CN101698499A - Preparation method of electronic grade high-purity blue copperas - Google Patents
Preparation method of electronic grade high-purity blue copperas Download PDFInfo
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- CN101698499A CN101698499A CN200910193421A CN200910193421A CN101698499A CN 101698499 A CN101698499 A CN 101698499A CN 200910193421 A CN200910193421 A CN 200910193421A CN 200910193421 A CN200910193421 A CN 200910193421A CN 101698499 A CN101698499 A CN 101698499A
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Abstract
The invention relates to a preparation method of electronic grade high-purity blue copperas; the preparation method comprises the following steps: copper mine is crushed by degreasing treatment and is placed in a vessel, sulfuric acid, of which the quality equals to 4-5 times of copper mine quality, is added under 40-50DEG C condition, and then aqueous hydrogen peroxide solution with 20-40 percent of mass percentage concentration is dropwise added, after the reaction is carried out for 25-35min, the reaction liquid is heated and concentrated until cottony substances appear, the cottony substances are removed by filtration, and then the concentration is carried out continuously, so as to obtain blue copperas crystallization. In the preparation process, foreign ions are not led in, the purity and quality of the product can not be affected, and the product crystal form is integral; in addition, the process is simple and the cost is low, therefore, the preparation method is suitable for large-scale industrial production.
Description
Technical field
The invention belongs to new chemical material and preparing technical field thereof, particularly a kind of preparation method of electronic grade high-purity blue copperas.
Background technology
Cupric sulfate pentahydrate is commonly called as blue stone, and lapis divinus or blue vitriol are a kind of important inorganic chemical products, and its purposes is different with purity.Analytical pure, chemical pure cupric sulfate pentahydrate all use for chemical reagent, and the technical grade cupric sulfate pentahydrate is in petrochemical complex, and departments such as plating have been widely used, and are the important source material that is used for producing other mantoquita in chemical industry.The mordant that also can be used for cotton textiles is made green and blue dyes; Wood preservative, the sterilant of water.Be used for fruit tree on the agricultural, the sterilant of farm crop such as cotton, fodder additives, and be used for flotation of non-ferrous metal etc. in a large number.
The cupric sulfate pentahydrate production technique is broadly divided into two kinds by raw material sources: being raw material production with copper mine stone 1), is that raw material production copper sulfate generally can adopt the dilute sulphuric acid direct leaching with copper mine stone, and this method mainly is at being raw material production with the oxidized ore; 2) with useless red copper or copper-bearing waste material production, adopt high-temperature roasting dilute sulphuric acid lixiviation process, this method is primarily aimed at sulphide ores or the oxidized ore of sulphide ores association is arranged is raw material production.These two kinds of methods are owing to reasons such as Mineral resources or environmental pollutions, and application is restricted.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art part, the object of the present invention is to provide a kind of preparation method of electronic grade high-purity blue copperas.Technology of the present invention is simple, and is with low cost, is fit to large-scale commercial production.
Purpose of the present invention is achieved through the following technical solutions: a kind of preparation method of electronic grade high-purity blue copperas comprises following operation steps:
Copper mine after handling, is pulverized in degreasing, place container, the sulfuric acid that under 40～50 ℃ of conditions, adds 4～5 times of copper mine quality, drip mass percent concentration then and be 20～40% aqueous hydrogen peroxide solution, behind reaction 25～35min, the reaction solution heating is concentrated into the cotton shape material has occurred, removed by filter the cotton shape material, continue again to concentrate, obtain the cupric sulfate pentahydrate crystallization.
Described vitriolic volumetric molar concentration is 1～3mol/L.
The present invention compared with prior art has following advantage and beneficial effect: (1) the inventive method does not need to adopt high energy consumption treatment steps such as electrolysis, displacement, has reduced energy consumption and cost, has improved economic benefit; (2) do not introduce foreign ion in the preparation process, can not influence the purity and the quality of product; The purity of prepared cupric sulfate pentahydrate reaches more than 25.2% in the mass percent of cupric ion, the content of metallic impurity Cr, Ca, Mg, As, K, Cd all below 5ppm, the product complete in crystal formation; (3) parameter that is adopted in the inventive method comprises the relation of measuring between temperature of reaction, reaction times and the material, has definitely guaranteed the high-quality of gained potassium pyrophosphate product; (4) technology of the present invention is simple, and abundant raw material is with low cost, and is low in the pollution of the environment.
Embodiment
The present invention is described in further detail below in conjunction with embodiment and accompanying drawing, but embodiments of the present invention are not limited thereto.
Embodiment 1
Copper mine after handling, is pulverized in degreasing, get 50 grams and place container, adding volumetric molar concentration under 40 ℃ of conditions is 1mol/L sulfuric acid 250mL, drips mass percent concentration then and be 20% aqueous hydrogen peroxide solution, behind the reaction 25min, after reaction finishes, solution is decanted in the furnace pot, and heating has been concentrated into the cotton shape material and has occurred, and removes by filter the cotton shape material, continue again to concentrate, obtain the cupric sulfate pentahydrate crystallization.
After testing, this cupric sulfate pentahydrate crystalline purity reaches 25.4% in the mass percent of cupric ion, the content of metallic impurity Cr, Ca, Mg, As, K and Cd all≤5ppm.
