CN101195497A - Process for producing cupric hydroxide or cupric oxide - Google Patents
Process for producing cupric hydroxide or cupric oxide Download PDFInfo
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- CN101195497A CN101195497A CNA2006101190456A CN200610119045A CN101195497A CN 101195497 A CN101195497 A CN 101195497A CN A2006101190456 A CNA2006101190456 A CN A2006101190456A CN 200610119045 A CN200610119045 A CN 200610119045A CN 101195497 A CN101195497 A CN 101195497A
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Abstract
The invention discloses a process for preparing copper hydroxide or copper oxide. Soluble cupriferous ions (cupric nitrate, copper chloride and copper sulphate) generated in the production of wiring boards are taken as raw materials to be synthesized with ammonium ions of basic copper chloride or sodium hydroxide to generate basic copper salt (basic copper nitrate, basic copper sulphate and basic copper chloride), furthermore, products of basic copper salt reacts with the sodium hydroxide to generate copper hydroxide or copper oxide, and glycerin as stabilizing agent is added in. .The process of preparation has the advantages of stable products, easy washing, high purity, easy raw material achievement, high absorption rate and little environmental pollution.
Description
Technical field
The present invention relates to the preparation method of a kind of copper hydroxide or cupric oxide.
Background technology
Copper hydroxide is a kind of important catalyst, industrial chemicals and pesticide material, and the synthetic method of copper hydroxide mainly is by two kinds at present: first kind is to generate copper hydroxide when becoming copper sulfate ammonium ion repeated hydrogenation sodium oxide with copper sulfate and ammonia synthesis.This technology cost height, excess of ammonia and cuprammonium ionic soil are heavy, and productive rate is low, the present domestic scale operation that do not form.Second kind is to carry out the neutralization reaction generation with solubility chlorination cupric ion that produces in the circuit board industrial and alkaline cupric chloride ammonium ion to contain a large amount of copper hydroxide products based on basic copper chloride, can't generate purer copper hydroxide, the product that in fact this technology the produce copper hydroxide of to say so, can only think to contain the basic copper chloride copper sludge of copper hydroxide, the product of this method production can not use as copper hydroxide at present, but is used to produce the basic material and the copper smelting industry of Chemicals such as cuprous chloride as copper-containing raw material.
At present the main application of copper hydroxide product is agricultural chemicals and mantoquita Chemical market, and this market demand purity is greater than 98% copper hydroxide, and fineness can effectively be controlled to reach and is difficult for precipitation.Because production technology does not reach the purity of market demand, so the content among the Q/HG22-2032-82 of domestic standard Shanghai can only be decided to be 95%, can't formulate content greater than 98% in the past, so can't satisfy market demand, we have carried out big quantity research for this reason.
Summary of the invention
Studies show that, adopting synthetic copper hydroxide of branch two step method or cupric oxide mainly is that the first step reaction is the solubility cupric nitrate that produces during wiring board is produced, the copper ions of cupric chloride and copper sulfate and solubility chlorination cuprammonium ion or sodium hydroxide reaction generate insoluble basic copper nitrate, Basic Chrome Sulphate and basic copper chloride, just be easy to solubility chlorination ammonium or the sodium chloride solution of reaction by-product separated through centrifugal or press filtration this moment, again will be through the basic copper nitrate after the washing, Basic Chrome Sulphate and basic copper chloride and aqueous sodium hydroxide solution reaction generate copper hydroxide or cupric oxide, in the slurry of moisture copper hydroxide, add glycerine as stablizer, after air stream drying or drying room drying, be finished product.
Separate through mother liquor owing to having produced side product sodium chloride after synthetic in the above-mentioned reaction, avoided the side reaction of generation when back road alkali type nantokite and sodium hydroxide reaction, be that ammonium chloride and sodium hydroxide can generate sodium-chlor and ammonia, cause ammonia to pollute and consume sodium hydroxide, simultaneously excessive sodium-chlor and ammonium chloride can be adsorbed on the copper hydroxide and cause the content of copper hydroxide on the low side and to produce color be abnormal grey black.
Description of drawings
Fig. 1 is preparation method's process flow sheet of copper hydroxide of the present invention or cupric oxide.
Embodiment
Below in conjunction with specific embodiment copper hydroxide preparation method of the present invention is described in further detail.
