CN104163449A - Preparation method of gamma-copper iodide - Google Patents
Preparation method of gamma-copper iodide Download PDFInfo
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- CN104163449A CN104163449A CN201410402480.4A CN201410402480A CN104163449A CN 104163449 A CN104163449 A CN 104163449A CN 201410402480 A CN201410402480 A CN 201410402480A CN 104163449 A CN104163449 A CN 104163449A
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- iodine
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- hydrazine hydrate
- cuprous iodide
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Abstract
The invention discloses a preparation method of gamma-copper iodide. The preparation method comprises the following steps: adding iodine into water so as to obtain an iodic aqueous solution and adding hydrazine hydrate into the iodic aqueous solution for mixed reaction to obtain an iodide ion solution, wherein the molar ratio of the iodine to the water is controlled at 1:(50-90) and the molar ratio of the hydrazine hydrate to the iodine is controlled at (4.1-4.5):1.0; and adding the iodide ion solution into a copper sulfate solution under the stirring effect, controlling the molar ratio of copper sulfate to iodine at (2.0-2.2):1.0, fully reacting, filtering and drying to obtain gamma-copper iodide. According to the preparation method, the iodine utilization rate is high, a product is less in possibility of being oxidized and decomposed, the production cost is low, and the process is simple.
Description
Technical field
The present invention relates to chemical technology field, relate in particular to a kind of preparation method of γ-cuprous iodide.
Background technology
γ-cuprous iodide (γ-CuI) belongs to zincblende lattce structure, band gap 3.1eV, and stability is not high, oxidizable decomposition.Can be used for the fields such as solar cell, superconducting material, photocatalyst, superelevation counter, food and feed additive, of many uses, added value is high.
At present, the synthetic of γ-cuprous iodide is mainly to adopt liquid-phase precipitation method, and take respectively soluble copper salt (copper sulfate, neutralized verdigris etc.) and solubility salt compounded of iodine (sodium iodide, potassiumiodide etc.) is copper source and propiodal, and water is that solvent carries out chemical precipitation and reacts and make.But the method Shortcomings, is mainly in preparation process, to produce a large amount of free-iodine while being converted into cuprous iodide (initial product cupric iodide is unstable by-product free-iodine), and product separation difficulty causes iodine utilization ratio to reduce, and production cost increases; Adopt organic solvent to carry out free-iodine extraction to product mixed solution and reclaim, operation steps is complicated, and because free-iodine recovering effect is not good, causes the iodine wasting of resources.
Summary of the invention
A kind of iodine utilization ratio of the object of the invention is to overcome above-mentioned shortcoming and providing is high, product is difficult for oxygenolysis, production cost is low, the preparation method of the simple γ-cuprous iodide of technique.
The preparation method of a kind of γ-cuprous iodide of the present invention, comprises the steps:
(1) hydrazine hydrate reduction Iod R: iodine is added to the water, then hydrazine hydrate is added to hybrid reaction in the aqueous solution of iodine, control the mol ratio 1:50-90 of iodine and water, hydrazine hydrate and iodine mol ratio 4.1-4.5:1.0, obtain iodide ion solution;
(2) preparation of γ-cuprous iodide: under stirring action, iodide ion solution is added in copper-bath, control copper sulfate and iodine mol ratio 2.0-2.2:1.0, stirring velocity 200-600rmin
-1, rate of addition 5-15mLmin
-1, fully react 10-20min, filter, dry and obtain γ-cuprous iodide.
The present invention compared with prior art, has obvious beneficial effect, as can be known from the above technical solutions: the present invention is usingd the iodine of lower price and substituted solubility salt compounded of iodine as propiodal, has reduced raw materials cost; In reaction process, the free-iodine of by-product is reduced to iodide ion, reacts completely, and has avoided the generation of elemental iodine, and product is easily separated, has improved γ-cuprous iodide output; Reductive agent hydrazine hydrate can prevent the oxygenolysis of γ-cuprous iodide product, has improved quality product; Whole reaction process produces nitrogen, environmentally safe, and reaction conditions is easy to control, and simple machine can be realized serialization and produce.
