CN103482676A - Green preparation method of cuprous chloride - Google Patents
Green preparation method of cuprous chloride Download PDFInfo
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- CN103482676A CN103482676A CN201310450680.2A CN201310450680A CN103482676A CN 103482676 A CN103482676 A CN 103482676A CN 201310450680 A CN201310450680 A CN 201310450680A CN 103482676 A CN103482676 A CN 103482676A
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- cuprous chloride
- water
- chloride
- hydrazine hydrate
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Abstract
The invention discloses a green preparation method of cuprous chloride. According to points of the technical scheme, the green preparation method of the cuprous chloride is characterized by comprising the steps as follows: (1), copper chloride is dissolved in water, wherein the copper chloride is CuCl2*2H2O, and the dosage ratio of the water to the copper chloride is 0.5-10L of water for the copper chloride per mole; (2), hydrazine hydrate is added dropwise with stirring at the temperature of 5-40 DEG C, wherein the mole ratio of the hydrazine hydrate to the copper chloride is (0.3-1):1; and (3), after addition, the mixture is stirred continuously at the temperature of 5-40 DEG C for 5-20min and filtered, and solids filtered out are subjected to water washing, alcohol washing and vacuum drying to obtain the white cuprous chloride. According to the green preparation method, the reaction system is simple, raw materials are cheap and easy to obtain, harmful waste can be avoided, the green preparation method accords with the green production concept, the process route is simple, reaction conditions are mild, the reaction time is short, and the green preparation method is convenient to operate, high in efficiency and suitable for mass production.
Description
Technical field
The present invention relates to chemosynthesis technical field, be specifically related to a kind of environment-friendly preparation method thereof of cuprous chloride.
Background technology
Cuprous chloride is white cube crystallization or white powder, is placed in air and easily is oxidized to green high price mantoquita, sees that light decomposes overstrike.Cuprous chloride is important catalyzer in the organic synthesis field, can produce multiple organic chemistry product under its katalysis, as vinylacetylene, vinyl cyanide etc.Petrochemical industry is commonly used cuprous chloride as discoloring agent, sweetening agent and release agent in producing.In dyestuffs industries, cuprous chloride can be used in phthalocyanine blue, activity is emerald green, phthalein is dark green and the aniline dyes production technique in, as the absorption agent of oxygen and carbon monoxide.Cuprous chloride also can be as the additive in sterilant and sanitas.In addition, in the industries such as plating, metallurgy, battery, rubber and medicine, cuprous chloride also has application very widely.
The industrial production cuprous chloride mainly contains following several method at present:
1. copper scrap air oxidation process: the copper wire (copper sheet, copper powder) of take is raw material with hydrochloric acid, sodium-chlor, at a certain temperature, passes into air and is reacted, and makes Na (CuCl
2) solution generates cuprous chloride through hydrolysis again.
2. copper scrap salt acid system: take cupric oxide, copper powder, hydrochloric acid and sodium-chlor as raw material, reacting by heating makes Na (CuCl
2) solution generates cuprous chloride through hydrolysis again.
3. copper scrap chlorine direct oxidation method: copper scrap is dipped in water, passes into chlorine, control certain temperature, first elemental copper is oxidized to Cu
2+, Cu
2+with excessive elemental copper generation chemical reaction, and then make cuprous chloride.Present method adopts industrial chlorine, therefore high to the requirement for anticorrosion of equipment material.
4. cupric salt reduction method: a kind of is that to take copper powder, copper scale be reductive agent, first makes Na (CuCl under the hydrochloric acid condition
2), then hydrolysis generates cuprous chloride.Another kind is with Na
2sO
3or SO
2for reductive agent, directly prepare cuprous chloride in hydrochloric acid medium.
All there are some problems in aforesaid method: 1. the sodium-chlor raw material is disposable use basically, causes the significant wastage of raw material, and production cost is high; 2. need heating, produce big energy-consuming; 3. big for environment pollution, do not meet the green production theory.
Summary of the invention
The technical problem that the present invention solves has been to provide a kind of method that adopts the hydrazine hydrate reduction cupric chloride to prepare cuprous chloride.
