CN105036174A - Production method for submicron electronic-grade copper oxide powder - Google Patents
Production method for submicron electronic-grade copper oxide powder Download PDFInfo
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- CN105036174A CN105036174A CN201510404441.2A CN201510404441A CN105036174A CN 105036174 A CN105036174 A CN 105036174A CN 201510404441 A CN201510404441 A CN 201510404441A CN 105036174 A CN105036174 A CN 105036174A
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- Prior art keywords
- oxide powder
- copper oxide
- production method
- solution
- atomization
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- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 239000000843 powder Substances 0.000 claims abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 13
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 12
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 claims abstract description 10
- 238000005118 spray pyrolysis Methods 0.000 claims abstract description 8
- 230000000694 effects Effects 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 4
- 239000003595 mist Substances 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims abstract description 3
- 238000000889 atomisation Methods 0.000 claims description 21
- 229960004643 cupric oxide Drugs 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 12
- 238000009826 distribution Methods 0.000 claims description 10
- 230000002463 transducing effect Effects 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229960003280 cupric chloride Drugs 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004064 recycling Methods 0.000 abstract 2
- 239000005751 Copper oxide Substances 0.000 abstract 1
- 229910000431 copper oxide Inorganic materials 0.000 abstract 1
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(i) oxide Chemical compound [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 17
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 229920002955 Art silk Polymers 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 235000003599 food sweetener Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- NNFCIKHAZHQZJG-UHFFFAOYSA-N potassium cyanide Chemical compound [K+].N#[C-] NNFCIKHAZHQZJG-UHFFFAOYSA-N 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000003765 sweetening agent Substances 0.000 description 1
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a production method for submicron electronic-grade copper oxide powder. The production method comprises the following steps of: (1) firstly, preparing a copper chloride precursor solution; (2) adding the precursor solution prepared in the step (1) into an ultrasonic atomizing device, and atomizing the solution into a mist gas state by virtue of cavitation effect of ultrasonic waves, thereby forming droplets of the submicron solution; (3) pumping the droplets generated in the step (2) by use of a fan into a high-temperature atmosphere to carry out spray pyrolysis, thereby generating high-purity and submicron copper oxide copper; (4) recycling the copper oxide powder generated in the step (3) by an ultrafine powder recycling device, thereby obtaining a finished product; and (5) absorbing a hydrogen chloride gas by an absorbing tower, thereby obtaining a hydrochloric acid solution for preparing the copper chloride precursor in the step (1). The copper oxide produced by the method disclosed by the invention is high in purity and good in particle dimension, and product fineness reaches submicron requirements.
Description
Technical field
The present invention relates to non-ferrous metal powder technology field, particularly relate to a kind of production method of submicroscale electronic grade copper oxide powder.
Background technology
Cupric oxide (CuO) is a kind of black oxide of copper, shows slightly both sexes, slightly water absorbability.Relative molecular mass is 79.545, and density is 6.3 ~ 6.9g/cm
3, fusing point 1326 DEG C.Water insoluble and ethanol, is dissolved in acid, ammonium chloride and potassium cyanide solution, slowly dissolves in ammonia solution, can react with highly basic.Cupric oxide is mainly used in artificial silk processed, pottery, glaze and enamel, battery, petroleum sweetening agent, sterilant, also for hydrogen manufacturing, catalyzer, green glass etc.
Current domestic production cupric oxide powder mainly utilizes spray pyrolysis technologies, and the metal chlorination copper solutions of configuration is sent into pressure jet apparatus under the conveying of high-pressure pump, and formation jet enters oxidized still and carries out spray pyrolysis production cupric oxide powder.Mainly adopt Mechanical nozzle, the formation jet that pumps up enters oxidized still and carries out spray pyrolysis production cupric oxide.The cupric oxide purity not high (more than 100 microns) that domestic prior art produces at solution presoma spray pyrolysis, fineness does not reach the requirement of submicron order.I.e. 1-5 micron.
Summary of the invention
The invention provides a kind of production method of submicroscale electronic grade copper oxide powder, ultrasonic oscillation sheet is utilized to assemble ultrasonic atomizer, configuring certain density metallic solution utilizes hyperacoustic cavitation effect metallic solution to be atomized into the smog gaseous state of submicron order, through oxidized still atomization pyrolysis, production high purity electronic grade super-fine cupric oxide powder.