Below by embodiment, the invention will be further described.
Embodiment
embodiment 1
A preparation method for γ-cuprous iodide, comprises the steps:
(1) hydrazine hydrate reduction Iod R: the iodine that is 99% by 25.64g mass concentration adds in 90g water, the hydrazine hydrate that is then 80% by 25.66g mass concentration adds hybrid reaction in the aqueous solution of iodine, obtains iodide ion solution;
(2) preparation of γ-cuprous iodide: at 200rmin
-1under stirring action, by iodide ion solution with 5mLmin
-1it is in 99% copper-bath that flow velocity adds 50.44g mass concentration, fully reacts 10min, filters, and dries and obtains γ-cuprous iodide.
embodiment 2
A preparation method for γ-cuprous iodide, comprises the steps:
(1) hydrazine hydrate reduction Iod R: the iodine that is 99% by 25.64g mass concentration adds in 126g water, the hydrazine hydrate that is then 80% by 26.91g mass concentration adds hybrid reaction in the aqueous solution of iodine, obtains iodide ion solution;
(2) preparation of γ-cuprous iodide: at 400rmin
-1under stirring action, by iodide ion solution with 10mLmin
-1it is in 99% copper-bath that flow velocity adds 52.96g mass concentration, fully reacts 15 min, filters, and dries and obtains γ-cuprous iodide.
embodiment 3
A preparation method for γ-cuprous iodide, comprises the steps:
(1) hydrazine hydrate reduction Iod R: the iodine that is 99% by 25.64g mass concentration adds in 162g water, the hydrazine hydrate that is then 80% by 28.16g mass concentration adds hybrid reaction in the aqueous solution of iodine, obtains iodide ion solution;
(2) preparation of γ-cuprous iodide: at 600rmin
-1under stirring action, by iodide ion solution with 15mLmin
-1it is in 99% copper-bath that flow velocity adds 50.44g mass concentration, fully reacts 20 min, filters, and dries and obtains γ-cuprous iodide.
The above, it is only preferred embodiment of the present invention, not the present invention is done to any pro forma restriction, any technical solution of the present invention content that do not depart from, according to technical spirit of the present invention, to any simple modification made for any of the above embodiments, equivalent variations and modification, all still belong in the scope of technical solution of the present invention.
Claims (2)
1. a preparation method for γ-cuprous iodide, comprises the steps:
(1) hydrazine hydrate reduction Iod R: iodine is added to the water, then hydrazine hydrate is added to hybrid reaction in the aqueous solution of iodine, control the mol ratio 1:50-90 of iodine and water, hydrazine hydrate and iodine mol ratio 4.1-4.5:1.0, obtain iodide ion solution;
(2) preparation of γ-cuprous iodide: under stirring action, iodide ion solution is added in copper-bath, control copper sulfate with iodine mol ratio 2.0-2.2:1.0, fully react, filtration, oven dry obtains γ-cuprous iodide.
