# US 10,479,694 B2 · Process of clean production of electronic grade high-purity copper oxide

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- Number: US 10,479,694 B2
- Document ID: US10479694B2
- Status: Granted
- Kind: B2
- Application number: 15/871,147
- Filed: 2018-01-15
- Published: 2018-06-28
- Granted: 2019-11-19
- Earliest claimed: 2016-12-23
- Applicants: Guangdong Guanghua Sci-Tech Co., Ltd.; Guangdong Toneset Science & Technology Co., Ltd.
- Inventors: Ze Tan; Siping Huang; Yilang Zhou; Wei He; Chong Wang; Haiyan Lu
- Web page: https://patentgrep.com/patent/US10479694B2

## CPC

- C01G 3/02: Oxides; Hydroxides
- B01D 21/262: {by using a centrifuge}
- C01C 1/185: {Preparation}
- C01C 1/242: Preparation from ammonia and sulfuric acid or sulfur trioxide
- C01P 2006/80: Compositional purity
- C01G: COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F (metal hydrides {monoborane, diborane or addition complexes thereof} C01B6/00; salts of oxyacids of halogens C01B11/00; peroxides, salts or peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium, or tellurium C01B19/00; binary compounds of nitrogen with metals C01B21/06; azides C01B21/08; {compounds containing nitrogen, other non-metals and metal C01B21/082}; metal amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; carbides C01B32/90; compounds containing silicon C01B33/00; compounds containing boron C01B35/00; compounds having molecular sieve properties but not having base-exchange properties C01B37/00; compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites, C01B39/00; cyanides C01C3/08; salts of cyanamide C01C3/16; thiocyanates C01C3/20)
- B01D: SEPARATION (separating solids from solids by wet methods B03B, B03D; by pneumatic jigs or tables B03B; by other dry methods B07; magnetic or electrostatic separation of solid materials from solid materials or fluids, separation by high-voltage electric fields B03C; centrifuges, vortex apparatus B04; presses per se for squeezing-out liquid from liquid-containing material B30B9/02; treatment of water C02F, e.g. softening by ion-exchange C02F1/42; {arrangements of air intake cleaners in gas turbine plants F02C7/05} ; arrangements or mounting of filters in air-conditioning, air-humidification or ventilation F24F13/28)
- C01C: AMMONIA; CYANOGEN; COMPOUNDS THEREOF ({metal hydrides, monoborane, diborane or addition complexes thereof C01B6/00}; salts of oxyacids of halogens C01B11/00; peroxides, salts of peroxyacids C01B15/00; thiosulfates, dithionites, polythionates C01B17/64; compounds containing selenium or tellurium C01B19/00; azides C01B21/08; {compounds other than ammonia or cyanogen, containing nitrogen, non-metals and optionally metals C01B21/082}; metal imides or amides C01B21/092; nitrites C01B21/50; {compounds of noble gases C01B23/0005}; phosphides C01B25/08; salts of oxyacids of phosphorus C01B25/16; compounds containing silicon C01B33/00; compounds containing boron C01B35/00)
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

The present disclosure provides a process of clean production of electronic grade high-purity copper oxide. The process includes (1) preparing a carbon-ammonia system solution with a certain ratio of CO2, NH3 and H2O; (2) dissolving copper under a slightly negative pressure and at a system temperature less than or equal to 60° C.; the reaction ends until the concentration of copper in the carbon-ammonia system solution reaches 80 to 140 g/L; (3) adding sodium polyacrylate; the reaction solution is heated to 60-80° C. under a reduced pressure for deamination; (4) disposing basic copper carbonate to separate the solid from the liquid by a centrifuge to give an filter cake and copper-containing clear solution; (5) calcining the filter cake at 250-600° C. for 1-5 hours to give an electronic grade high purity copper oxide; ammonia collected in step (3), the copper-containing clear solution collected in step (4), and carbon dioxide and water vapor collected in step (5) are transferred to the solution-preparing device of step (1) and directly used as raw materials for preparing carbonate-ammonia system solution, wherein the copper-containing clear solution is used as water. The process of production of the disclosure has a shortened processing line and a low energy consumption; it is not only cost saving but also can achieve goals of energy saving, reduced emission and environment pollution.

## Claims

### Claim 1

A process of clean production of an electronic grade high-purity copper oxide, comprising the following steps in sequence:
(1) continuously preparing a carbon-ammonia system solution, wherein the molar ratio of CO2:NH3:H2O is 1:1.3-2:17-20;
(2) adding the carbon-ammonia system solution into a reaction vessel preloaded with metallic copper, and constantly inputting air, oxygen or ozone under a negative pressure of between −0.01 and −0.02 Mpa to keep the temperature of the reaction system equal to or less than 60° C.; the negative pressure is closed when the concentration of copper in the carbon-ammonia system solution reaches 80-140 g/L;
(3) filtering the copper, carbon-ammonia system solution to a reaction kettle for deamination, adding sodium polyacrylate to obtain a reaction solution after stirring evenly; the reaction solution is heated to a temperature of 60-80° C. under a pressure of between −0.03 and −0.08 MPa for deamination and ammonia water is collected during deamination, wherein the sodium polyacrylate is added in an amount of 0.2-0.6 g/L based on a volume of the copper, carbon-ammonia system solution filtrate;
(4) separating solid from liquid by a centrifuge obtaining a copper carbonate including copper and collecting a copper-containing clear solution;
(5) calcining the copper carbonate at a temperature of 250-600° C. for 1-5 hours to give an electronic grade high-purity copper oxide, and carbon dioxide and water vapor are produced during the calcination; the ammonia water collected in the above step (3), the copper-containing clear solution collected in the step (4) and carbon dioxide and water vapor collected in the step (5) are directly used as raw materials to prepare the carbon-ammonia system solution, wherein the copper-containing clear solution is used as water.

### Claim 2 (depends on 1)

The process of clean production of the electronic grade high-purity copper oxide according to the claim 1, wherein the carbon-ammonia system solution of the above step (1) is prepared by firstly adding the ammonia water and then introducing carbon dioxide, which is followed by spraying with the copper-containing clear solution and/or pure water, and the procedure is a continuous closed-loop operation.

### Claim 3 (depends on 1)

The process of clean production of the electronic grade high-purity copper oxide according to the claim 1, wherein the water vapor collected in the above step (5), after dust removing, is added along with carbon dioxide by a fan.

### Claim 4 (depends on 3)

The process of clean production of the electronic grade high-purity copper oxide according to the claim 3, wherein ammonia gas volatilized during dissolving copper in the above step (2) is added by the fan to form a part of the closed-loop operation for recycling.

### Claim 5 (depends on 4)

The process of clean production of the electronic grade high-purity copper oxide according to the claim 4, wherein micro-amount ammonia gas generated in the above steps due to the problem of airtightness is uniformly recycled by a gas-collecting hood, and then absorbed by circulating spray of a dilute acid spraying solution to give analytically pure ammonium salt.

### Claim 6 (depends on 5)

The process of clean production of the electronic grade high-purity copper oxide according to the claim 5, wherein the dilute acid spraying solution is sulfuric acid, nitric acid or acetic acid.