Preparation method of cubic micro/nano cuprous oxide powder

A cuprous oxide, micro-nano technology, which is applied in the preparation of high-purity ultra-fine cuprous oxide powder and the preparation of cubic micro-nano cuprous oxide powder, can solve the problems of high raw material cost, high local pH value, explosiveness, etc., and achieve The process is easy to control, the specific surface area is small, and the bulk density is small

Active Publication Date: 2015-05-06
GUANGDONG GUANGHUA SCI TECH
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Problems solved by technology

Chinese patent application (CN104030339A) discloses a method for preparing cubic cuprous oxide nanomaterials. The method uses copper sulfate pentahydrate as the copper source and glucose as the reducing agent. The cuprous oxide material with the appearance of the cuprous oxide, because the method adds a strong alkali to the reaction solution, it is easy to cause the local pH value to be too high, and the specific surface area of ​​the prepared cuprous oxide is large, which is not conducive to the control of the shape, and is not suitable for antifouling of ships. Coatings, in addition, use glucose as a reducing agent, the cost is too high, from the perspective of industrialization, it is unrealistic
Chinese patent (101412530A) discloses a preparation method of using organic additives to control the external morphology of cuprous oxide crystals. The method uses sodium lactate as a copper salt complexing agent and reducing agent to prepare cuprous oxide crystals in a hydrothermal environment. Control the type and dosage of organic additives to realize the shape control of cuprous oxide. Adding acetone can prepare cubic cuprous oxide, but this method needs to add a large amount of organic solvent, and the organic solvent is flammable, explosive and toxic. , which brings great danger and difficulty to production, storage, transportation and use
In addition, the liquid-phase reduction method mostly uses copper sulfate as the raw material. Due to the high cost of raw materials, the industrialization process of the liquid-phase reduction method is limited, and the printed circuit board (PCB) is a basic component of electronic products. With the rapid development of the electronic information industry , the demand for printed circuit boards is also increasing. During the production process of printed circuit boards, 80% to 90% of the copper foil is removed by etching solution. As the proportion of copper in the etching solution reaches a certain level, the etching solution cannot meet the requirements. Make needs and become waste liquid, how to recycle these waste liquids is also the topic that the applicant of the present invention is committed to researching.

Method used

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  • Preparation method of cubic micro/nano cuprous oxide powder
  • Preparation method of cubic micro/nano cuprous oxide powder
  • Preparation method of cubic micro/nano cuprous oxide powder

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Experimental program
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Effect test

Embodiment 1

[0023] (1) Mix the acidic etching waste liquid and alkaline etching waste liquid recovered from printed circuit boards in a certain proportion, control the pH of the copper liquid after mixing at 3.0, and prepare Cu by concentrating or replenishing water. 2+ Concentration is the copper liquid A of 100g / L;

[0024] (2) Dissolve sodium carbonate and sodium sulfite in water respectively, and prepare sodium carbonate solution B with a concentration of 200g / L and sodium sulfite solution C with a concentration of 200g / L;

[0025] (3) Take 500mL of solution A, stir and preheat to 50°C, add 0.8g of composite dispersant, the composite dispersant is gelatin and sodium dodecylbenzenesulfonate with a mass ratio of 1:1;

[0026] (4) Quickly add 750mL solution C to the solution in step (3), slowly add solution B dropwise, control the pH value of the reaction solution to 4.5, continue to stir and heat to 90°C;

[0027] (5) After 2 hours of reaction, filter the collected reaction final produ...

Embodiment 2

[0029] (1) Mix the acidic etching solution recovered from the printed circuit board with the alkaline etching waste solution in a certain proportion, control the pH of the mixed copper solution at 3.0, and prepare Cu by concentrating or replenishing water. 2+ Concentration is the copper liquid A of 120g / L;

[0030] (2) Dissolve sodium carbonate and sodium sulfite in water respectively to prepare sodium carbonate solution B with a concentration of 210g / L and sodium sulfite solution C with a concentration of 200g / L.

[0031] (3) Take 500mL of solution A, stir and preheat to 45°C, add 0.5g of composite dispersant, the composite dispersant is gelatin and sodium dodecylbenzenesulfonate with a mass ratio of 1:1;

[0032] (4) Quickly add 700mL solution C to the solution in step (3), slowly add solution B dropwise, control the pH value of the reaction solution to 4.5, continue to stir and heat to 83°C;

[0033] (5) After reacting for 2.5 hours, filter the collected reaction final pro...

Embodiment 3

[0035] (1) Mix the acidic etching solution recovered from the printed circuit board with the alkaline etching waste solution in a certain proportion, control the pH of the mixed copper solution at 2.5, and prepare Cu by concentrating or replenishing water. 2+ Concentration is copper liquid A of 90g / L;

[0036] (2) Dissolve sodium carbonate and sodium sulfite in water respectively, and prepare sodium carbonate solution B with a concentration of 190g / L and sodium sulfite solution C with a concentration of 200g / L;

[0037] (3) Take 500mL of solution A, stir and preheat to 50°C, add 1g of composite dispersant, the composite dispersant is gelatin and sodium dodecylbenzenesulfonate with a mass ratio of 1:1;

[0038] (4) Quickly add 800mL solution C to the solution in step (3), slowly add solution B dropwise, control the pH of the reaction solution to 3.5, continue to stir and heat to 100°C;

[0039](5) After reacting for 4 hours, filter the collected reaction final product, wash it...

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Abstract

The invention provides a preparation method of cubic micro/nano cuprous oxide powder suitable for ship antifouling paints, which comprises the following steps: preparing a copper solution with certain concentration and pH value, preheating to 40-50 DEG C while stirring, adding a composite dispersing agent, quickly adding a sodium sulfite solution with certain concentration, slowly and dropwisely adding a sodium carbonate solution to control the pH value of the reaction solution, continuing heating to 60-100 while stirring, reacting for 1-5 hours, and carrying out solid-liquid separation, washing and drying on the collected reaction end product to obtain the cubic micro/nano cuprous oxide powder, wherein the composite dispersing agent is prepared from gelatin and sodium dodecyl benzene sulfonate in a mass ratio of 1:1. The preparation method is simple to operate and controllable in technique. The cuprous oxide powder prepared by the method is cubic, has the particle size of 0.4-3.0 mu m, has the advantages of small specific area, slow release of copper ions, low bulk density, favorable suspensibility and low oil absorption, and is especially suitable to be used in ship antifouling paints.

Description

technical field [0001] The invention relates to a method for preparing cuprous oxide, in particular to a method for preparing high-purity ultrafine cuprous oxide powder, and more particularly to a method for preparing cubic micronano cuprous oxide powder suitable for ship antifouling coatings. Background technique [0002] Cuprous oxide (Cu 2 O) Powder is a red or yellow inorganic chemical raw material and product, which is widely used, such as ship antifouling coatings, glass enamel colorants, organic synthesis catalysts, pesticide fungicides and electronic materials, etc., of which more than 80% are used in Marine antifouling coatings. [0003] The prevention and control of marine fouling organisms has always been a matter of great concern to ships, marine bioengineers and biologists, especially the biofouling at the bottom of the ship, which not only increases the ship's navigation resistance, reduces the speed of the ship, increases fuel consumption, but also acc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G3/02B82Y40/00
CPCC01G3/02C01P2004/03C01P2004/38C01P2004/61C01P2004/62
Inventor 谭泽黄司平陈锐宋陈汉昭王胜广何为
Owner GUANGDONG GUANGHUA SCI TECH
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