneously obtaining in damping fluid, is 9～12 at pH, in temperature, is 80～90 oC, react 4 hours, filter, washing, 100 oC are dry above, obtain CuO powder;
4) above-mentioned steps 3 is obtained to CuO powder and put High Temperature Furnaces Heating Apparatus into, through 500～900oC high-temperature calcination, obtain loose density and be greater than 1.5g/cm
3the fine and close CuO powder of height.
The invention has the beneficial effects as follows: owing to adopting technique scheme, the process that CuO powder has experienced forming core and progressively grown up, thus it is spherical in shape to form outward appearance, and size distribution is even, without the product of reuniting.Preparation technology of the present invention is simple, quick and prepare the standby controlled CuO powder of particle diameter.
Embodiment
below in conjunction with specific embodiment, technical scheme of the present invention is described further.
Embodiment 1
Take a certain amount of copper sulfate, be configured to the copper sulfate solution that concentration is 1 mol/L, it is the 4 mol/L aqueous solution that the NaOH with copper sulfate equivalent is made into concentration; Get 1/10th copper sulfate solutions and the NaOH aqueous solution, produce a large amount of precipitations after mixing, adding concentration is the aqueous solution of 5wt% ammonia, and precipitation is dissolved gradually, and pH value is 9, obtains damping fluid, standby; The aqueous solution of remaining copper sulfate and NaOH is added drop-wise in reaction system, controls pH value 11, control temperature of reaction is 80oC, reacts 4 hours, filter, and washing, 120 oC are dry; Put above-mentioned CuO powder into retort furnace, through 700oC high-temperature calcination, obtain high fine and close CuO powder, the loose density of powder is 1.92g/cm
3.
Embodiment 2
Taking a certain amount of cupric nitrate, to be configured to strength of solution be 3 mol/L copper nitrate aqueous solutions; To be made into the aqueous solution with the KOH of cupric nitrate equivalent, concentration is 6 mol/L; Get 1/10th copper nitrate aqueous solutions and the KOH aqueous solution, produce a large amount of precipitations after mixing, adding concentration is the aqueous solution of 10wt% ammonia, and precipitation is dissolved gradually, and pH is 10, forms damping fluid; The aqueous solution of remaining cupric nitrate and KOH is added drop-wise in reaction system, controls pH value 12, control temperature of reaction is 85oC, reacts 4 hours, filter, and washing, 120 oC are dry; Put above-mentioned CuO powder into retort furnace, through 500oC high-temperature calcination, obtain high fine and close CuO powder, the loose density of powder is 1.65g/cm
3.
Embodiment 3
Taking a certain amount of neutralized verdigris obtain solution concentration is 0.5 mol/L copper sulfate solution, and it is the 4.5 mol/L aqueous solution that the NaOH with neutralized verdigris equivalent is made into concentration; Get 1/10th neutralized verdigris aqueous solution and the NaOH aqueous solution, produce a large amount of precipitations after mixing, adding concentration is the aqueous solution of 15wt% ammonium salt, and precipitation is dissolved gradually, controls pH to 11, forms damping fluid; The aqueous solution of remaining neutralized verdigris and NaOH is added drop-wise in reaction system, controls pH value 10, control temperature of reaction is 90oC, reacts 4 hours, filter, and washing, 120 oC are dry; Put above-mentioned CuO powder into retort furnace, through 600oC high-temperature calcination, obtain high fine and close CuO powder, the loose density of powder is 1.83g/cm
3.
Embodiment 4
Preparation copper sulfate solution, strength of solution is 2 mol/L; To be made into the aqueous solution with the NaOH of copper sulfate equivalent, concentration is 5 mol/L; Get 1/10th copper sulfate solutions and the NaOH aqueous solution, produce a large amount of precipitations after mixing, concentration is the aqueous solution of 12wt% ammonia, and precipitation is dissolved gradually, controls pH to 12, forms damping fluid; The aqueous solution of remaining copper sulfate and NaOH is added drop-wise in reaction system, controls pH value 12, control temperature of reaction is 82oC, reacts 4 hours, filter, and washing, 140 oC are dry; Put above-mentioned CuO powder into retort furnace, through 800oC high-temperature calcination, obtain high fine and close CuO powder, the loose density of powder is 1.94g/cm
3.