As shown in Figure 1, to be that 1～30% solution is placed in the container 1 after filtration by the solubility cupric of the cupric nitrate that produces in the wiring board production, copper sulfate or cupric chloride, be 1～30% alkaline cupric chloride cuprammonium ion with cupric or be that 1～45% sodium hydroxide solution is placed in the container 2 after filtering, in reactor 4, the solution in two containers is added under stirring state simultaneously
When the PH in the molten device be controlled at 4.5～9 and liquor capacity in reactor 4 rise to 2000L and begin to open reactor 4 end opening baiting valves in charging reaction limit, limit when above, open that the press filtration pump carries out press filtration or whizzer is centrifugal, be washed with water to PH6～8, unload basic copper nitrate or Basic Chrome Sulphate or basic copper chloride and place it in and add water in the reactor 5 earlier to break into pulpous state stand-by.Adding sodium hydroxide and water in container 3, to be made into content be 1～45% aqueous sodium hydroxide solution, add in the reactor 5 then while stirring, the total amount that adds sodium hydroxide be copper hydroxide 20% in, the content of sodium hydroxide is controlled in 20% in the aqueous solution.The reinforced restir 2 hours of finishing, add glycerine this moment in reactor 5, add-on is 0～20% of a copper hydroxide total amount, open reactor 5 end opening baiting valves this moment, open that press filtration pump 6 carries out press filtration or whizzer is centrifugal, the aqueous solution that preparation contains 0～10% glycerine in reactor 5 is used to wash to PH6～8, unloads the copper hydroxide wet feed, in air stream drying or drying room 7, carry out the dry hydrogen cupric oxide, analyze qualified back packing warehouse-in then.
Claims (6)
1. the preparation method of copper hydroxide or cupric oxide, by the solubility cupric of the cupric nitrate that produces in the wiring board production, copper sulfate or cupric chloride is that the sodium hydroxide solution that 1～30% solution and cupric are 1～30% alkaline cupric chloride cuprammonium ion or 1～45% reacts at aqueous phase, makes basic copper nitrate, Basic Chrome Sulphate or basic copper chloride product; Basic copper nitrate, Basic Chrome Sulphate or basic copper chloride product after by-product solubility chlorination ammonium or the sodium-chlor separation are reacted with sodium hydroxide again, make copper hydroxide or cupric oxide; Add glycerine as stablizer in washing water or wet copper hydroxide, add-on is 0～20% of a copper hydroxide amount, makes stable form high purity content after drying greater than 98% copper hydroxide.
2. the preparation method of copper hydroxide as claimed in claim 1 is characterized in that: describedly reacted at aqueous phase by soluble copper salts such as cupric nitrate, copper sulfate and cupric chloride and alkaline cupric chloride ammonium ion or sodium hydroxide.
3. the preparation method of copper hydroxide as claimed in claim 1, it is characterized in that: the intermediate product that described reaction obtains is alkali type nantokites such as basic copper nitrate, basic copper chloride, Basic Chrome Sulphate.
4. the preparation method of copper hydroxide as claimed in claim 1 is characterized in that: described reaction generates alkali type nantokites such as water-fast basic copper nitrate, basic copper chloride, Basic Chrome Sulphate and separates with reaction by-product salt.
5. the preparation method of copper hydroxide as claimed in claim 1 or cupric oxide is characterized in that: described basic copper nitrate, basic copper chloride, Basic Chrome Sulphate and aqueous sodium hydroxide solution reaction generate copper hydroxide or cupric oxide.
