CN113968588A - Production method of copper oxide - Google Patents

Production method of copper oxide Download PDF

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Publication number
CN113968588A
CN113968588A CN202111375162.XA CN202111375162A CN113968588A CN 113968588 A CN113968588 A CN 113968588A CN 202111375162 A CN202111375162 A CN 202111375162A CN 113968588 A CN113968588 A CN 113968588A
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China
Prior art keywords
copper oxide
vacuum drying
vacuum
drying oven
slurry
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CN202111375162.XA
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Chinese (zh)
Inventor
盛勤明
黄勇键
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Wujiang Weishida Copper Technology Co ltd
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Wujiang Weishida Copper Technology Co ltd
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Priority to CN202111375162.XA priority Critical patent/CN113968588A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00Compounds of copper
    • C01G3/02Oxides; Hydroxides
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/10Solid density

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Oxygen, Ozone, And Oxides In General (AREA)

Abstract

The invention discloses a production method of copper oxide, which relates to the field of chemical production and comprises a reactor, a vacuum pumping barrel and a vacuum drying oven, wherein a vacuum drying system is arranged in the vacuum drying oven, and the production method further comprises the following steps: the method comprises the following steps: mixing the following components in a mass ratio of 10: 1, mixing the copper salt and the alkali compound in a reactor to synthesize copper oxide, sending the copper oxide into a vacuum filtration barrel, and carrying out solid-liquid separation; step two: adding water into the vacuum pumping and filtering barrel, and washing copper oxide to obtain clean copper oxide; step three: adding water into clean copper oxide for wetting to obtain copper oxide slurry; step four: putting the copper oxide slurry into a tray and moving the tray into a vacuum drying oven; step five: drying the copper oxide slurry in vacuum to obtain dry copper oxide; step six: and crushing the dried copper oxide, and packaging to obtain a finished product. Compared with the copper oxide manufactured by the traditional method, the copper oxide manufactured by the method has the advantages of loose structure, large surface area, light weight, good dispersion performance, easier dissolution and high dissolution speed.

