CN105293559A - High-purity basic cupric carbonate microsphere and preparation method - Google Patents
High-purity basic cupric carbonate microsphere and preparation method Download PDFInfo
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- CN105293559A CN105293559A CN201510817117.3A CN201510817117A CN105293559A CN 105293559 A CN105293559 A CN 105293559A CN 201510817117 A CN201510817117 A CN 201510817117A CN 105293559 A CN105293559 A CN 105293559A
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Abstract
The present invention discloses a high-purity basic cupric carbonate microsphere and a preparation method. The method uses the direct precipitation method, and the preparation process comprises the steps of: (1) copper chloride and sodium carbonate powder are respectively prepared into solutions with certain concentrations; (2) the copper chloride solution and the sodium carbonate solution are added dropwise into a container containing a quantity of water; the raw material liquid dropping speed is controlled, the mixed solution pH is kept at 6.5-7.0, the temperature is kept at 45-50 DEG C; and (3) viridis basic cupric carbonate powder is obtained by thermal insulation standing, filtering, washing and drying. The basic cupric carbonate microsphere prepared by the method has regular morphology, particle size distribution is in 5-7mum, purity is high, copper content is 56.0%-56.5%, iron content is less than 5ppm, lead content is less than 3ppm, Zn content is less than 10ppm, and sodium content is less than 50ppm. The basic cupric carbonate microsphere has the advantages of easily obtained raw materials, low cost, simple operation, mild reaction conditions, no adding of additives, and environmental friendliness.
Description
Technical field
The present invention relates to chemical production technical field, particularly relate to a kind of high-purity alkali type copper carbonate microballoon and preparation method thereof.
Background technology
Ventilation breather [Cu
2(OH)
2cO
3], also known as malachite, green in peacock, be the important presoma of obtained cupric oxide, and the aspect such as cupric oxide is as P-type semiconductor material, has narrow energy gap, is widely used in isomerized catalysis, gas sensor, lithium cell; In addition ventilation breather self also has a wide range of applications, and not only as the catalyzer of organic synthesis, but also can be used as coating, pigment etc.
At present, the preparation method of ventilation breather has a lot, classify from raw material, there are copper sulfate method, cupric nitrate method and ammonia process, wherein applying maximum is copper sulfate method, but the ventilation breather of these methods not easily obtained regular appearance, and when being raw material with copper sulfate, often be mingled with Basic Chrome Sulphate in product, reduce the purity of product.Therefore, utilize simple method, suitable raw material, prepare regular appearance, basic copper carbonate microspheres that purity is high is significant.
Summary of the invention
In order to overcome the deficiencies in the prior art, the object of the present invention is to provide a kind of high-purity alkali type copper carbonate microballoon and preparation method thereof.The present invention, by adopting simple technological line, prepares the basic copper carbonate microspheres that purity height pattern is good.
The inventive method is with CuCl
2for copper source, Na
2cO
3for alkali source, prepare ventilation breather by direct precipitation method, the ventilation breather purity obtained is high, and crystal formation is good, and pattern is homogeneous.
The present invention realizes by following technical solution.
The invention provides a kind of high-purity alkali type copper carbonate microballoon, its even particle size distribution is at 5-7 μm, and copper content is at 56%-56.5%, and iron level is less than 5ppm, and lead content is less than 3ppm, and Zn content is less than 10ppm, and sodium content is less than 50ppm.
The present invention also provides a kind of preparation method of high-purity alkali type copper carbonate microballoon, and it adopts direct precipitation method to be prepared, and concrete steps are as follows:
(1) by CuCl
2with Na
2cO
3be dissolved in respectively in deionized water, obtained CuCl
2with Na
2cO
3solution;
(2) by above-mentioned CuCl
2solution and Na
2cO
3solution is added drop-wise to simultaneously and is equipped with in the container of water, controls drop rate, maintains reaction solution pH within the scope of 6.5-7.0, and the temperature simultaneously in control container is between 45-50 DEG C;
(3) after stock liquid dropwises, be incubated still aging at 45-50 DEG C of temperature;
(4) reaction terminates, and filters, and washing, after drying, obtains emerald green Cu
2(OH)
2cO
3powder.
