CN110922318A - Preparation method of calcium acetylacetonate - Google Patents
Preparation method of calcium acetylacetonate Download PDFInfo
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- CN110922318A CN110922318A CN201911383798.1A CN201911383798A CN110922318A CN 110922318 A CN110922318 A CN 110922318A CN 201911383798 A CN201911383798 A CN 201911383798A CN 110922318 A CN110922318 A CN 110922318A
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- calcium
- preparation
- calcium acetylacetonate
- acetylacetonate
- acetylacetone
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/77—Preparation of chelates of aldehydes or ketones
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method of calcium acetylacetonate, which adopts a dry method for preparation, wherein the acetylacetone and calcium hydroxide quantitatively enter a special reactor, and a solvent is not used any more, so that the influence of the solvent on a functional complex is eliminated, the defects of long reaction time, low yield, more byproducts and the like of a liquid phase method are avoided, and the preparation method has the advantages of high reaction speed, mild conditions, simplicity in operation, high selectivity, high yield, low energy consumption and the like.
Description
Technical Field
The invention belongs to the technical field of organic synthesis, and particularly relates to a preparation method of calcium acetylacetonate.
Background
The calcium acetylacetonate is a halide heat stabilizer such as hard PVC and the like, and has obvious synergistic effect with stearoylbenzoylmethane and dibenzoylmethane; the service life of the plastic product can be greatly prolonged, so that the plastic product can keep the original color and transparency for a long time; is a non-toxic novel plastic stabilizer, has better cost performance than organic tin series stabilizers, and is an environment-friendly product for replacing lead-containing additives. Due to the attention of many special properties, the synthesis process and the application development become the current hot topic. At present, most of preparation methods of calcium acetylacetonate are liquid phase methods, and the traditional liquid phase method process has the defects of long preparation time, more byproducts, low yield, poor color, high cost and the like due to the fact that the calcium acetylacetonate is partially decomposed by reaction in an aqueous solution and the large energy consumption is needed for liquid phase separation, so that the improvement of the synthesis method of the calcium acetylacetonate is of great significance.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the preparation method of the calcium acetylacetonate, which has the advantages of simple process, low cost and high yield.
The invention aims to realize the preparation method of calcium acetylacetonate, which adopts the following technical scheme that the molar ratio of raw materials of acetylacetone and calcium hydroxide is 2-4: 1.
The preferred molar ratio of starting materials acetylacetone to calcium hydroxide is 3: 1.
A preparation method of calcium acetylacetonate comprises the following steps:
the method comprises the following steps: weighing acetylacetone and solid calcium hydroxide, and grinding the solid calcium hydroxide for later use;
step two: starting a feeding device, and allowing acetylacetone and ground solid calcium hydroxide to enter a special reactor at the temperature of 20-30 ℃ to obtain wet product calcium acetylacetonate;
step three: and drying the wet calcium acetylacetonate in the second step to obtain the final product calcium acetylacetonate.
Preferably, in step two, the special reactor is an atomization device.
In the invention, the acetylacetone feed liquid is fed to the top of the tower, and the acetylacetone is sprayed into atomized liquid drops by atomizing equipment, the surface area of the liquid drop groups is large, the liquid drops rapidly react after contacting ground solid calcium hydroxide particles, moisture is rapidly evaporated after contacting high-temperature hot air, and a dry calcium acetylacetonate product is obtained in a very short time.
The invention provides a novel preparation method of calcium acetylacetonate, aiming at the defects of long preparation time, more byproducts, low yield, poor color, complex purification, high cost and the like of the existing preparation process of calcium acetylacetonate. The method adopts dry preparation, acetylacetone and calcium hydroxide quantitatively enter a special reactor, and the influence of a solvent on a functional complex is eliminated because the solvent is not used any more, so that the defects of long reaction time, low yield, more byproducts and the like of a liquid phase method are overcome, and the method has the advantages of high reaction speed, mild conditions, simplicity in operation, high selectivity, high yield, low energy consumption and the like.
Detailed Description
Example 1: a preparation method of calcium acetylacetonate comprises the following specific steps:
the method comprises the following steps: weighing acetylacetone and solid calcium hydroxide according to the molar ratio of 2:1, and grinding the solid calcium hydroxide for later use;
step two: starting a feeding device, and allowing acetylacetone and ground solid calcium hydroxide to enter a special reactor at the temperature of 20-30 ℃ to obtain wet product calcium acetylacetonate;
step three: and drying the wet calcium acetylacetonate in the second step to obtain the final product calcium acetylacetonate.
