CN102275973A - Preparation method of basic copper carbonate microspheres - Google Patents
Preparation method of basic copper carbonate microspheres Download PDFInfo
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- CN102275973A CN102275973A CN2011101462023A CN201110146202A CN102275973A CN 102275973 A CN102275973 A CN 102275973A CN 2011101462023 A CN2011101462023 A CN 2011101462023A CN 201110146202 A CN201110146202 A CN 201110146202A CN 102275973 A CN102275973 A CN 102275973A
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- preparation
- microballoon
- ventilation breather
- basic copper
- copper carbonate
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Abstract
The invention discloses a preparation method of basic copper carbonate microspheres, and the preparation method is characterized by comprising the following steps: 1) uniformly mixing a copper nitrate solution with a sodium carbonate solution and standing; and 2) taking the precipitate obtained in step 1) out, centrifuging, washing and drying to obtain the basic copper carbonate microspheres. The basic copper carbonate microspheres prepared by the preparation method disclosed by the invention have the advantages of regular morphology, uniform distribution and high purity; and the preparation method disclosed by the invention has the advantages of simplicity and feasibility, high yield, low cost, mild reaction conditions, no pollution and environmental friendliness.
Description
Technical field
The present invention relates to a kind of preparation method of ventilation breather microballoon.
Background technology
Ventilation breather has another name called malachite, it is a kind of famous and precious mineral jewel, also be a kind of important catalyst simultaneously, industrial chemicals and wood preservation raw material, be mainly used in system paint pigment, pyrotechnics, sterilant, other mantoquitas and solid fluorescence powder activator etc., also be used for seed treatment and make sterilant etc., also as pigment.But as a kind of microballoon, not only require its not only purity height, also require fineness and distribution uniformly from microcosmic angle.
In the prior art, ventilation breather is generally the auxiliary product of taking from other chemical industry, impure rate height, cost height, purity are not high, fineness and homogeneity are not good, therefore, be necessary to develop a kind of preparation high yield, low cost, simple synthetic method with ventilation breather of regular pattern.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of ventilation breather microballoon.
The technical solution used in the present invention is:
A kind of preparation method of ventilation breather microballoon may further comprise the steps:
1) copper nitrate solution and sodium carbonate solution are mixed, leave standstill;
2) take out the precipitation that step 1) obtains, centrifugal, washing, drying promptly obtain the ventilation breather microballoon.
The mol ratio of cupric nitrate and yellow soda ash is 1:1-1.5.
In the copper nitrate solution, the concentration of cupric ion is 0.01-0. 5mol/L.
Insulation dwell temperature in the step 1) is 20-50 ℃.
Insulation time of repose in the step 1) is 12-48h.
The invention has the beneficial effects as follows: the pattern of the ventilation breather microballoon of the present invention preparation is regular, be evenly distributed, and the purity height, preparation method of the present invention is simple, productive rate is higher, cost is low, reaction conditions is gentle, pollution-free, environmentally friendly.
Description of drawings
Fig. 1 is the X-ray diffractogram of the ventilation breather microballoon that makes of the embodiment of the invention 2.
Fig. 2 is the SEM picture of the ventilation breather microballoon that makes of the embodiment of the invention 2.
Fig. 3 is the SEM picture of the ventilation breather microballoon that makes of the embodiment of the invention 2.
Embodiment
Below in conjunction with embodiment the present invention is described:
Embodiment 1:
Under agitation, copper nitrate solution at the uniform velocity is added drop-wise to the precursor solution that is mixed with blueness in isopyknic sodium carbonate solution, the gained flocculent precipitate continues to stir 0.5～1h, and in the precursor aqueous solution that is made into, the volumetric molar concentration of cupric nitrate and yellow soda ash is 0.25mol/L;
Resulting precursor solution is rested on 12h in 20 ℃ of waters bath with thermostatic control, the grass green throw out under collecting;
Centrifugal with distilled water to the grass green throw out of collecting, about 6 times of repetitive scrubbing, air-dry under field conditions (factors) drying, the product that obtains is the ventilation breather microballoon.
Embodiment 2:
Measure 60ml, the 0.15mol/L sodium carbonate solution is added drop-wise to 60ml with constant pressure funnel, and in the copper nitrate solution of 0.15mol/L, reaction under agitation obtains blue cotton-shaped precursor solution;
The precursor solution that obtains rested in 35 ℃ the water bath with thermostatic control behind the insulation 24h, obtain the grass green throw out;
Collect the reaction product of gained, centrifugal with distilled water to the grass green throw out of collecting, repetitive scrubbing 6 times, air-dry under field conditions (factors), obtaining product is the ventilation breather microballoon.
Embodiment 3:
Measure 60ml, the 0.05mol/L sodium carbonate solution is added drop-wise to 90ml with constant pressure funnel, the cupric nitrate of 0.05mol/L, and reaction under agitation obtains blue cotton-shaped precursor solution;
The precursor solution that obtains rested in 45 ℃ the water bath with thermostatic control behind the insulation 12h, obtain the grass green throw out;
Collect the reaction product of gained, centrifugal with distilled water to the grass green throw out of collecting, repetitive scrubbing 6 times, dry in 20-40 ℃ vacuum drying oven, obtaining product is the ventilation breather microballoon.
Embodiment 4:
Measure 60ml, the 0.05mol/L sodium carbonate solution is added drop-wise to 75ml with constant pressure funnel, the cupric nitrate of 0.05mol/L, and reaction under agitation obtains blue cotton-shaped precursor solution;
The precursor solution that obtains rested in 50 ℃ the water bath with thermostatic control behind the insulation 48h, obtain the grass green throw out;
Collect the reaction product of gained, centrifugal with distilled water to the grass green throw out of collecting, repetitive scrubbing 6 times, dry in 20-40 ℃ vacuum drying oven, obtaining product is the ventilation breather microballoon.