Technical scheme of the present invention is: a kind of environment-friendly preparation method thereof of cuprous chloride is characterized in that comprising the following steps: (1), cupric chloride is dissolved in the water, wherein cupric chloride is CuCl
22H
2o, the amount ratio of water and cupric chloride is every mole of cupric chloride water 0.5-10L; (2), under the condition of the temperature of 5-40 ℃ and stirring, drip hydrazine hydrate, wherein the mol ratio of hydrazine hydrate and cupric chloride is 0.3-1:1; (3), be added dropwise to complete after, continue stirring reaction 5-20min at the temperature of 5-40 ℃, filter, the solid leached makes white cuprous chloride through washing, alcohol wash, vacuum-drying.
The environment-friendly preparation method thereof of cuprous chloride of the present invention, in described step (2), stirring velocity is controlled at 250-2000r/min, and the time that drips hydrazine hydrate is 10-20min.
The environment-friendly preparation method thereof of cuprous chloride of the present invention, in described step (3), the vacuum-drying temperature is 30-70 ℃.
Principle of the present invention is: bivalent cupric ion, under the effect of a certain amount of reductive agent hydrazine hydrate, first generates univalent copper ion; Univalent copper ion is combined with chlorion and is generated cuprous chloride.Thereby cuprous chloride is separated out because solubleness in water is less, so just impel reaction constantly to carry out to positive dirction, finally obtain cuprous chloride.Reaction equation is as follows:
The invention has the beneficial effects as follows:
1, reaction system is simple, does not add any tensio-active agent, only uses CuCl
22H
2o(copper source), water (solvent) and hydrazine hydrate (reductive agent), and they all belong to general chemistry reagent, cheap and easy to get;
2, the present invention produces without bazardous waste, meets the green production theory;
3, operational path of the present invention is simple, easy and simple to handle, the reaction conditions gentleness, and the reaction times is short, and efficiency is high, is applicable to scale operation.
The accompanying drawing explanation
fig. 1 is the XRD figure of the cuprous chloride of the embodiment of the present invention 2 preparations, and Fig. 2 is the SEM figure of the cuprous chloride of the embodiment of the present invention 2 preparations.
Embodiment
The embodiment of form, be described in further details foregoing of the present invention by the following examples, but this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following embodiment.All technology realized based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
By 0.01molCuCl
22H
2o is dissolved in 5ml water, under the stirring velocity of 5 ℃ and 250-500r/min, drips the 0.003mol hydrazine hydrate, and time for adding is controlled at 10-15min; After adding, continue to stir 5min, filter, the solid leached is through washing, alcohol wash, and 30 ℃ of vacuum-dryings, obtain white cuprous chloride.
By 0.01molCuCl
22H
2o is dissolved in 10ml water, under the stirring velocity of 10 ℃ and 500-1000r/min, drips the 0.005mol hydrazine hydrate, and time for adding is controlled at 10-15min; After adding, continue to stir 5min, filter, the solid leached is through washing, alcohol wash, and 30 ℃ of vacuum-dryings, obtain white cuprous chloride.Fig. 1 has shown the XRD figure spectrum of the cuprous chloride of preparation, by with standard diagram, comparing the product that can find out preparation, is cuprous chloride, and Fig. 2 has shown the SEM collection of illustrative plates of the cuprous chloride of preparation, can find out the ball-like structure of cuprous chloride by accompanying drawing.
Embodiment 3
By 0.01molCuCl
22H
2o is dissolved in 20ml water, under the stirring velocity of 20 ℃ and 500-1000r/min, drips the 0.005mol hydrazine hydrate, and time for adding is controlled at 10-15min; After adding, continue to stir 10min, filter, the solid leached is through washing, alcohol wash, and 30 ℃ of vacuum-dryings, obtain white cuprous chloride.
Embodiment 4
By 0.01molCuCl
22H
2o is dissolved in 40ml water, under the stirring velocity of 20 ℃ and 500-1000r/min, drips the 0.005mol hydrazine hydrate, and time for adding is controlled at 15-20min; After adding, continue to stir 10min, filter, the solid leached is through washing, alcohol wash, and 50 ℃ of vacuum-dryings, obtain white cuprous chloride.
Embodiment 5
By 0.01molCuCl
22H
2o is dissolved in 60ml water, under the stirring velocity of 30 ℃ and 1000-1500r/min, drips the 0.006mol hydrazine hydrate, and time for adding is controlled at 10-15min; After adding, continue to stir 20min, filter, the solid leached is through washing, alcohol wash, and 60 ℃ of vacuum-dryings, obtain white cuprous chloride.