6. the preparation method of copper hydroxide as claimed in claim 1 is characterized in that: described product copper hydroxide adds glycerine as stablizer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200610119045A CN101195497B (en) | 2006-12-04 | 2006-12-04 | Process for producing cupric hydroxide or cupric oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN200610119045A CN101195497B (en) | 2006-12-04 | 2006-12-04 | Process for producing cupric hydroxide or cupric oxide |
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| Publication Number | Publication Date |
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| CN101195497A true CN101195497A (en) | 2008-06-11 |
| CN101195497B CN101195497B (en) | 2012-10-03 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN200610119045A Active CN101195497B (en) | 2006-12-04 | 2006-12-04 | Process for producing cupric hydroxide or cupric oxide |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633290A (en) * | 2012-03-26 | 2012-08-15 | 廖勇志 | Preparation method for basic copper nitrate |
| CN103011253A (en) * | 2012-12-21 | 2013-04-03 | 嘉兴德达资源循环利用有限公司 | Method for preparing copper hydroxide with copper ammonia etching waste liquid |
| CN103466683A (en) * | 2013-09-12 | 2013-12-25 | 昆山德阳新材料科技有限公司 | Preparation method of high-purity electroplating-grade copper oxide |
| CN103739000A (en) * | 2013-12-25 | 2014-04-23 | 广州科城环保科技有限公司 | Production method of high-purity electroplating grade copper oxide |
| CN104297415A (en) * | 2014-10-27 | 2015-01-21 | 扬州协鑫光伏科技有限公司 | Detection method for glycerin content in cutting fluid |
| CN106673048A (en) * | 2017-03-24 | 2017-05-17 | 东莞市广华化工有限公司 | Method for converting basic copper chloride into basic copper carbonate |
| CN107381746A (en) * | 2017-08-23 | 2017-11-24 | 华南理工大学 | A kind of method for being removed in waste water and reclaiming copper |
| CN109845759A (en) * | 2019-03-15 | 2019-06-07 | 威海市农业科学院 | A kind of Bordeaux mixture and preparation method, application method of improvement |
| CN111847496A (en) * | 2020-06-23 | 2020-10-30 | 吴江市威士达铜业科技有限公司 | Preparation method of stable-state copper hydroxide |
| CN114516654A (en) * | 2022-02-09 | 2022-05-20 | 广州科城环保科技有限公司 | Preparation method of modified copper hydroxide and modified copper hydroxide prepared by same |
| CN114959732A (en) * | 2022-06-15 | 2022-08-30 | 昆明理工大学 | Preparation method and purification process of copper hydroxide |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1047069A (en) * | 1989-05-12 | 1990-11-21 | 叶远安 | Alikali cupric carbonate produced by boiling water |
| CN1082004A (en) * | 1992-08-12 | 1994-02-16 | 黄石市能源综合科学技术研究所 | Produce a kind of efficient process of ventilation breather or cupric oxide |
| CN1172074A (en) * | 1997-08-15 | 1998-02-04 | 张礼英 | Preparation method of cupric oxide or cupric sulfate using copper sheathed steel by ammonia immersion |
-
2006
- 2006-12-04 CN CN200610119045A patent/CN101195497B/en active Active
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102633290A (en) * | 2012-03-26 | 2012-08-15 | 廖勇志 | Preparation method for basic copper nitrate |
| CN103011253A (en) * | 2012-12-21 | 2013-04-03 | 嘉兴德达资源循环利用有限公司 | Method for preparing copper hydroxide with copper ammonia etching waste liquid |
| CN103466683B (en) * | 2013-09-12 | 2015-11-25 | 昆山德阳新材料科技有限公司 | A kind of preparation method of high-purity electroplating-gradecopper copper oxide |
| CN103466683A (en) * | 2013-09-12 | 2013-12-25 | 昆山德阳新材料科技有限公司 | Preparation method of high-purity electroplating-grade copper oxide |
| CN103739000A (en) * | 2013-12-25 | 2014-04-23 | 广州科城环保科技有限公司 | Production method of high-purity electroplating grade copper oxide |
| CN103739000B (en) * | 2013-12-25 | 2015-11-18 | 广州科城环保科技有限公司 | A kind of production method of high-purity plating-grade copper oxide |
| CN104297415A (en) * | 2014-10-27 | 2015-01-21 | 扬州协鑫光伏科技有限公司 | Detection method for glycerin content in cutting fluid |
| CN104297415B (en) * | 2014-10-27 | 2016-08-24 | 扬州协鑫光伏科技有限公司 | The detection method of glycerin components in cutting liquid |
| CN106673048A (en) * | 2017-03-24 | 2017-05-17 | 东莞市广华化工有限公司 | Method for converting basic copper chloride into basic copper carbonate |
| CN107381746A (en) * | 2017-08-23 | 2017-11-24 | 华南理工大学 | A kind of method for being removed in waste water and reclaiming copper |
| CN109845759A (en) * | 2019-03-15 | 2019-06-07 | 威海市农业科学院 | A kind of Bordeaux mixture and preparation method, application method of improvement |
| CN111847496A (en) * | 2020-06-23 | 2020-10-30 | 吴江市威士达铜业科技有限公司 | Preparation method of stable-state copper hydroxide |
| CN114516654A (en) * | 2022-02-09 | 2022-05-20 | 广州科城环保科技有限公司 | Preparation method of modified copper hydroxide and modified copper hydroxide prepared by same |
| CN114516654B (en) * | 2022-02-09 | 2024-02-27 | 广州科城环保科技有限公司 | Preparation method of modified copper hydroxide and modified copper hydroxide prepared by preparation method |
| CN114959732A (en) * | 2022-06-15 | 2022-08-30 | 昆明理工大学 | Preparation method and purification process of copper hydroxide |
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| CN101195497B (en) | 2012-10-03 |
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