The present invention adopts following technical scheme:
The concrete steps of the production method of submicroscale electronic grade copper oxide powder of the present invention are as follows:
(1) first cupric chloride precursor solution is prepared;
(2) precursor solution that step (1) prepares is joined in ultrasonic atomizing device, utilize hyperacoustic cavitation effect, make solution mist change into smog gaseous state, form the droplet of submicron order solution;
(3) with blower fan the droplet that step (2) produces pumped in high-temperature atmosphere and carry out spray pyrolysis, produce cupric oxide powder that is high-purity, submicron order;
(4) cupric oxide powder utilizing ultrafine powder retrieving arrangement step (3) to be produced, obtains finished product;
(5) utilize absorption tower absorbing hydrogen chloride gas, obtain hydrochloric acid soln, for step (1) preparation cupric oxide presoma.
In step (2), distribution and atomizing generator is provided with bottom described ultrasonic atomizing device, the ultrasonic wave that the vibrational frequency higher than 20KHz utilizing direct current to produce produces, atomization transducer is provided with above distribution and atomizing generator, be provided with atomization transducing liquid above atomization transducer, the ultrasonic wave that distribution and atomizing generator produce passes to precursor solution by atomization transducer and atomization transducing liquid successively.
The composition of described atomization transducing liquid is deionized water (industrial pure water).
In step (2), the particle diameter of described submicron order solution is 1-5 μm.
Ultrasonic wave has following characteristic:
1) ultrasonic wave can have effect spread in the media such as gas, liquid, solid, Solid solution.
2) ultrasonic wave can transmit very strong energy.
3) ultrasonic wave can produce reflection, interference, superposition and resonance effect.
4), when ultrasonic wave is propagated in liquid medium, strong impact and cavitation phenomenon can be produced on interface.
The present invention compared with prior art, has following notable feature and beneficial effect:
The requirement that cupric oxide purity is high, particle dispersion good, product fineness reaches submicron order of the production method production of submicroscale electronic grade copper oxide powder of the present invention.Solvent evaporation and the pyrolysis of metal fused salt are occurred simultaneously, operational path section, One-step production cupric oxide.
Accompanying drawing explanation
Fig. 1 is the structural representation of the ultrasonic atomizing device in the present invention;
1 distribution and atomizing generator, 2 atomization transducing liquid, 3 spray chambers, 4 cupric chloride precursor solutions, 5 atomization transducers.
Fig. 2 is the process flow sheet of the production method of submicroscale electronic grade copper oxide powder of the present invention.
Embodiment
Below by embodiment, the present invention is specifically described; what be necessary to herein means out is that the present embodiment is only used to further illustrate the present invention; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field must belong to protection scope of the present invention according to the nonessential improvement more made for the present invention of the invention described above content and adjustment.
Embodiment 1
The concrete steps of the production method of submicroscale electronic grade copper oxide powder of the present invention are as follows:
(1) first cupric chloride precursor solution is prepared;
(2) precursor solution that step (1) prepares is joined in ultrasonic atomizing device, utilize hyperacoustic cavitation effect, make solution mist change into smog gaseous state, form the droplet of submicron order solution;
(3) with blower fan the droplet that step (2) produces pumped in high-temperature atmosphere and carry out spray pyrolysis, produce cupric oxide powder that is high-purity, submicron order;
(4) cupric oxide powder utilizing ultrafine powder retrieving arrangement step (3) to be produced, obtains finished product;
(5) utilize absorption tower absorbing hydrogen chloride gas, obtain hydrochloric acid soln, for step (1) preparation cupric oxide presoma.
In step (2), distribution and atomizing generator is provided with bottom described ultrasonic atomizing device, the ultrasonic wave that the vibrational frequency higher than 20KHz utilizing direct current to produce produces, atomization transducer is provided with above distribution and atomizing generator, be provided with atomization transducing liquid above atomization transducer, the ultrasonic wave that distribution and atomizing generator produce passes to precursor solution by atomization transducer and atomization transducing liquid successively.
Described atomization transducing liquid is deionized water (industrial pure water).
Although illustrate and describe embodiments of the invention, for the ordinary skill in the art, be appreciated that and can carry out multiple change, amendment, replacement and modification to these embodiments without departing from the principles and spirit of the present invention, scope of the present invention is by claims and equivalents thereof.