Embodiment 6
By 0.01molCuCl
22H
2o is dissolved in 60ml water, under the stirring velocity of 30 ℃ and 1000-1500r/min, drips the 0.007mol hydrazine hydrate, and time for adding is controlled at 15-20min; After adding, continue to stir 20min, filter, the solid leached is through washing, alcohol wash, and 70 ℃ of vacuum-dryings, obtain white cuprous chloride.
Embodiment 7
By 0.01molCuCl
22H
2o is dissolved in 70ml water, under the stirring velocity of 40 ℃ and 1500-2000r/min, drips the 0.008mol hydrazine hydrate, and time for adding is controlled at 15-20min; After adding, continue to stir 20min, filter, the solid leached is through washing, alcohol wash, and 70 ℃ of vacuum-dryings, obtain white cuprous chloride.
Embodiment 8
By 0.01molCuCl
22H
2o is dissolved in 100ml water, under the stirring velocity of 30 ℃ and 1500-2000r/min, drips the 0.009mol hydrazine hydrate, and time for adding is controlled at 15-20min; After adding, continue to stir 20min, filter, the solid leached is through washing, alcohol wash, and 60 ℃ of vacuum-dryings, obtain white cuprous chloride.
Embodiment 9
By 0.01molCuCl
22H
2o is dissolved in 60ml water, under the stirring velocity of 25 ℃ and 1500-2000r/min, drips the 0.01mol hydrazine hydrate, and time for adding is controlled at 15-20min; After adding, continue to stir 20min, filter, the solid leached is through washing, alcohol wash, and 70 ℃ of vacuum-dryings, obtain white cuprous chloride.
Embodiment 10
By 0.01molCuCl
22H
2o is dissolved in 50ml water, under the stirring velocity of 25 ℃ and 1500-2000r/min, drips the 0.01mol hydrazine hydrate, and time for adding is controlled at 15-20min; After adding, continue to stir 5min, filter, the solid leached is through washing, alcohol wash, and 50 ℃ of vacuum-dryings, obtain white cuprous chloride.
Embodiment 11
By 0.01molCuCl
22H
2o is dissolved in 20ml water, under the stirring velocity of 25 ℃ and 1500-2000r/min, drips the 0.005mol hydrazine hydrate, and time for adding is controlled at 15-20min; After adding, continue to stir 20min, filter, the solid leached is through washing, alcohol wash, and 50 ℃ of vacuum-dryings, obtain white cuprous chloride.
Embodiment 12
By 0.01molCuCl
22H
2o is dissolved in 30ml water, under the stirring velocity of 25 ℃ and 1000-1500r/min, drips the 0.005mol hydrazine hydrate, and time for adding is controlled at 15-20min; After adding, continue to stir 20min, filter, the solid leached is through washing, alcohol wash, and 50 ℃ of vacuum-dryings, obtain white cuprous chloride.
Embodiment 13
By 0.01molCuCl
22H
2o is dissolved in 40ml water, under the stirring velocity of 25 ℃ and 1500-2000r/min, drips the 0.005mol hydrazine hydrate, and time for adding is controlled at 10-15min; After adding, continue to stir 20min, filter, the solid leached is through washing, alcohol wash, and 60 ℃ of vacuum-dryings, obtain white cuprous chloride.
Embodiment 14
By 0.01molCuCl
22H
2o is dissolved in 80ml water, under the stirring velocity of 25 ℃ and 1000-1500r/min, drips the 0.005mol hydrazine hydrate, and time for adding is controlled at 10-15min; After adding, continue to stir 20min, filter, the solid leached is through washing, alcohol wash, and 50 ℃ of vacuum-dryings, obtain white cuprous chloride.
Embodiment 15
By 0.01molCuCl
22H
2o is dissolved in 90ml water, under the stirring velocity of 25 ℃ and 1000-1500r/min, drips the 0.005mol hydrazine hydrate, and time for adding is controlled at 10-15min; After adding, continue to stir 20min, filter, the solid leached is through washing, alcohol wash, and 60 ℃ of vacuum-dryings, obtain white cuprous chloride.
Embodiment 16
By 0.01molCuCl
22H
2o is dissolved in 100ml water, under the stirring velocity of 25 ℃ and 1000-1500r/min, drips the 0.006mol hydrazine hydrate, and time for adding is controlled at 15-20min; After adding, continue to stir 20min, filter, the solid leached is through washing, alcohol wash, and 70 ℃ of vacuum-dryings, obtain white cuprous chloride.
Above embodiment has described ultimate principle of the present invention, principal character and advantage.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; under the scope that does not break away from the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the scope of protection of the invention.