Description

Production method of copper oxide
Technical Field
The invention relates to the field of chemical production, in particular to a production method of copper oxide.
Background
The copper oxide powder is brown black metal oxide powder, is a multifunctional fine inorganic material with wide application, is mainly used in the aspects of artificial silk, ceramics, glaze, enamel, batteries, petroleum desulfurizer, pesticide and the like, and also has application in hydrogen production, catalysts, green glass and the like. At present, the domestic production of copper oxide mainly comprises two major types, namely dry production and wet production.
And (3) dry production, namely oxidizing the elemental copper and oxygen in the air into copper oxide at high temperature. The method comprises the steps of roasting copper ash and copper slag as raw materials to obtain crude copper oxide, then carrying out acid dissolution, replacing to obtain copper powder with high grade, and carrying out high-temperature oxidation in an oxidation furnace to obtain copper oxide powder.
And (3) wet production: adding a copper salt solution into an alkaline compound at a certain temperature to carry out a series of reactions to synthesize copper oxide, then washing to remove other impurities, and baking at a higher temperature under normal pressure to drive water in the copper oxide powder to obtain the copper oxide powder.
The copper oxide produced by the dry method is finished by high-temperature oxidation, and the generated copper oxide particles are large and hard through high-temperature sintering, have small specific volume (heavier), and are slow in dissolution speed in the use process, and some copper oxide particles are even difficult to dissolve, so that the use effect is influenced. The copper oxide produced by the wet method also has similar problems in the production process, and after the wet product copper oxide with moisture is formed in the production process, the copper oxide can be completely removed by baking at a higher temperature generally above 150 ℃ under normal pressure, so that the obtained copper oxide has a compact structure, hardness and large specific volume, and the dissolution speed is not ideal when the copper oxide is used.
Disclosure of Invention
The invention aims to provide a method for producing copper oxide with loose structure, large surface area, good dispersibility and high dissolution speed.
The technical scheme adopted by the invention for solving the technical problems is as follows: the production method of the copper oxide comprises a reactor, a vacuum filtration barrel and a vacuum drying oven, wherein a vacuum drying system is arranged in the vacuum drying oven, and the production method further comprises the following steps:
the method comprises the following steps: mixing the components in a mass ratio of 10: 1, mixing the copper salt and the alkali compound in a reactor to synthesize copper oxide, conveying the copper oxide in the reactor to a vacuum filtration barrel by using a pump, and carrying out solid-liquid separation;
step two: adding water into the vacuum pumping and filtering barrel, and washing the copper oxide to obtain the cleanly washed copper oxide;
step three: adding water into clean copper oxide for wetting to obtain copper oxide slurry with the water content of 8-10%;
step four: putting the copper oxide slurry into a tray, and then moving the tray into a vacuum drying oven;
step five: starting a vacuum drying system and a temperature switch of a vacuum drying oven, and carrying out vacuum drying on the copper oxide slurry to obtain dried copper oxide;
step six: and crushing the dried copper oxide, and then metering and packaging to obtain a finished product.
Further, the method comprises the following steps: and in the second step, the washing is divided into four times, each time of washing is 10 minutes, the mass ratio of water to copper oxide is 1:5, and the temperature of water is 50-55 ℃.
Further, the method comprises the following steps: and in the fourth step, the weight of the copper oxide slurry in each tray is 15-20 kg.
Further, the method comprises the following steps: in the fifth step, the vacuum degree in the vacuum drying oven is-0.92 to-0.99 MPa, and the temperature in the vacuum drying oven is 60 to 80 ℃.
Further, the method comprises the following steps: and in the fifth step, the vacuum drying time is 20-24 hours.
The invention has the beneficial effects that: compared with the copper oxide manufactured by the traditional method, the copper oxide manufactured by the method has the advantages of loose structure, large surface area, light weight, good dispersion performance, easier dissolution and high dissolution speed.
Detailed Description
The present invention will be further described with reference to the following embodiments.
The embodiment of the application provides a production method of copper oxide, and the production method of the copper oxide comprises a reactor, a vacuum filtration barrel and a vacuum drying oven, wherein a vacuum drying system is arranged in the vacuum drying oven, and the production method further comprises the following steps:
the method comprises the following steps: mixing the components in a mass ratio of 10: 1, mixing the copper salt and the alkali compound in a reactor to synthesize copper oxide, conveying the copper oxide in the reactor to a vacuum filtration barrel by using a pump, and carrying out solid-liquid separation;
step two: adding water into the vacuum pumping and filtering barrel, and washing the copper oxide to obtain the cleanly washed copper oxide;
step three: adding water into clean copper oxide for wetting to obtain copper oxide slurry with the water content of 8-10%;
step four: putting the copper oxide slurry into a tray, and then moving the tray into a vacuum drying oven;
step five: starting a vacuum drying system and a temperature switch of a vacuum drying oven, and carrying out vacuum drying on the copper oxide slurry to obtain dried copper oxide;
step six: and crushing the dried copper oxide, and then metering and packaging to obtain a finished product.
On the basis, the washing in the second step is divided into four times, each time for 10 minutes, the mass ratio of water to copper oxide is 1:5, and the temperature of water is 50-55 ℃.
On the basis of the above, the weight of the copper oxide slurry in each tray in the fourth step is 15-20 kg.
On the basis, in the fifth step, the vacuum degree in the vacuum drying oven is-0.92 to-0.99 MPa, and the temperature in the vacuum drying oven is 60 to 80 ℃.
On the basis, the vacuum drying time in the fifth step is 20-24 hours.
The first embodiment is as follows:
the production method of the copper oxide comprises a reactor, a vacuum filtration barrel and a vacuum drying oven, wherein a vacuum drying system is arranged in the vacuum drying oven, and the production method further comprises the following steps:
