CN102276437A - Preparation method of flaky acetylacetone copper microcrystal - Google Patents
Preparation method of flaky acetylacetone copper microcrystal Download PDFInfo
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- CN102276437A CN102276437A CN201110177130A CN201110177130A CN102276437A CN 102276437 A CN102276437 A CN 102276437A CN 201110177130 A CN201110177130 A CN 201110177130A CN 201110177130 A CN201110177130 A CN 201110177130A CN 102276437 A CN102276437 A CN 102276437A
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- acetylacetone
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Abstract
The invention belongs to the field of inorganic non-metal materials, in particular relates to a preparation method of a flaky acetylacetone copper microcrystal. The preparation method comprises the following steps: based on a mixed solution of a metal copper substrate, acetylacetone and an oxidation accelerator as a raw material, firstly carrying out ultrasonic washing on a copper sheet; then directly putting the washed copper sheet in the mixed solution containing acetylacetone and reacting for 3-15 days at the temperature of 20-40 DEG C; and after the reaction is finished, washing and drying, so that the flaky acetylacetone copper microcrystal is prepared. The preparation method is characterized in that in the mixed solution of acetylacetone and oxidation accelerator, the oxidation accelerator is one or a mixture of more than two of ammonia water, formamide or urea. According to the invention, the process is simple and practicable, the prepared flaky acetylacetone copper microcrystal has high purify, low impurity content, low preparation cost and flaky topography, and the thickness of a slice ranges from 3mm to 8mm; and the flaky acetylacetone copper microcrystal obtained by the preparation method can be widely applied to the fields of chemical industry, national defense, electronic industry and the like.
Description
Technical field
The invention belongs to the preparing technical field of ceramic, specifically relate to the preparation method of sheet acetylacetone copper crystallite.
Background technology
Acetylacetone copper, molecular formula: Cu (CH
3
COCHCOCH
3
)
2
Molecular weight: 261.76; English name: Copper (II) acetylacetonate; CAS No:13395-16-9.Acetylacetone copper is a kind of important inorganic salt product, is widely used in industries such as chemical industry, national defence, electronic industry.Be commonly used for resin cross-linking agent and curing catalyst; Rubber accelerator; Fuel oil additive can improve oilness and incendivity, but can not stop carbon laydown, as organic catalyst compound.
At present, main production method both domestic and external is as follows: Gerhardite is soluble in water, add strong aqua, and can be made into cuprammonia, under agitation, add methyl ethyl diketone slowly, separate out the blueness precipitation of acetylacetone copper, filter, use cold water washing, seasoning can make crude product; In methyl alcohol-benzene or benzene, carry out recrystallization again, can make highly finished product; Purer as need, can under vacuum, distil.The acetylacetone copper purity that this method is produced is low, foreign matter content is high, and complicated process of preparation can not satisfy the requirement of modern industry to the methyl ethyl diketone copper products.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art part and provides a kind of technology simple, purpose product yield height, and preparation cost is low, and operating procedure is simple, the preparation method of the sheet acetylacetone copper crystallite of good dispersity.
For achieving the above object, the present invention is achieved in that a kind of preparation method of sheet acetylacetone copper crystallite, is after the metallic copper substrate is cleaned, directly put into methyl ethyl diketone and oxidation promotor mixed solution, after reaction finishes, wash, drying, promptly get the purpose product.
As a kind of preferred version, in methyl ethyl diketone of the present invention and the oxidation promotor mixed solution, the mol ratio of methyl ethyl diketone and oxidation promotor is 1: 0.1～10.
As another kind of preferred version, in methyl ethyl diketone of the present invention and the oxidation promotor mixed solution, the volumetric molar concentration of methyl ethyl diketone is 0.1～10 mol/L.
Further, oxidation promotor of the present invention is one or more the mixture in ammoniacal liquor, methane amide or the urea.
In addition, temperature of reaction of the present invention can be selected 20～40 ° of C, and the reaction times can be selected 3～15 days.
Secondly, can select 2～5 hours time of drying of the present invention, and drying temperature can be selected 30～50 ° of C.
The thickness of metallic copper substrate of the present invention can be selected 0.1～0.2 mm.
Compared with prior art, the present invention has following characteristics: (1) operational path of the present invention is simple, and preparation cost is low, and is easy to control, has higher production efficiency.
(2) the purpose product sheet acetylacetone copper crystallite of the present invention's preparation, its purity height (95%～99%), foreign matter content is low, and good dispersity (by SEM figure as can be seen) can satisfy the requirement of modern industry to the methyl ethyl diketone copper products.