Claims (4)
1. a production method for submicroscale electronic grade copper oxide powder, is characterized in that: the concrete steps of described method are as follows:
(1) first cupric chloride precursor solution is prepared;
(2) precursor solution that step (1) prepares is joined in ultrasonic atomizing device, utilize hyperacoustic cavitation effect, make solution mist change into smog gaseous state, form the droplet of submicron order solution;
(3) with blower fan the droplet that step (2) produces pumped in high-temperature atmosphere and carry out spray pyrolysis, produce cupric oxide powder that is high-purity, submicron order;
(4) cupric oxide powder utilizing ultrafine powder retrieving arrangement step (3) to be produced, obtains finished product;
(5) utilize absorption tower absorbing hydrogen chloride gas, obtain hydrochloric acid soln, for step (1) preparation cupric oxide presoma.
2. the production method of submicroscale electronic grade copper oxide powder as claimed in claim 1, it is characterized in that: in step (2), distribution and atomizing generator is provided with bottom described ultrasonic atomizing device, the ultrasonic wave that the vibrational frequency higher than 20KHz utilizing direct current to produce produces, atomization transducer is provided with above distribution and atomizing generator, be provided with atomization transducing liquid above atomization transducer, the ultrasonic wave that distribution and atomizing generator produce passes to precursor solution by atomization transducer and atomization transducing liquid successively.
3. the production method of submicroscale electronic grade copper oxide powder as claimed in claim 2, is characterized in that: the composition of described atomization transducing liquid is deionized water (industrial pure water).
4. the production method of submicroscale electronic grade copper oxide powder as claimed in claim 1, it is characterized in that: in step (2), the particle diameter of described submicron order solution is 1-5 μm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510404441.2A CN105036174A (en) | 2015-07-10 | 2015-07-10 | Production method for submicron electronic-grade copper oxide powder |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510404441.2A CN105036174A (en) | 2015-07-10 | 2015-07-10 | Production method for submicron electronic-grade copper oxide powder |
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| CN105036174A true CN105036174A (en) | 2015-11-11 |
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| CN201510404441.2A Pending CN105036174A (en) | 2015-07-10 | 2015-07-10 | Production method for submicron electronic-grade copper oxide powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107983374A (en) * | 2016-03-22 | 2018-05-04 | 湖州慧金材料科技有限公司 | The method that activity spherical cuprous chloride catalyst is prepared using atomized molten system |
| CN108862364A (en) * | 2018-09-21 | 2018-11-23 | 东北大学 | A kind of molten salt solvent method preparation nanometer Cu2The method of O particle |
| CN114956152A (en) * | 2021-12-27 | 2022-08-30 | 昆明理工大学 | Method for preparing needle-shaped CuO powder by ultrasonic atomization |
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| CN103482619A (en) * | 2013-09-09 | 2014-01-01 | 东南大学 | Graphene-copper oxide three-dimensional foam composite material |
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2015
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| CN1683266A (en) * | 2004-04-16 | 2005-10-19 | 天津理工学院 | Device and process for producing nano TiO2 film by supersonic atomization |
| CN1657422A (en) * | 2005-01-27 | 2005-08-24 | 北京科技大学 | Device and method for preparing nanometer tungsten trioxide powder using ultrasonic spray microwave drying method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107983374A (en) * | 2016-03-22 | 2018-05-04 | 湖州慧金材料科技有限公司 | The method that activity spherical cuprous chloride catalyst is prepared using atomized molten system |
| CN108862364A (en) * | 2018-09-21 | 2018-11-23 | 东北大学 | A kind of molten salt solvent method preparation nanometer Cu2The method of O particle |
| CN114956152A (en) * | 2021-12-27 | 2022-08-30 | 昆明理工大学 | Method for preparing needle-shaped CuO powder by ultrasonic atomization |
| CN114956152B (en) * | 2021-12-27 | 2024-01-23 | 昆明理工大学 | Method for preparing needle-like CuO powder by ultrasonic atomization |
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| TA01 | Transfer of patent application right |
Effective date of registration: 20160708 Address after: 737100 Jinchang Gansu economic and Technological Development Zone Jinchang Xu industry and Trade Co., Ltd. Applicant after: Jinchang Zhengxu Industry and Trade Co., Ltd. Address before: 737100 Jinchang economic and Technological Development Zone, Fuzhou Road, east of Gansu, south of Tai'an Road Applicant before: An Pengjiu |
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Application publication date: 20151111 |
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