the method comprises the following steps: mixing 500kg of copper sulfate and 50kg of sodium hydroxide in a reactor to synthesize 550kg of copper oxide, conveying 550kg of copper oxide in the reactor into a vacuum filtration barrel by using a pump for solid-liquid separation, conveying liquid into a sewage treatment station through a special pipeline, and keeping solid copper oxide in the vacuum filtration barrel;
step two: adding 110kg of water into a vacuum pumping and filtering barrel, wherein the temperature of the water is 50 ℃, washing the copper oxide, and continuously washing for four times to obtain the washed copper oxide;
step three: adding 55kg of water into clean copper oxide for wetting to obtain copper oxide slurry with the water content of 10%;
step four: putting the copper oxide slurry into trays, wherein each tray is filled with 20kg of copper oxide slurry, and then moving the trays into a vacuum drying oven;
step five: closing a door of a vacuum drying oven, sealing, starting a vacuum drying system and a temperature switch of the vacuum drying oven, starting vacuumizing and heating, keeping the vacuum degree at-0.92 MPa and the temperature at 60 ℃ in the drying process, carrying out vacuum drying on the copper oxide slurry for 20 hours, increasing the vacuum degree to-0.99 MPa, and obtaining dried copper oxide A1 after drying is finished;
step six: the dried copper oxide A1 was pulverized and then metered and packaged as finished product.
Example two:
the production method of the copper oxide comprises a reactor, a vacuum filtration barrel and a vacuum drying oven, wherein a vacuum drying system is arranged in the vacuum drying oven, and the production method further comprises the following steps:
the method comprises the following steps: mixing 500kg of copper oxide and 50kg of sodium carbonate in a reactor to synthesize 550kg of copper oxide, conveying 550kg of copper oxide in the reactor to a vacuum filtration barrel by using a pump, carrying out solid-liquid separation, conveying liquid to a sewage treatment station through a special pipeline, and keeping solid copper oxide in the vacuum filtration barrel;
step two: adding 110kg of water into a vacuum pumping and filtering barrel, wherein the temperature of the water is 50 ℃, washing the copper oxide, and continuously washing for four times to obtain the washed copper oxide;
step three: adding 44kg of water into clean copper oxide for wetting to obtain copper oxide slurry with the water content of 8%;
step four: putting the copper oxide slurry into trays, wherein each tray is filled with 20kg of copper oxide slurry, and then moving the trays into a vacuum drying oven;
step five: closing a door of a vacuum drying oven, sealing, starting a vacuum drying system and a temperature switch of the vacuum drying oven, starting vacuumizing and heating, keeping the vacuum degree at-0.95 MPa and the temperature at 70 ℃ in the drying process, carrying out vacuum drying on the copper oxide slurry for 20 hours, and increasing the vacuum degree to-0.99 MPa, thus obtaining dried copper oxide A2 after drying is finished;
step six: the dried copper oxide A2 was pulverized and then metered and packaged as finished product.
Example three:
the production method of the copper oxide comprises a reactor, a vacuum filtration barrel and a vacuum drying oven, wherein a vacuum drying system is arranged in the vacuum drying oven, and the production method further comprises the following steps:
the method comprises the following steps: mixing 200kg of copper chloride and 20kg of sodium bicarbonate in a reactor to synthesize 220kg of copper oxide, conveying the 220kg of copper oxide in the reactor into a vacuum filtration barrel by using a pump for solid-liquid separation, conveying liquid into a sewage treatment station through a special pipeline, and keeping the solid copper oxide in the vacuum filtration barrel;
step two: adding 44kg of water into the vacuum pumping and filtering barrel, wherein the temperature of the water is 53 ℃, washing the copper oxide, and continuously washing for four times to obtain the washed copper oxide;
step three: adding 20kg of water into clean copper oxide for wetting to obtain copper oxide slurry with the water content of 9.1%;
step four: putting the copper oxide slurry into trays, wherein each tray is filled with 20kg of copper oxide slurry, and then moving the trays into a vacuum drying oven;
step five: closing a door of a vacuum drying oven, sealing, starting a vacuum drying system and a temperature switch of the vacuum drying oven, starting vacuumizing and heating, keeping the vacuum degree at-0.97 MPa and the temperature at 80 ℃ in the drying process, carrying out vacuum drying on the copper oxide slurry for 20 hours, and increasing the vacuum degree to-0.99 MPa, thus obtaining dried copper oxide A3 after drying is finished;
step six: the dried copper oxide A3 was pulverized and then metered and packaged as finished product.
Experimental data:
the copper oxide a1 obtained in example one, the copper oxide a2 obtained in example two, the copper oxide A3 obtained in example three, and the finished copper oxide B produced using atmospheric pressure and high temperature were analyzed for comparison in terms of bulk density, dissolution rate, and the like:
bulk density:
adding copper oxide A1/copper oxide A2/copper oxide A3 or copper oxide B into a 1L measuring cylinder, and shaking the measuring cylinder continuously until the copper oxide inside is compacted to obtain the bulk density:
A1:1.72g/cm3 A2:1.61g/cm3 A3:1.57g/cm3 B:1.87g/cm3
the measuring method comprises the following steps: vibrating the copper oxide in the measuring cylinder to pile the copper oxide in the measuring cylinder, reading the scale of the measuring cylinder to obtain the volume of the copper oxide, then pouring the copper oxide in the measuring cylinder, weighing the weight of the poured copper oxide, and dividing the obtained weight of the copper oxide by the volume of the copper oxide to obtain the bulk density.
Dissolution speed:
copper oxide A1, copper oxide A2, copper oxide A3 and copper oxide B were weighed to 5.0g each, and added to a sulfuric acid solution having a solution concentration of 12% under stirring at a temperature of 30 ℃ and a rotation speed of 250 rpm, and the time for which they were completely dissolved in the sulfuric acid solution was measured:
a1:25 seconds A2:18 seconds A3:15 seconds B:32 seconds
From the above data, it is known that the dissolution rate of the copper oxide obtained in the three embodiments of the present application is faster than that of the copper oxide obtained at normal pressure and high temperature, and meanwhile, the higher the vacuum degree is, the looser the structure of the copper oxide is, and the fluffier the copper oxide is, the faster the dissolution rate is.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (5)