Description of drawings
The invention will be further described below in conjunction with the drawings and specific embodiments.Protection scope of the present invention not only is confined to the statement of following content.
Fig. 1 is the X-ray diffractogram of the prepared sheet acetylacetone copper crystallite of the present invention.
Fig. 2 is the SEM shape appearance figure of the prepared sheet acetylacetone copper crystallite of the present invention.
Fig. 3 is the SEM shape appearance figure of the prepared sheet acetylacetone copper crystallite of the present invention.
Fig. 4 is the SEM shape appearance figure of the prepared sheet acetylacetone copper crystallite of the present invention.
Embodiment
The present invention is a raw material with metallic copper substrate (99.9%, thickness 0.12 mm) and the mixed solution that contains methyl ethyl diketone, earlier copper sheet is carried out ultrasonic cleaning, directly puts into then and contains the methyl ethyl diketone mixed solution, under 20～40 ° of C conditions, reacts 3～15 days.After reaction finishes, wash, drying, promptly make flaky acetylacetone copper crystallite, its preparation process is: (1) is with metallic copper substrate (99.9%, thickness 0.12 mm) carried out ultrasonic cleaning 20～30 minutes, clean respectively with deionized water and dehydrated alcohol again, standby after the drying at room temperature.
(2) methyl ethyl diketone and oxidation promotor are mixed with mixed solution according to the mol ratio of 1:0.1～10, the concentration of its methyl ethyl diketone is 0.1～10 mol/L, and it is standby to obtain mixed solution.
(3) copper base after will cleaning is directly put into mixed solution, reacts 3～15 days under 20～40 ° of C conditions.
(4) should finish after, take out product, after the washing, put into baking oven, under 30～50 ° of C conditions, dry 2～5 hours, promptly make flaky acetylacetone copper crystallite.
Fig. 1 is the X-ray diffractogram of the prepared sheet acetylacetone copper crystallite of the present invention, and the peak that wherein adds * is the diffraction peak of copper base.
Shown in Fig. 2～4, the flaky acetylacetone copper crystallite that the present invention will prepare gained carries out scanning electron microscope (SEM) analysis, and consequently, products obtained therefrom acetylacetone copper crystallite has flaky pattern, and the thickness of sheet is between 3～8 mm.
Embodiment 1.
Metallic copper substrate (99.9%, thickness 0.12 mm) is carried out ultrasonic cleaning 20 minutes, clean the back drying at room temperature respectively with deionized water and dehydrated alcohol again.Methyl ethyl diketone and ammoniacal liquor (30%m--mass concentration) are mixed with mixed solution according to the mol ratio of 1:5, and the concentration of its methyl ethyl diketone is 0.5 mol/L.Copper base after cleaning is directly put into mixed solution, and reaction is 7 days under 30 ° of C conditions.After reaction finishes, take out product, after the washing, put into baking oven, under 30 ° of C conditions, dry 2 hours, promptly make flaky acetylacetone copper crystallite.
Metallic copper substrate (99.9%, thickness 0.12 mm) is carried out ultrasonic cleaning 20 minutes, clean the back drying at room temperature respectively with deionized water and dehydrated alcohol again.Methyl ethyl diketone and ammoniacal liquor (30%m) are mixed with mixed solution according to the mol ratio of 1:9, and the concentration of its methyl ethyl diketone is 0.2 mol/L.Copper base after cleaning is directly put into mixed solution, and reaction is 12 days under 25 ° of C conditions.After should finishing, take out product, after the washing, put into baking oven, under 30 ° of C conditions, dry 2 hours, promptly make flaky acetylacetone copper crystallite.
Embodiment 3.
Metallic copper substrate (99.9%, thickness 0.12 mm) is carried out ultrasonic cleaning 25 minutes, clean the back drying at room temperature respectively with deionized water and dehydrated alcohol again.Methyl ethyl diketone and ammoniacal liquor (30%m) are mixed with mixed solution according to the mol ratio of 1:3, and the concentration of its methyl ethyl diketone is 0.4 mol/L.Copper base after cleaning is directly put into mixed solution, and reaction is 15 days under 20 ° of C conditions.After should finishing, take out product, after the washing, put into baking oven, under 30 ° of C conditions, dry 2 hours, promptly make flaky acetylacetone copper crystallite.
Embodiment 4.