2. the preparation method of a kind of γ-cuprous iodide as claimed in claim 1, wherein: stirring velocity 200-600rmin in (2) step
-1, rate of addition 5-15mLmin
-1, fully react 10-20min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410402480.4A CN104163449A (en) | 2014-08-16 | 2014-08-16 | Preparation method of gamma-copper iodide |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410402480.4A CN104163449A (en) | 2014-08-16 | 2014-08-16 | Preparation method of gamma-copper iodide |
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| CN104163449A true CN104163449A (en) | 2014-11-26 |
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| CN201410402480.4A Pending CN104163449A (en) | 2014-08-16 | 2014-08-16 | Preparation method of gamma-copper iodide |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105825990A (en) * | 2016-03-30 | 2016-08-03 | 淮北师范大学 | Preparation method of CuI-Fe3O4 magnetic nano-composite |
| CN105858711A (en) * | 2016-03-30 | 2016-08-17 | 淮北师范大学 | Preparation method of CuI-graphene oxide nanocomposite |
| CN105883895A (en) * | 2016-05-25 | 2016-08-24 | 浙江汇能生物股份有限公司 | Preparation method of copper iodide |
| CN107200345A (en) * | 2017-03-20 | 2017-09-26 | 宁波大学 | A kind of preparation method of γ cuprous iodides |
| CN107583656A (en) * | 2017-09-14 | 2018-01-16 | 华中科技大学 | A kind of self-supporting Cu/CuI catalysis materials and preparation method thereof |
| CN108455654A (en) * | 2018-04-18 | 2018-08-28 | 贵州大学 | A kind of preparation method of the nanometer γ-CuI based on microfabricated chemical reactor technology |
| CN108557867A (en) * | 2018-04-18 | 2018-09-21 | 贵州大学 | A kind of preparation method of nanometer of γ-CuI |
| CN108609644A (en) * | 2018-03-21 | 2018-10-02 | 陈亚 | A kind of recovery method of copper ion |
| CN108675484A (en) * | 2018-03-21 | 2018-10-19 | 陈亚 | A kind of recovery method of copper ion |
| CN112429753A (en) * | 2020-12-31 | 2021-03-02 | 江西赣锋锂业股份有限公司 | Method for preparing high-purity cesium iodide from cesium carbonate |
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| CN1609285A (en) * | 2004-09-21 | 2005-04-27 | 同济大学 | New CuI Crystal and growing method thereof |
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2014
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Patent Citations (1)
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| CN1609285A (en) * | 2004-09-21 | 2005-04-27 | 同济大学 | New CuI Crystal and growing method thereof |
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| 刘飞等: "利用液相沉淀法制备纳米球形碘化亚铜晶体", 《大连工业大学学报》 * |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105825990A (en) * | 2016-03-30 | 2016-08-03 | 淮北师范大学 | Preparation method of CuI-Fe3O4 magnetic nano-composite |
| CN105858711A (en) * | 2016-03-30 | 2016-08-17 | 淮北师范大学 | Preparation method of CuI-graphene oxide nanocomposite |
| CN105858711B (en) * | 2016-03-30 | 2018-03-13 | 淮北师范大学 | A kind of preparation method of CuI stannic oxide/graphene nano composites |
| CN105883895A (en) * | 2016-05-25 | 2016-08-24 | 浙江汇能生物股份有限公司 | Preparation method of copper iodide |
| CN107200345A (en) * | 2017-03-20 | 2017-09-26 | 宁波大学 | A kind of preparation method of γ cuprous iodides |
| CN107200345B (en) * | 2017-03-20 | 2019-05-03 | 宁波大学 | A kind of preparation method of γ-cuprous iodide |
| CN107583656A (en) * | 2017-09-14 | 2018-01-16 | 华中科技大学 | A kind of self-supporting Cu/CuI catalysis materials and preparation method thereof |
| CN108675484A (en) * | 2018-03-21 | 2018-10-19 | 陈亚 | A kind of recovery method of copper ion |
| CN108609644A (en) * | 2018-03-21 | 2018-10-02 | 陈亚 | A kind of recovery method of copper ion |
| CN108609644B (en) * | 2018-03-21 | 2020-09-11 | 陈亚 | Copper ion recovery method |
| CN108675484B (en) * | 2018-03-21 | 2021-02-05 | 陈亚 | Copper ion recovery method |
| CN108557867A (en) * | 2018-04-18 | 2018-09-21 | 贵州大学 | A kind of preparation method of nanometer of γ-CuI |
| CN108455654A (en) * | 2018-04-18 | 2018-08-28 | 贵州大学 | A kind of preparation method of the nanometer γ-CuI based on microfabricated chemical reactor technology |
| CN112429753A (en) * | 2020-12-31 | 2021-03-02 | 江西赣锋锂业股份有限公司 | Method for preparing high-purity cesium iodide from cesium carbonate |
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Application publication date: 20141126 |