Claims (4)
1. the environment-friendly preparation method thereof of a cuprous chloride is characterized in that comprising the following steps: (1), cupric chloride is dissolved in the water, wherein cupric chloride is CuCl
22H
2o, the amount ratio of water and cupric chloride is every mole of cupric chloride water 0.5-10L; (2), under the condition of the temperature of 5-40 ℃ and stirring, drip hydrazine hydrate, wherein the mol ratio of hydrazine hydrate and cupric chloride is 0.3-1:1; (3), be added dropwise to complete after, continue stirring reaction 5-20min at the temperature of 5-40 ℃, filter, the solid leached makes white cuprous chloride through washing, alcohol wash, vacuum-drying.
2. the environment-friendly preparation method thereof of cuprous chloride according to claim 1 is characterized in that: in described step (2), stirring velocity is controlled at 250-2000r/min, and the time that drips hydrazine hydrate is 10-20min.
3. the environment-friendly preparation method thereof of cuprous chloride according to claim 1 is characterized in that: in described step (3), the vacuum-drying temperature is 30-70 ℃.
4. the environment-friendly preparation method thereof of cuprous chloride according to claim 1 is characterized in that the principal reaction equation in preparation process is as follows:
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|---|---|---|---|
| CN201310450680.2A CN103482676A (en) | 2013-09-29 | 2013-09-29 | Green preparation method of cuprous chloride |
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|---|---|---|---|
| CN201310450680.2A CN103482676A (en) | 2013-09-29 | 2013-09-29 | Green preparation method of cuprous chloride |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105819489A (en) * | 2016-03-13 | 2016-08-03 | 河南师范大学 | Green synthesis method of cuprous chloride |
| CN107740088A (en) * | 2017-09-24 | 2018-02-27 | 盐城师范学院 | A kind of interface quick controllable method for preparing of stannous chloride micro crystal material |
| CN112062148A (en) * | 2020-09-09 | 2020-12-11 | 东华大学 | Method for preparing cuprous chloride by using copper-containing sludge in electroplating circuit board wastewater |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4582579A (en) * | 1984-12-24 | 1986-04-15 | Hughes Aircraft Company | Method for preparing cupric ion-free cuprous chloride |
| CN1191215A (en) * | 1998-03-20 | 1998-08-26 | 湖北省化学研究所 | Method for fast increasing copper ratio of copper ammonium acetate liquid |
| CN101070181A (en) * | 2006-05-17 | 2007-11-14 | 盐城师范学院 | Water heating reduction method preparing process for cuprous chloride |
| KR20080018302A (en) * | 2006-08-24 | 2008-02-28 | 서안켐텍 주식회사 | Process for preparing cuprous chloride with high quality from cupric chloride containing waste |
| CN101844794A (en) * | 2009-03-27 | 2010-09-29 | 中国科学院安徽光学精密机械研究所 | Method for preparing and purifying cuprous halide |
-
2013
- 2013-09-29 CN CN201310450680.2A patent/CN103482676A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4582579A (en) * | 1984-12-24 | 1986-04-15 | Hughes Aircraft Company | Method for preparing cupric ion-free cuprous chloride |
| CN1191215A (en) * | 1998-03-20 | 1998-08-26 | 湖北省化学研究所 | Method for fast increasing copper ratio of copper ammonium acetate liquid |
| CN101070181A (en) * | 2006-05-17 | 2007-11-14 | 盐城师范学院 | Water heating reduction method preparing process for cuprous chloride |
| KR20080018302A (en) * | 2006-08-24 | 2008-02-28 | 서안켐텍 주식회사 | Process for preparing cuprous chloride with high quality from cupric chloride containing waste |
| CN101844794A (en) * | 2009-03-27 | 2010-09-29 | 中国科学院安徽光学精密机械研究所 | Method for preparing and purifying cuprous halide |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105819489A (en) * | 2016-03-13 | 2016-08-03 | 河南师范大学 | Green synthesis method of cuprous chloride |
| CN107740088A (en) * | 2017-09-24 | 2018-02-27 | 盐城师范学院 | A kind of interface quick controllable method for preparing of stannous chloride micro crystal material |
| CN112062148A (en) * | 2020-09-09 | 2020-12-11 | 东华大学 | Method for preparing cuprous chloride by using copper-containing sludge in electroplating circuit board wastewater |
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Application publication date: 20140101 |