1. The production method of the copper oxide comprises a reactor, a vacuum filtration barrel and a vacuum drying oven, wherein a vacuum drying system is arranged in the vacuum drying oven, and the production method is characterized in that: also comprises the following steps:
the method comprises the following steps: mixing the components in a mass ratio of 10: 1, mixing the copper salt and the alkali compound in a reactor to synthesize copper oxide, conveying the copper oxide in the reactor to a vacuum filtration barrel by using a pump, and carrying out solid-liquid separation;
step two: adding water into the vacuum pumping and filtering barrel, and washing the copper oxide to obtain the cleanly washed copper oxide;
step three: adding water into clean copper oxide for wetting to obtain copper oxide slurry with the water content of 8-10%;
step four: putting the copper oxide slurry into a tray, and then moving the tray into a vacuum drying oven;
step five: starting a vacuum drying system and a temperature switch of a vacuum drying oven, and carrying out vacuum drying on the copper oxide slurry to obtain dried copper oxide;
step six: and crushing the dried copper oxide, and then metering and packaging to obtain a finished product.
2. The method for producing copper oxide according to claim 1, wherein: and in the second step, the washing is divided into four times, each time of washing is 10 minutes, the mass ratio of water to copper oxide is 1:5, and the temperature of water is 50-55 ℃.
3. The method for producing copper oxide according to claim 1, wherein: and in the fourth step, the weight of the copper oxide slurry in each tray is 15-20 kg.
4. The method for producing copper oxide according to claim 1, wherein: in the fifth step, the vacuum degree in the vacuum drying oven is-0.92 to-0.99 MPa, and the temperature in the vacuum drying oven is 60 to 80 ℃.
5. The method for producing copper oxide according to claim 1, wherein: and in the fifth step, the vacuum drying time is 20-24 hours.
CN202111375162.XA 2021-11-19 2021-11-19 Production method of copper oxide Pending CN113968588A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20120047340A (en) * 2010-10-20 2012-05-14 서안켐텍 주식회사 Process for preparing cupric oxide powder for electric plating
CN102951671A (en) * 2012-10-22 2013-03-06 洛阳师范学院 Preparation method of copper oxide nano particle
CN103263963A (en) * 2013-04-22 2013-08-28 薛运河 Wet-to-dry dispersant-free method for producing ultrafine nanoscale dry powder and involved device
CN111268716A (en) * 2020-04-01 2020-06-12 昂星新型碳材料常州有限公司 Carbon material-coated tetrapod-like zinc oxide, carbon material with hollow tetrapod-like structure, filling mold and preparation method thereof
CN113303337A (en) * 2021-06-02 2021-08-27 吴江市威士达铜业科技有限公司 Production method of copper calcium sulfate
CN214681698U (en) * 2020-12-30 2021-11-12 深圳市祺鑫环保科技有限公司 Preparation device of copper oxide powder

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20120047340A (en) * 2010-10-20 2012-05-14 서안켐텍 주식회사 Process for preparing cupric oxide powder for electric plating
CN102951671A (en) * 2012-10-22 2013-03-06 洛阳师范学院 Preparation method of copper oxide nano particle
CN103263963A (en) * 2013-04-22 2013-08-28 薛运河 Wet-to-dry dispersant-free method for producing ultrafine nanoscale dry powder and involved device
CN111268716A (en) * 2020-04-01 2020-06-12 昂星新型碳材料常州有限公司 Carbon material-coated tetrapod-like zinc oxide, carbon material with hollow tetrapod-like structure, filling mold and preparation method thereof
CN214681698U (en) * 2020-12-30 2021-11-12 深圳市祺鑫环保科技有限公司 Preparation device of copper oxide powder
CN113303337A (en) * 2021-06-02 2021-08-27 吴江市威士达铜业科技有限公司 Production method of copper calcium sulfate

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