In the present invention, in step (1), CuCl
2solution and Na
2cO
3strength of solution is identical.
In the present invention, in step (1), CuCl
2solution and Na
2cO
3the volumetric molar concentration of solution is 0.5-1.0mol/L.
In the present invention, in step (3), still aging 2-4h.
In the present invention, in step (4), drying temperature 80-90 DEG C, the time is 5h-6h.
Control pH in reaction solution in the present invention between 6.5-7.0, the product of acquisition can be made to have better degree of crystallinity.When pH is less than 6.5, CO
3 2-with H
+in conjunction with, and then generate CO
2effusion, product can adulterate basic copper chloride, purity drop; And when pH is greater than 7.0, nucleating surface HO
-amount increases, and changes nucleating surface nucleo plasmic relation, and the degree of crystallinity of product reduces, and can not get yardstick uniform microsphere, does not even form microballoon.
The present invention controls material concentration in certain interval, during excessive concentration, product can be caused acutely to reunite, and can not get the microballoon of rule; When concentration is lower, in the temperature range controlled, the product obtained is impure, has portion of product and is decomposed into CuO, even can not get target product.
Beneficial effect of the present invention is as follows:
(1) cheaper starting materials required for preparation method, cost is low;
(2) technique is simple, and reaction conditions is gentle, favorable repeatability;
(3) obtained product is regular microballoon, and pattern is homogeneous, and purity is high, with Cu
2(OH)
2cO
3meter, the purity of product of the present invention is between 97.5%-98.5%;
(4) do not need to add additive, technique environmental protection, without toxic pharmaceuticals and by product, avoid the pollution to environment.
Accompanying drawing explanation
Fig. 1 is the SEM figure of product high-purity alkali type copper carbonate microballoon.
Fig. 2 is the XRD figure of product high-purity alkali type copper carbonate microballoon.
Embodiment
Embodiment 1
(1) 25.65gCuCl is taken
22H
2o and 19.08gNa
2cO
3, be then dissolved in respectively in 300mL and 360mL deionized water, be mixed with the CuCl that volumetric molar concentration is 0.5mol/L
2with Na
2cO
3solution;
(2) by above-mentioned CuCl
2solution and Na
2cO
3solution is added drop-wise in the three-necked flask containing 300mL deionized water under stirring simultaneously, and the temperature in control three-necked flask is at 50 DEG C, and control the drop rate of two kinds of solution, to regulate the PH of reaction soln at 6.5-7.0, time for adding is at about 10min simultaneously;
(3) after stock liquid dropwises, stop stirring, allow mixed serum slowly sedimentation, keep reacting liquid temperature constant, still aging 3h;
(4), after ageing terminates, mixed solution is filtered, after deionized water wash 5 times, then uses absolute ethanol washing 3 times, then in baking oven, after 90 DEG C of dry 5h, obtain emerald green Cu
2(OH)
2cO
3powder.Take the pressed powder obtained on a small quantity, adding dilute hydrochloric acid solution makes it all dissolve, add deionized water again and carry out dilution constant volume, adopting Atomic Absorption Spectroscopy AAS (AAS) to detect copper content is 56.15%, iron level is 0.87ppm, lead content is 0.50ppm, and Zn content is 2.42ppm, and sodium content is 22.12ppm.
Fig. 1 is the SEM figure of the product high-purity alkali type copper carbonate microballoon of embodiment 1.As seen from the figure, the product obtained is the microspheroidal of rule, and even particle size distribution is at 5-7 μm.Fig. 2 is the XRD figure of the product high-purity alkali type copper carbonate microballoon of embodiment 1.Extremely mate with (JCPDSNo.76-0660) in powdery diffractometry standard diagram, peak shape degree of fitting is high, and this shows that the product obtained is ventilation breather powder, be monocline crystalline phase, and purity is high, impure peak hardly, from peak shape more sharply, the better crystallinity degree of powder.