Metallic copper substrate (99.9%, thickness 0.12 mm) is carried out ultrasonic cleaning 20 minutes, clean the back drying at room temperature respectively with deionized water and dehydrated alcohol again.With ammoniacal liquor (30%m) and the mixed oxidation promotor that is mixed with of methane amide (mol ratio of ammoniacal liquor and methane amide is 1:1).Methyl ethyl diketone and oxidation promotor are mixed with mixed solution according to the mol ratio of 1:5, and its methyl ethyl diketone concentration is the mixed solution of 0.5 mol/L.Copper base after cleaning is directly put into mixed solution, and reaction is 14 days under 30 ° of C conditions.After should finishing, take out product, after the washing, put into baking oven, under 30 ° of C conditions, dry 2 hours, promptly make flaky acetylacetone copper crystallite.
Embodiment 5.
Metallic copper substrate (99.9%, thickness 0.12 mm) is carried out ultrasonic cleaning 20 minutes, clean the back drying at room temperature respectively with deionized water and dehydrated alcohol again.With ammoniacal liquor (30%m) and the mixed oxidation promotor that is mixed with of urea (mol ratio of ammoniacal liquor and urea is 1:1).Methyl ethyl diketone and oxidation promotor are mixed with mixed solution according to the mol ratio of 1:5, and the concentration of its methyl ethyl diketone is 0.5 mol/L.Copper base after cleaning is directly put into mixed solution, and reaction is 14 days under 30 ° of C conditions.After should finishing, take out product, after the washing, put into baking oven, under 30 ° of C conditions, dry 2 hours, promptly make flaky acetylacetone copper crystallite.
The above is the preferred embodiments of the present invention only, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.Within the spirit and principles in the present invention all, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (7)
1. the preparation method of a sheet acetylacetone copper crystallite is characterized in that, after the metallic copper substrate is cleaned, directly puts into the mixed solution of methyl ethyl diketone and oxidation promotor, continues and reacts, washs, is drying to obtain the purpose product.
2. the preparation method of sheet acetylacetone copper crystallite according to claim 1 is characterized in that: in the mixed solution of described methyl ethyl diketone and oxidation promotor, the mol ratio of methyl ethyl diketone and oxidation promotor is 1: 0.1～10.
3. the preparation method of sheet acetylacetone copper crystallite according to claim 2 is characterized in that: in the mixed solution of described methyl ethyl diketone and oxidation promotor, wherein the methyl ethyl diketone volumetric molar concentration is 0.1～10 mol/L.
4. sheet acetylacetone copper crystallite preparation method according to claim 3 is characterized in that: in the mixed solution of described methyl ethyl diketone and oxidation promotor, oxidation promotor is one or more the mixture in ammoniacal liquor, methane amide or the urea.
5. according to the arbitrary described sheet acetylacetone copper crystallite preparation method of claim 1～4, it is characterized in that: described temperature of reaction is at 20～40 ° of C, and the reaction times is 3～15 days.
6. sheet acetylacetone copper crystallite preparation method according to claim 5, it is characterized in that: be 2～5 hours described time of drying, drying temperature is 30～50 ° of C.
7. sheet acetylacetone copper crystallite preparation method according to claim 6, it is characterized in that: the thickness of described metallic copper substrate is 0.1～0.2 mm.
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| CN 201110177130 CN102276437B (en) | 2011-06-28 | 2011-06-28 | Preparation method of flaky acetylacetone copper microcrystal |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157605A (en) * | 2007-10-19 | 2008-04-09 | 扬州市兴业助剂有限公司 | Method for producing acetylacetone copper |
| CN101508635A (en) * | 2009-03-24 | 2009-08-19 | 山东大学 | Method of preparing copper acetylacetone |
| CN101857537A (en) * | 2010-06-10 | 2010-10-13 | 扬州工业职业技术学院 | Method for preparing ferric acetyl acetonade |
-
2011
- 2011-06-28 CN CN 201110177130 patent/CN102276437B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157605A (en) * | 2007-10-19 | 2008-04-09 | 扬州市兴业助剂有限公司 | Method for producing acetylacetone copper |
| CN101508635A (en) * | 2009-03-24 | 2009-08-19 | 山东大学 | Method of preparing copper acetylacetone |
| CN101857537A (en) * | 2010-06-10 | 2010-10-13 | 扬州工业职业技术学院 | Method for preparing ferric acetyl acetonade |
Non-Patent Citations (1)
| Title |
|---|
| S. R. LONG ER AL.: "The Direct Electrochemical Synthesis of Transition Metal Acetylacetonates", 《SYNTHESIS AND REACTIVITY IN INORGANIC, METAL-ORGANIC, AND NANO-METAL CHEMISTRY》, vol. 37, 31 December 2007 (2007-12-31), pages 813 - 815 * |
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