Embodiment 2
Copper mine after handling, is pulverized in degreasing, get 20 grams and place container, adding volumetric molar concentration under 45 ℃ of conditions is 3mol/L sulfuric acid 100mL, drips mass percent concentration then and be 30% aqueous hydrogen peroxide solution, behind the reaction 35min, after reaction finishes, solution is decanted in the furnace pot, and heating has been concentrated into the cotton shape material and has occurred, and removes by filter the cotton shape material, continue again to concentrate, obtain the cupric sulfate pentahydrate crystallization.
After testing, this cupric sulfate pentahydrate crystalline purity reaches 25.3% in the mass percent of cupric ion, the content of metallic impurity Cr, Ca, Mg, As, K and Cd all≤5ppm.
Embodiment 3
Copper mine after handling, is pulverized in degreasing, get 30 grams and place container, adding volumetric molar concentration under 45 ℃ of conditions is 2mol/L sulfuric acid 130mL, drips mass percent concentration then and be 40% aqueous hydrogen peroxide solution, behind the reaction 30min, after reaction finishes, solution is decanted in the furnace pot, and heating has been concentrated into the cotton shape material and has occurred, and removes by filter the cotton shape material, continue again to concentrate, obtain the cupric sulfate pentahydrate crystallization.
After testing, this cupric sulfate pentahydrate crystalline purity reaches 25.5% in the mass percent of cupric ion, the content of metallic impurity Cr, Ca, Mg, As, K and Cd all≤5ppm.
Embodiment 4
Copper mine after handling, is pulverized in degreasing, get 25 grams and place container, adding volumetric molar concentration under 47 ℃ of conditions is 2.5mol/L sulfuric acid 150mL, drips mass percent concentration then and be 35% aqueous hydrogen peroxide solution, behind the reaction 28min, after reaction finishes, solution is decanted in the furnace pot, and heating has been concentrated into the cotton shape material and has occurred, and removes by filter the cotton shape material, continue again to concentrate, obtain the cupric sulfate pentahydrate crystallization.
After testing, this cupric sulfate pentahydrate crystalline purity reaches 25.5% in the mass percent of cupric ion, the content of metallic impurity Cr, Ca, Mg, As, K and Cd all≤5ppm.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and the principle, substitutes, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (2)
1. the preparation method of an electronic grade high-purity blue copperas is characterized in that comprising following operation steps:
Copper mine after handling, is pulverized in degreasing, place container, the sulfuric acid that under 40～50 ℃ of conditions, adds 4～5 times of copper mine quality, drip mass percent concentration then and be 20～40% aqueous hydrogen peroxide solution, behind reaction 25～35min, the reaction solution heating is concentrated into the cotton shape material has occurred, removed by filter the cotton shape material, continue again to concentrate, obtain the cupric sulfate pentahydrate crystallization.
2. the preparation method of a kind of electronic grade high-purity blue copperas according to claim 1, it is characterized in that: described vitriolic volumetric molar concentration is 1～3mol/L.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN200910193421A CN101698499A (en) | 2009-10-29 | 2009-10-29 | Preparation method of electronic grade high-purity blue copperas |
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| Application Number | Priority Date | Filing Date | Title |
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| CN200910193421A CN101698499A (en) | 2009-10-29 | 2009-10-29 | Preparation method of electronic grade high-purity blue copperas |
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| CN101698499A true CN101698499A (en) | 2010-04-28 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058258A (en) * | 2012-12-29 | 2013-04-24 | 广东光华科技股份有限公司 | Preparation method for electronic grade high-purity copper sulfate pentahydrate |
| CN107986317A (en) * | 2017-11-16 | 2018-05-04 | 厦门建霖健康家居股份有限公司 | A kind of preparation method of cupric sulfate purified |
| CN112357947A (en) * | 2020-12-21 | 2021-02-12 | 泰兴冶炼厂有限公司 | Preparation method for producing high-purity anhydrous copper sulfate by dynamic drying method |
| CN114318436A (en) * | 2022-03-09 | 2022-04-12 | 深圳市创智成功科技有限公司 | Preparation method of high-purity copper sulfate for wafer copper interconnection and copper electroplating process thereof |
-
2009
- 2009-10-29 CN CN200910193421A patent/CN101698499A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058258A (en) * | 2012-12-29 | 2013-04-24 | 广东光华科技股份有限公司 | Preparation method for electronic grade high-purity copper sulfate pentahydrate |
| CN107986317A (en) * | 2017-11-16 | 2018-05-04 | 厦门建霖健康家居股份有限公司 | A kind of preparation method of cupric sulfate purified |
| CN107986317B (en) * | 2017-11-16 | 2022-06-21 | 厦门建霖健康家居股份有限公司 | Preparation method of electroplating-grade copper sulfate |
| CN112357947A (en) * | 2020-12-21 | 2021-02-12 | 泰兴冶炼厂有限公司 | Preparation method for producing high-purity anhydrous copper sulfate by dynamic drying method |
| CN114318436A (en) * | 2022-03-09 | 2022-04-12 | 深圳市创智成功科技有限公司 | Preparation method of high-purity copper sulfate for wafer copper interconnection and copper electroplating process thereof |
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Open date: 20100428 |