Embodiment 2
(1) 51.20gCuCl is taken
22H
2o and 38.16gNa
2cO
3, be then dissolved in respectively in 300mL and 360mL deionized water, be mixed with the CuCl that volumetric molar concentration is 1.0mol/L
2with Na
2cO
3solution;
(2) by above-mentioned CuCl
2solution and Na
2cO
3solution is added drop-wise in the three-necked flask containing 300mL deionized water under stirring simultaneously, and the temperature in control three-necked flask is at 45 DEG C, and control the drop rate of two kinds of solution, to regulate the PH of reaction soln at 6.5-7.0, time for adding is at about 12min simultaneously;
(3) after stock liquid dropwises, stop stirring, allow mixed serum slowly sedimentation, keep reacting liquid temperature constant, still aging 2.5h;
(4), after ageing terminates, mixed solution is filtered, after deionized water wash 5 times, then uses absolute ethanol washing 3 times, then in baking oven, after 90 DEG C of dry 3h, obtain emerald green Cu
2(OH)
2cO
3powder.Take the pressed powder obtained on a small quantity, adding dilute hydrochloric acid solution makes it all dissolve, add deionized water again and carry out dilution constant volume, adopting Atomic Absorption Spectroscopy AAS (AAS) to detect copper content is 56.32%, iron level is 1.02ppm, lead content is 0.54ppm, and Zn content is 3.43ppm, and sodium content is 25.87ppm.
Claims (6)
1. a high-purity alkali type copper carbonate microballoon, is characterized in that, its even particle size distribution is at 5-7 μm, and copper content is at 56.0%-56.5%, and iron level is less than 5ppm, and lead content is less than 3ppm, and Zn content is less than 10ppm, and sodium content is less than 50ppm.
2. a preparation method for high-purity alkali type copper carbonate microballoon, is characterized in that, it adopts direct precipitation method to be prepared, and concrete steps are as follows:
(1) by CuCl
2with Na
2cO
3be dissolved in respectively in deionized water, obtained CuCl
2with Na
2cO
3solution;
(2) by above-mentioned CuCl
2solution and Na
2cO
3solution is added drop-wise to simultaneously and is equipped with in the container of water, controls drop rate, maintains reaction solution pH within the scope of 6.5-7.0, and the temperature simultaneously in control container is between 45-50 DEG C;
(3) after stock liquid dropwises, be incubated still aging at 45-50 DEG C of temperature;
(4) reaction terminates, and filters, and washing, after drying, obtains emerald green Cu
2(OH)
2cO
3powder.
3. preparation method according to claim 2, is characterized in that: in step (1), CuCl
2solution and Na
2cO
3strength of solution is identical.
4. preparation method according to claim 3, is characterized in that, CuCl in step (1)
2solution and Na
2cO
3the volumetric molar concentration of solution is 0.5-1.0mol/L.
5. preparation method according to claim 2, is characterized in that: in step (3), still aging 2-4h.
6. preparation method according to claim 2, is characterized in that: in step (4), drying temperature 80-90 DEG C, and the time is 5h-6h.
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|---|---|---|---|
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1883894A (en) * | 2006-06-13 | 2006-12-27 | 上海大不同木业科技有限公司 | Mixture containing nano copper compound and process for preparing same |
| CN102275973A (en) * | 2011-06-01 | 2011-12-14 | 华南师范大学 | Preparation method of basic copper carbonate microspheres |
| CN103232055A (en) * | 2013-04-10 | 2013-08-07 | 廖勇志 | Method of preparing basic copper carbonate |
| CN105060331A (en) * | 2015-08-15 | 2015-11-18 | 淮北师范大学 | Preparation method of regulable basic cupric carbonate micro-nano hierarchical structure |
-
2015
- 2015-11-23 CN CN201510817117.3A patent/CN105293559A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1883894A (en) * | 2006-06-13 | 2006-12-27 | 上海大不同木业科技有限公司 | Mixture containing nano copper compound and process for preparing same |
| CN102275973A (en) * | 2011-06-01 | 2011-12-14 | 华南师范大学 | Preparation method of basic copper carbonate microspheres |
| CN103232055A (en) * | 2013-04-10 | 2013-08-07 | 廖勇志 | Method of preparing basic copper carbonate |
| CN105060331A (en) * | 2015-08-15 | 2015-11-18 | 淮北师范大学 | Preparation method of regulable basic cupric carbonate micro-nano hierarchical structure |
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Application publication date: 20160203 |
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