CN102898294A - Preparation method for calcium acetylacetonate - Google Patents
Preparation method for calcium acetylacetonate Download PDFInfo
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- CN102898294A CN102898294A CN2012103324075A CN201210332407A CN102898294A CN 102898294 A CN102898294 A CN 102898294A CN 2012103324075 A CN2012103324075 A CN 2012103324075A CN 201210332407 A CN201210332407 A CN 201210332407A CN 102898294 A CN102898294 A CN 102898294A
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Abstract
The invention discloses a preparation method for calcium acetylacetonate. The preparation method comprises the following basic steps: (1) fully reacting an aqueous solution of calcium chloride with an aqueous solution of sodium hydroxide, carrying out pumping filtration on a reaction product to obtain a calcium hydrate precipitate and standing the calcium hydrate precipitate for subsequent usage; and (2) adding excessive acetylacetone with a concentration of 2 to 5% into methanol, then adding the calcium hydrate precipitate for a reflux reaction, carrying out pumping filtration on a reaction product after the reflux reaction is finished, washing a filter cake with methanol and drying the washed filter cake at a temperature of 90 DEG C so as to obtain the product calcium acetylacetonate. According to the invention, methanol is used as a dispersant, a two-phase reaction system is employed, newly prepared calcium hydrate is easily dispersed in methanol because of cladding of water, reactants fully contact, and the product has the advantages of high yield and a good color; reacted methanol can be cyclically used after simple treatment, and the method has low cost and is simple.
Description
Technical field
The present invention relates to the preparation method of the chemical synthesis of industrial chemicals, particularly a kind of calcium acetylacetonate.
Background technology
Calcium acetylacetonate is the halogenide thermo-stabilizers such as hard PVC, with stearoyl benzoyl methane, diphenylpropane-1,3-dione(DPPO) significant synergy is arranged.Can greatly prolong the work-ing life of plastics, make plastics can keep for a long time its former colored and transparency.Be a kind of nontoxic novel plastic stablizer, cost performance is better than organotin series stablizer, is the environmentally friendly machine that substitutes leaded auxiliary agent.
At present, the method for preparing calcium acetylacetonate mostly is liquid phase method, and traditional liquid phase method is that water or methyl ethyl diketone are done dispersion agent.When water was cooked dispersion agent, system was three-phase, and reactant can not fully contact, and yield is on the low side.When doing dispersion agent with methyl ethyl diketone, in the reaction process methyl ethyl diketone loss large because the methyl ethyl diketone price is high, cause synthetic high expensive.
Summary of the invention
In order to overcome above shortcomings in the existing calcium acetylacetonate production technique, the object of the present invention is to provide the calcium acetylacetonate preparation method that a kind of technique is simple, cost is low, yield is high.
The objective of the invention is to be achieved by the following technical programs, a kind of preparation method of calcium acetylacetonate is characterized in that, comprises following basic step:
A kind of preparation method of calcium acetylacetonate is characterized in that, comprises following basic step:
(1) calcium chloride water and aqueous sodium hydroxide solution complete reaction, the calcium hydroxide precipitation behind the reaction product suction filtration stays for subsequent use;
(2) pressing amount of substance calculates, add the methyl ethyl diketone that surpasses reacting weight 2%～5% in the methyl alcohol, then add above-mentioned calcium hydroxide back flow reaction, suction filtration reaction product after reaction finishes, and use the methanol wash filter cake, the filter cake after the washing obtains the product calcium acetylacetonate after 90 ℃ of lower dryings;
(3) filtrate merges washing methyl alcohol, adds Calcium Chloride Powder Anhydrous and dewaters, and then removes by filter the calcium chloride after the suction, and the methyl alcohol after the dehydration directly uses as next synthetic.
Reflux time is 1～2h in the step (2).
Use methanol wash filter cake 2～3 times in the step (2), the filter cake after the washing is obtaining the product calcium acetylacetonate behind 90 ℃ of lower dry 5h.
The degree of drying of self-control calcium hydroxide has remarkably influenced to the calcium acetylacetonate yield, will prepare calcium acetylacetonate after the homemade calcium hydroxide drying, and yield significantly descends.This is that particle is little, and larger surfactivity is arranged because of the calcium hydroxide of precipitator method preparation.And in the drying process, particle produces reunites, and dry rear particle becomes large, and surface-area reduces, thereby greatly reduces response capacity.Experiment finds, self-control calcium hydroxide namely moistens, and with prolonging storage period, yield also can reduce, and its reason also is due to the particle agglomeration.So every secondary response all will be used freshly prepd calcium hydroxide.