Embodiment 5
Preparation copper sulfate solution, strength of solution is 2.5 mol/L; To be made into the aqueous solution with the KOH of copper sulfate equivalent, concentration is 5.5 mol/L; Get 1/10th copper sulfate solutions and the KOH aqueous solution, produce a large amount of precipitations after mixing, adding concentration is the aqueous solution of 7.5wt% ammonium salt, and precipitation is dissolved gradually, controls pH to 11, forms damping fluid; The aqueous solution of remaining copper sulfate and KOH is added drop-wise in reaction system, controls pH value 11, control temperature of reaction is 87oC, reacts 4 hours, filter, and washing, 160 oC are dry; Put above-mentioned CuO powder into retort furnace, through 900oC high-temperature calcination, obtain high fine and close CuO powder, the loose density of powder is 1.96g/cm
3.
Claims (1)
1. a method for preparing copper oxide powder by using complexed-precipitation method, is characterized in that, specifically comprises the following steps:
1) a certain amount of copper sulfate, cupric nitrate or neutralized verdigris are made into the aqueous solution that concentration is 0.5 ~ 3 mol/L, take with NaOH or the KOH of described copper sulfate, cupric nitrate or neutralized verdigris equivalent and be made into the aqueous solution that concentration is 4～6 mol/L, standby;
2) get copper sulfate, cupric nitrate or the neutralized verdigris aqueous solution and NaOH or the KOH aqueous solution that 1/10th step 1) preparations obtain, produce a large amount of precipitations after mixing, adding concentration is the complexing agent of 5 ~ 15wt%, precipitation is dissolved gradually, control pH 9～12, obtain damping fluid, standby; Wherein, complexing agent is for adopting the aqueous solution of ammonia or ammonium salt;
3) aqueous solution of remaining copper sulfate, cupric nitrate or the neutralized verdigris aqueous solution and NaOH or KOH is added drop-wise to step 2 simultaneously) in the damping fluid that obtains, at pH, be 9～12, in temperature, be 80～90 ℃, react 4 hours, filter, washing, 100 ℃ above dry, obtains CuO powder;
4) above-mentioned steps is obtained to CuO powder and put High Temperature Furnaces Heating Apparatus into, through 500～900 ℃ of high-temperature calcinations, obtain loose density and be greater than 1.5g/cm
3the fine and close CuO powder of height.
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| CN103232055B (en) * | 2013-04-10 | 2015-04-15 | 廖勇志 | Method of preparing basic copper carbonate |
| CN103232056B (en) * | 2013-04-10 | 2015-04-15 | 廖勇志 | Method of preparing copper oxide |
| CN104445360A (en) * | 2014-12-03 | 2015-03-25 | 金川集团股份有限公司 | Production method of high-purity active copper oxide powder |
| CN104692446B (en) * | 2015-03-18 | 2016-08-31 | 合肥工业大学 | A kind of preparation method of high-purity low chlorine oxide of high activity copper |
| CN109096685A (en) * | 2018-07-18 | 2018-12-28 | 安徽江淮汽车集团股份有限公司 | A kind of ABS composite material and preparation method thereof of the low VOC of antibacterial |
| CN109111597A (en) * | 2018-07-18 | 2019-01-01 | 安徽江淮汽车集团股份有限公司 | A kind of preparation method of antibacterial agent |
| CN109575362A (en) * | 2018-12-07 | 2019-04-05 | 安徽江淮汽车集团股份有限公司 | A kind of antibacterial agent and preparation method thereof |
| CN110642284A (en) * | 2019-09-16 | 2020-01-03 | 浙江天能能源科技股份有限公司 | Preparation method of flower-shaped CuO negative electrode material |
| JP2021088492A (en) * | 2019-12-06 | 2021-06-10 | 三菱マテリアル株式会社 | Method for producing copper oxide powder, and copper oxide powder |
| CN112897566B (en) * | 2021-01-21 | 2023-06-13 | 佛山市华希盛化工有限公司 | Process for producing high-purity active copper oxide by complexation displacement method |
| CN114836631B (en) * | 2022-06-15 | 2023-12-01 | 蜂巢能源科技股份有限公司 | Recycling method of copper-manganese liquid generated by extraction and recovery of battery materials |
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| US3635668A (en) * | 1969-03-21 | 1972-01-18 | Cities Service Co | Copper hydrate production |
| CN101988882B (en) * | 2009-08-03 | 2012-04-25 | 中国科学院理化技术研究所 | Quartz crystal microbalance sensor for detecting HCN gas and manufacturing method and application thereof |
| CN102234128A (en) * | 2010-05-05 | 2011-11-09 | 温佳丽 | Process for preparing nano copper hydroxide by homogeneous precipitation |
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