Preferably, in step two, the special reactor is an atomization device.
The purity of the calcium acetylacetonate is 99.1 percent, and the product yield is more than 99.6 percent.
Example 2: a preparation method of calcium acetylacetonate comprises the following specific steps:
the method comprises the following steps: weighing acetylacetone and solid calcium hydroxide according to a molar ratio of 3:1, and grinding the solid calcium hydroxide for later use;
step two: starting a feeding device, and allowing acetylacetone and ground solid calcium hydroxide to enter a special reactor at the temperature of 20-30 ℃ to obtain wet product calcium acetylacetonate;
step three: and drying the wet calcium acetylacetonate in the second step to obtain the final product calcium acetylacetonate.
Preferably, in step two, the special reactor is an atomization device.
The purity of the calcium acetylacetonate is 99.5 percent, and the product yield is more than 99.2 percent.
Example 3: a preparation method of calcium acetylacetonate comprises the following specific steps:
the method comprises the following steps: weighing acetylacetone and solid calcium hydroxide according to a molar ratio of 4:1, and grinding the solid calcium hydroxide for later use;
step two: starting a feeding device, and allowing acetylacetone and ground solid calcium hydroxide to enter a special reactor at the temperature of 20-30 ℃ to obtain wet product calcium acetylacetonate;
step three: and drying the wet calcium acetylacetonate in the second step to obtain the final product calcium acetylacetonate.
Preferably, in step two, the special reactor is an atomization device.
The purity of the calcium acetylacetonate is 99.2 percent, and the product yield is more than 99.3 percent.
Finally, it is also noted that the above-mentioned lists merely illustrate a few specific embodiments of the invention. It is obvious that the invention is not limited to the above embodiments, but that many variations are possible. All modifications which can be derived or suggested by a person skilled in the art from the disclosure of the present invention are to be considered within the scope of the invention.
Claims (4)
1. The preparation method of calcium acetylacetonate is characterized in that the molar ratio of acetylacetone to calcium hydroxide in the process is 2-4: 1.
2. The method for preparing calcium acetylacetonate according to claim 1, wherein a molar ratio of said acetylacetone to said calcium hydroxide is 3: 1.
3. The preparation method of calcium acetylacetonate is characterized by comprising the following steps:
the method comprises the following steps: weighing acetylacetone and solid calcium hydroxide, and grinding the solid calcium hydroxide for later use;
step two: starting a feeding device, and allowing acetylacetone and ground solid calcium hydroxide to enter a special reactor at the temperature of 20-30 ℃ to obtain wet product calcium acetylacetonate;
step three: and drying the wet calcium acetylacetonate in the second step to obtain the final product calcium acetylacetonate.
4. The method for preparing calcium acetylacetonate according to claim 3, wherein in step two, said special reactor is an atomization equipment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911383798.1A CN110922318A (en) | 2019-12-28 | 2019-12-28 | Preparation method of calcium acetylacetonate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911383798.1A CN110922318A (en) | 2019-12-28 | 2019-12-28 | Preparation method of calcium acetylacetonate |
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| CN110922318A true CN110922318A (en) | 2020-03-27 |
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| CN201911383798.1A Pending CN110922318A (en) | 2019-12-28 | 2019-12-28 | Preparation method of calcium acetylacetonate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113816842A (en) * | 2021-10-11 | 2021-12-21 | 山东键兴新材料科技有限公司 | Calcium acetylacetonate, preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6093844A (en) * | 1996-03-15 | 2000-07-25 | Henkel Kommanditgesellschaft Auf Aktien (Kgaa) | Method of producing alkaline-earth salts of aliphatic β-keto compounds |
| CN1280120A (en) * | 1999-07-12 | 2001-01-17 | 河北省邢台市人民制药厂 | Process for preparing sodium diacetate |
-
2019
- 2019-12-28 CN CN201911383798.1A patent/CN110922318A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6093844A (en) * | 1996-03-15 | 2000-07-25 | Henkel Kommanditgesellschaft Auf Aktien (Kgaa) | Method of producing alkaline-earth salts of aliphatic β-keto compounds |
| CN1280120A (en) * | 1999-07-12 | 2001-01-17 | 河北省邢台市人民制药厂 | Process for preparing sodium diacetate |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113816842A (en) * | 2021-10-11 | 2021-12-21 | 山东键兴新材料科技有限公司 | Calcium acetylacetonate, preparation method and application thereof |
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Application publication date: 20200327 |
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