Beneficial effect of the present invention: select methyl alcohol to do dispersion agent, system is two phase reaction, and freshly prepd calcium hydroxide is because the coating of water is easy to be dispersed in the methyl alcohol, and the reactant contact is abundant, and yield is higher, and the product color and luster is good.Reacted methyl alcohol can recycle through simple process, and cost is low and technique is simple.
Embodiment
Embodiment 1:
With the water-soluble 150ml solution that is made into of 0.1mol Calcium Chloride Powder Anhydrous, with the water-soluble 150ml solution that is made into of the sodium hydroxide of 0.2mol, two solution are mixed, fully stir 15min, complete reaction generates the calcium hydroxide precipitation, and is for subsequent use behind the reaction product suction filtration; 100ml methyl alcohol is added there-necked flask, open and stir, add excessive 3% methyl ethyl diketone (scale herein shows amount of substance, and is lower same), then add the adding calcium hydroxide behind the above-mentioned suction filtration, back flow reaction 1h, reaction finishes, the suction filtration reaction product, and with a small amount of methanol wash filter cake 2 times, the filter cake of cleaning obtains the methyl ethyl diketone calcium product, yield: 96% at 90 ℃ of lower dry 5h.Filtrate merges washing methyl alcohol, adds the 10g Calcium Chloride Powder Anhydrous and dewaters, and refilters the calcium chloride of removing after the suction.Methyl alcohol after the dehydration can directly use as next synthetic.
Embodiment 2:
With the water-soluble 150ml solution that is made into of 0.1mol Calcium Chloride Powder Anhydrous, with the water-soluble 150ml solution that is made into of the sodium hydroxide of 0.2mol, two solution are mixed, fully stir 15min, complete reaction generates the calcium hydroxide precipitation, and is for subsequent use behind the reaction product suction filtration; 150ml methyl alcohol is added there-necked flask, open and stir, add excessive 2% methyl ethyl diketone, then add the calcium hydroxide behind the above-mentioned suction filtration, back flow reaction 2h, reaction finishes, the suction filtration reaction product, and with a small amount of methanol wash filter cake 3 times, the filter cake of cleaning is at 90 ℃ of lower dry 5h, obtain the methyl ethyl diketone calcium product, yield: 95%.Filtrate merges washing methyl alcohol, adds the 10g Calcium Chloride Powder Anhydrous and dewaters, and refilters the calcium chloride of removing after the suction.Methyl alcohol after the dehydration can directly use as next synthetic.
Embodiment 3:
With the water-soluble 150ml solution that is made into of 0.1mol Calcium Chloride Powder Anhydrous, with the water-soluble 150ml solution that is made into of the sodium hydroxide of 0.2mol, two solution are mixed, fully stir 15min, complete reaction generates the calcium hydroxide precipitation, and is for subsequent use behind the reaction product suction filtration; 120ml methyl alcohol is added there-necked flask, open and stir, add excessive 5% methyl ethyl diketone, then add the calcium hydroxide behind the above-mentioned suction filtration, back flow reaction 1h, reaction finishes, the suction filtration reaction product, and with a small amount of methanol wash filter cake 2 times, the filter cake of cleaning is at 90 ℃ of lower dry 5h, obtain the methyl ethyl diketone calcium product, yield: 96.5%.Filtrate merges washing methyl alcohol, adds the 10g Calcium Chloride Powder Anhydrous and dewaters, and refilters the calcium chloride of removing after the suction.Methyl alcohol after the dehydration can directly use as next synthetic.
The above only is preferred embodiment of the present invention, is not the present invention is done any pro forma restriction; Any those of ordinary skill in the art, do not breaking away from the technical solution of the present invention scope situation, all can utilize method and the technology contents of above-mentioned announcement that technical solution of the present invention is made many possible changes and modification, or be revised as the equivalent embodiment of equivalent variations.Therefore, every content that does not break away from technical solution of the present invention, any simple modification of above embodiment being done according to technical spirit of the present invention, be equal to replacements, equivalence changes and modify, all still belong in the scope that technical solution of the present invention protects.