Fig. 1 is the X-ray diffractogram of the product that obtains of embodiment 2, three crystal faces (220) of 23.93 °, 31.13 °, the 35.42 ° corresponding ventilation breathers of difference in three obvious diffraction peaks among Fig. 1,
With
, and all peaks of this figure proof all belong to ventilation breather oblique system (JCPDS No.10-0339), and microballoon does not contain any impurity.Fig. 2 is the electron scanning micrograph that embodiment 2 obtains the low power of ventilation breather microballoon, can see that sample contains a large amount of microballoons, and size distribution is even simultaneously; Fig. 3 is the electron scanning micrograph of gained sample, and the surface that can further find out sample is the coarse structure that is similar to strawberry-like.Confirmed jointly that by above analysis the sample that the embodiment of the invention obtains is purified ventilation breather microballoon, and diameter of micro ball is about the 4-5 micron.
Preparation method of the present invention is simple, do not use any additives in the reaction, do not introduce any impurity, the by product of reaction can be used the deionized water flush away, and the reaction conditions gentleness is pollution-free, environmentally friendly, owing to do not need follow-up high-temperature calcination, effectively save the energy simultaneously, reduced the cost of synthetic ventilation breather microballoon.
Claims (5)
1. the preparation method of a ventilation breather microballoon is characterized in that: may further comprise the steps:
1) copper nitrate solution and sodium carbonate solution are mixed, insulation is left standstill;
2) take out the precipitation that step 1) obtains, centrifugal, washing, drying promptly obtain the ventilation breather microballoon.
2. the preparation method of a kind of ventilation breather microballoon according to claim 1 is characterized in that: the mol ratio of cupric nitrate and yellow soda ash is 1:1-1.5.
3. the preparation method of a kind of ventilation breather microballoon according to claim 1 is characterized in that: in the copper nitrate solution, the concentration of cupric ion is 0.01-0. 5mol/L.
4. the preparation method of a kind of ventilation breather microballoon according to claim 1 is characterized in that: the insulation dwell temperature in the step 1) is 20-50 ℃.
5. the preparation method of a kind of ventilation breather microballoon according to claim 1 is characterized in that: the insulation time of repose in the step 1) is 12-48h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2011101462023A CN102275973A (en) | 2011-06-01 | 2011-06-01 | Preparation method of basic copper carbonate microspheres |
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| CN2011101462023A CN102275973A (en) | 2011-06-01 | 2011-06-01 | Preparation method of basic copper carbonate microspheres |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864133A (en) * | 2012-12-11 | 2014-06-18 | 财团法人工业技术研究院 | Preparation method of nano metal salt and formation method of absorption layer of solar cell |
| 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 |
| CN105293559A (en) * | 2015-11-23 | 2016-02-03 | 上海应用技术学院 | High-purity basic cupric carbonate microsphere and preparation method |
| CN108772084A (en) * | 2018-06-07 | 2018-11-09 | 郑州轻工业学院 | TiO with photocatalysis antibacterial performance2/Cu2(OH)2CO3The preparation method and application of composite nano materials |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428841A (en) * | 2007-11-05 | 2009-05-13 | 沈祖达 | Process for producing basic copper carbonate |
| JP2010143809A (en) * | 2008-12-22 | 2010-07-01 | Rasa Ind Ltd | Method for producing basic copper carbonate and basic copper carbonate |
| CN101885506A (en) * | 2010-07-17 | 2010-11-17 | 天津市化学试剂研究所 | Method for preparing analytically pure basic cupric carbonate |
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2011
- 2011-06-01 CN CN2011101462023A patent/CN102275973A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428841A (en) * | 2007-11-05 | 2009-05-13 | 沈祖达 | Process for producing basic copper carbonate |
| JP2010143809A (en) * | 2008-12-22 | 2010-07-01 | Rasa Ind Ltd | Method for producing basic copper carbonate and basic copper carbonate |
| CN101885506A (en) * | 2010-07-17 | 2010-11-17 | 天津市化学试剂研究所 | Method for preparing analytically pure basic cupric carbonate |
Non-Patent Citations (2)
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| 曹小华 等: "碱式碳酸铜的制备工艺研究", 《化工中间体》, no. 12, 31 December 2008 (2008-12-31), pages 43 - 45 * |
| 贺拥军 等: "碱式碳酸铜微球的表面改性和组装", 《物理化学学报(WULI HUAXUE XUEBAO)》, vol. 23, no. 5, 21 April 2007 (2007-04-21), pages 774 - 778 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864133A (en) * | 2012-12-11 | 2014-06-18 | 财团法人工业技术研究院 | Preparation method of nano metal salt and formation method of absorption layer of solar cell |
| 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 |
| CN105293559A (en) * | 2015-11-23 | 2016-02-03 | 上海应用技术学院 | High-purity basic cupric carbonate microsphere and preparation method |
| CN108772084A (en) * | 2018-06-07 | 2018-11-09 | 郑州轻工业学院 | TiO with photocatalysis antibacterial performance2/Cu2(OH)2CO3The preparation method and application of composite nano materials |
| CN108772084B (en) * | 2018-06-07 | 2021-06-18 | 郑州轻工业学院 | TiO with photocatalytic antibacterial property2/Cu2(OH)2CO3Preparation method and application of composite nano material |
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Application publication date: 20111214 |