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Zinc acetylacetonate and preparation method thereof

A technology of zinc acetylacetonate and acetylacetone, which is applied in the field of zinc acetylacetonate and its preparation, can solve the problems of low yield and achieve the effects of high yield, easy drying, and high product purity

Active Publication Date: 2022-04-08
ANHUI JIAXIAN FUNCTIONAL AUXILIARY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But all do not have the report of methyl alcohol as solvent preparation zinc acetylacetonate in the patent and literature, and this is because the solubility of zinc acetylacetonate in methanol is bigger reason, makes yield on the low side

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The preparation method of the zinc acetylacetonate that the present invention proposes, method step is as follows:

[0029] S1: Add 9.8g of zinc oxide and 100ml of reaction solvent into the reaction vessel, stir at 350r / min and heat up to a slightly boiling state. The reaction solvent is a mixture of methanol and propylene glycol methyl ether in a volume ratio of 1:0.9;

[0030] S2: Add acetylacetone with a molar ratio of 1.95:1 to the reaction vessel described in S1 dropwise in the state of slight boiling reflux, and evenly add dropwise within 0.8h, and keep the reaction for 1.8h;

[0031] S3: the temperature of the solution after the heat preservation reaction in S2 is cooled to 5° C., suction filtered, and zinc acetylacetonate is obtained after drying;

[0032] S4: Recover the mother liquor after suction filtration in S3, then add 20 ml of the reaction solvent described in S1 to the mother liquor, and repeat the recovery twice according to the method described in ste...

Embodiment 2

[0035] The preparation method of the zinc acetylacetonate that the present invention proposes, method step is as follows:

[0036] S1: Add 10.6g of zinc oxide and 100ml of reaction solvent into the reaction vessel, stir at 450r / min and heat up to a slightly boiling state. The reaction solvent is a mixture of methanol and propylene glycol methyl ether in a volume ratio of 1:1.1;

[0037] S2: Add acetylacetone with a molar ratio of 2.05:1 to the reaction vessel described in S1 dropwise in the state of slight boiling reflux, and evenly add dropwise within 1.2h, and keep the reaction for 2.2h;

[0038] S3: the temperature of the solution after the heat preservation reaction in S2 is lowered to 10° C., then suction filtered, and dried to obtain zinc acetylacetonate;

[0039] S4: Recover the mother liquor after suction filtration in S3, then add 20 ml of the reaction solvent described in S1 to the mother liquor, and repeat the recovery 4 times according to the method described in st...

Embodiment 3

[0042] The preparation method of the zinc acetylacetonate that the present invention proposes, method step is as follows:

[0043] S1: Add 10.2g of zinc oxide and 100ml of reaction solvent into the reaction vessel, stir at 400r / min and heat up to a slightly boiling state. The reaction solvent is a mixture of methanol and propylene glycol methyl ether in a volume ratio of 1:1;

[0044] S2: Add acetylacetone with a molar ratio of 2:1 to the reaction vessel described in S1 dropwise in the state of slight boiling reflux, and finish the dropwise addition evenly within 1 hour, and keep it warm for 2 hours;

[0045] S3: the temperature of the solution after the heat preservation reaction in S2 was lowered to 6° C., then suction filtered, and dried to obtain zinc acetylacetonate;

[0046] S4: Recover the mother liquor after suction filtration in S3, then add 20 ml of the reaction solvent described in S1 to the mother liquor, and repeat the recovery 3 times according to the method desc...

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PUM

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Abstract

The invention discloses zinc acetylacetonate and a preparation method thereof. The method steps are as follows: S1: add zinc oxide and a reaction solvent into a reaction vessel, stir and raise the temperature, and the reaction solvent is a mixture of methanol and propylene glycol methyl ether; S2: reflux at a slight boil Add acetylacetone dropwise to the reaction vessel described in S1 under the state, and keep it warm for reaction; S3: After cooling the solution in S2 after the heat preservation reaction, suction filter, and dry it to obtain zinc acetylacetonate; S4: After suction filtration in S3 The mother liquor is recovered, then the reaction solvent described in S1 is added to the mother liquor, and the reaction is carried out according to the method described in step S1-S3 to obtain zinc acetylacetonate. The invention does not add any catalyst, and the product has high purity; the mother liquor is continuously recycled, so that the zinc acetylacetonate dissolved in methanol in the previous reaction is continuously precipitated, thereby ensuring a high yield; at the same time, the invention has almost no waste liquid discharge, which is clean and environmentally friendly .

Description

technical field [0001] The invention relates to the technical field of chemical additives, in particular to zinc acetylacetonate and a preparation method thereof. Background technique [0002] Zinc acetylacetonate is a heat stabilizer for halides such as rigid PVC, and has a significant synergistic effect with stearyl benzoylmethane and dibenzoylmethane. It can greatly extend the service life of plastic products, so that plastic products can maintain their original color and transparency for a long time. It is a non-toxic new type of plastic stabilizer, and its cost performance is better than that of organotin series stabilizers. It is an environmentally friendly product that replaces lead-containing additives. [0003] JP2003342222 discloses a method for directly preparing zinc acetylacetonate from acetylacetone and zinc oxide. But the consumption of acetylacetone obviously exceeds stoichiometric ratio (1600ml acetylacetone reacts with 40.7g zinc oxide) in this method, be...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/92C07C45/77
Inventor 王艳李平陈新华陈翔迎
Owner ANHUI JIAXIAN FUNCTIONAL AUXILIARY