Claims (3)
1. the preparation method of a calcium acetylacetonate is characterized in that, comprises following basic step:
(1) calcium chloride water and aqueous sodium hydroxide solution complete reaction, the calcium hydroxide precipitation behind the reaction product suction filtration stays for subsequent use;
(2) then the methyl ethyl diketone of adding excessive 2%～5% in the methyl alcohol adds above-mentioned calcium hydroxide back flow reaction, suction filtration reaction product after reaction finishes, and use the methanol wash filter cake, the filter cake after the washing obtains the product calcium acetylacetonate after 90 ℃ of lower dryings;
(3) filtrate merges washing methyl alcohol, adds Calcium Chloride Powder Anhydrous and dewaters, and then removes by filter the calcium chloride after the suction, and the methyl alcohol after the dehydration directly uses as next synthetic.
2. the preparation method of a kind of calcium acetylacetonate according to claim 1 is characterized in that, reflux time is 1～2h in the step (2).
3. the preparation method of a kind of calcium acetylacetonate according to claim 1 is characterized in that, uses methanol wash filter cake 2～3 times in the step (2), and the filter cake after the washing is obtaining the product calcium acetylacetonate behind 90 ℃ of lower dry 5h.
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| CN2012103324075A CN102898294A (en) | 2012-09-11 | 2012-09-11 | Preparation method for calcium acetylacetonate |
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| CN2012103324075A CN102898294A (en) | 2012-09-11 | 2012-09-11 | Preparation method for calcium acetylacetonate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107057215A (en) * | 2016-12-21 | 2017-08-18 | 安徽佳先功能助剂股份有限公司 | A kind of modified calcium acetylacetonate zinc complexes and its application |
| CN109734569A (en) * | 2019-03-08 | 2019-05-10 | 合肥工业大学 | A kind of method that intensified by ultrasonic wave photocatalysis continuously prepares acetylacetone metallic compound |
| CN109824499A (en) * | 2019-03-08 | 2019-05-31 | 合肥工业大学 | A kind of method that microwave reinforced photocatalysis continuously prepares acetylacetone metallic compound |
| CN110128254A (en) * | 2019-06-11 | 2019-08-16 | 东莞市汉维科技股份有限公司 | A kind of preparation process of acetylacetonate |
| CN110723744A (en) * | 2018-07-17 | 2020-01-24 | 靖江市康高特塑料科技有限公司 | Hydrothermal synthesis method for improving initial whiteness of hydrotalcite |
-
2012
- 2012-09-11 CN CN2012103324075A patent/CN102898294A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 李广梅: "乙酰丙酮及乙酰丙酮钙的制备", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
| 李广梅等: "乙酰丙酮盐的制备与应用", 《化工中间体》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107057215A (en) * | 2016-12-21 | 2017-08-18 | 安徽佳先功能助剂股份有限公司 | A kind of modified calcium acetylacetonate zinc complexes and its application |
| CN107057215B (en) * | 2016-12-21 | 2019-08-30 | 安徽佳先功能助剂股份有限公司 | A kind of preparation method of modified calcium acetylacetonate zinc complexes |
| CN110723744A (en) * | 2018-07-17 | 2020-01-24 | 靖江市康高特塑料科技有限公司 | Hydrothermal synthesis method for improving initial whiteness of hydrotalcite |
| CN109734569A (en) * | 2019-03-08 | 2019-05-10 | 合肥工业大学 | A kind of method that intensified by ultrasonic wave photocatalysis continuously prepares acetylacetone metallic compound |
| CN109824499A (en) * | 2019-03-08 | 2019-05-31 | 合肥工业大学 | A kind of method that microwave reinforced photocatalysis continuously prepares acetylacetone metallic compound |
| CN110128254A (en) * | 2019-06-11 | 2019-08-16 | 东莞市汉维科技股份有限公司 | A kind of preparation process of acetylacetonate |
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Inventor after: Li Dui Inventor after: Huang Xiansheng Inventor after: Li Ping Inventor after: Wang Yan Inventor after: Chen Xinhua Inventor after: Zhang Guojing Inventor before: Li Dui Inventor before: Huang Xiansheng Inventor before: Li Ping Inventor before: Wang Yan Inventor before: Chen Xinhua |
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Free format text: CORRECT: INVENTOR; FROM: LI DUI HUANG XIANSHENG LI PING WANG YAN CHEN XINHUA TO: LI DUI HUANG XIANSHENG LI PING WANG YAN CHEN XINHUA ZHANG GUOLIANG |
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Application publication date: 20130130 |