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Calcium acetylacetonate, preparation method and application thereof

A technology of calcium acetylacetonate and acetylacetone, which is applied in the field of chemical raw material synthesis, can solve the problems of affecting the whiteness of products, complicated process, high cost, etc., achieve the effects of improving whiteness and thermal stability, suitable for popularization and application, and low production cost

Active Publication Date: 2021-12-21
山东键兴新材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] CN110922318A discloses a preparation method of calcium acetylacetonate, which utilizes the contact reaction of atomized acetylacetone and solid calcium hydroxide after grinding to prepare calcium acetylacetonate. Since the invention no longer uses solvents, it eliminates the effect of solvents on functional complexes. The impact of the liquid phase method avoids the disadvantages of long reaction time, low yield, and many by-products, and has the advantages of fast reaction speed, mild conditions, simple operation, high selectivity, high yield, and low energy consumption. However, the method prepares Calcium acetylacetonate has a strong odor and characteristic color. Adding it to PVC for processing will affect the whiteness of the product, so it is not suitable for industrialization
[0005] CN102898294A discloses a preparation method of calcium acetylacetonate, comprising the following basic steps: (1) complete reaction of calcium chloride aqueous solution and sodium hydroxide aqueous solution, and the calcium hydroxide precipitate after suction filtration of the reaction product is reserved for later use; (2) methanol Add an excess of 2% to 5% acetylacetone, then add the above-mentioned calcium hydroxide to reflux reaction, filter the reaction product after the reaction, and wash the filter cake with methanol, and dry the washed filter cake at 90°C to obtain the product acetylacetone Calcium; the invention selects methanol as a dispersant, and the system is a two-phase reaction. The newly prepared calcium hydroxide is easily dispersed in methanol due to the coating of water, the reactants are fully exposed, the yield is high, and the product color is good, but The invention uses methanol as a solvent, so it is difficult to completely recover methanol in the production process, and the environmental protection index is difficult to meet the relevant national standards, and there are problems such as complicated process, high energy consumption and high cost.

Method used

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preparation example Construction

[0029] The preparation method of described calcium hydroxide comprises the following steps:

[0030] (1) Add 1M hydrochloric acid to the calcium chloride aqueous solution to adjust the pH to 3.0 to obtain an acidic calcium chloride solution;

[0031] (2) in the acidic calcium chloride solution that step (1) obtains, drip the hydrogen peroxide of 32% by volume percentage, be warming up to 60 ℃, insulated and stirred for 60min, add sodium hydroxide to adjust pH to 7.0, filter, obtain calcium chloride Purified solution;

[0032] (3) adding sodium hydroxide to the calcium chloride purified solution obtained in step (2) to adjust the pH to 11, and then suction filtering, washing, drying, and pulverizing to obtain calcium hydroxide powder.

Embodiment 1

[0034] A preparation method for calcium acetylacetonate, comprising the following steps:

[0035] S1, mixing calcium hydroxide with fumed silica and β-cyclodextrin to obtain a calcium hydroxide mixture;

[0036] The mass ratio of calcium hydroxide, fumed silica and β-cyclodextrin is 1:0.2:0.04;

[0037] S2. Add acetylacetone dropwise while stirring to the calcium hydroxide mixture obtained in step S1. After the dropwise addition, continue stirring to obtain calcium acetylacetonate;

[0038] The molar ratio of acetylacetone and calcium hydroxide is 2.5:1.

Embodiment 2

[0040] A preparation method for calcium acetylacetonate, comprising the following steps:

[0041] S1, mixing calcium hydroxide with fumed silica and β-cyclodextrin to obtain a calcium hydroxide mixture;

[0042] The mass ratio of calcium hydroxide, fumed silica and β-cyclodextrin is 1:0.1:0.05;

[0043] S2. Add acetylacetone dropwise while stirring to the calcium hydroxide mixture obtained in step S1. After the dropwise addition, continue stirring to obtain calcium acetylacetonate;

[0044] The molar ratio of acetylacetone and calcium hydroxide is 2.2:1.

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Abstract

The invention discloses calcium acetylacetonate, a preparation method and application thereof. The preparation method comprises the following steps: S1, mixing calcium hydroxide with fumed silica and beta-cyclodextrine to obtain a calcium hydroxide mixture; and S2, dropwise adding acetylacetone into the calcium hydroxide mixture while stirring, and continuously stirring after dropwise adding to obtain the calcium acetylacetonate. According to the invention, acetylacetone and calcium hydroxide are taken as main raw materials for direct reaction, so that no wastewater is generated, environmental pollution is reduced, and the method is more environment-friendly; a proper amount of fumed silica and beta-cyclodextrine are added, so that the odor of calcium acetylacetonate can be effectively reduced, and the whiteness of calcium acetylacetonate can be increased; and the calcium acetylacetonate prepared by the invention can generate a synergistic effect with a main effect heat stabilizer, can obviously improve the whiteness and heat stability of a product when being applied to polyvinyl chloride production, and is more suitable for popularization and application.

Description

technical field [0001] The invention belongs to the technical field of chemical raw material synthesis, and relates to a heat stabilizer calcium acetylacetonate, a preparation method and an application thereof. Background technique [0002] Polyvinyl chloride (PVC) is an important plastic raw material with good physical and mechanical properties. Its annual output ranks second only to polyethylene. It can be used to produce various building materials, such as: plastic doors and windows, pipes, floors, building templates, agricultural films, cables, packaging and many other aspects. However, PVC has poor thermal stability. Under processing conditions, affected by heat and shear force, it shows poor thermal stability, and it is easy to release HCl and start to degrade, losing its proper performance. Therefore, heat stabilizers must be added to the PVC formulation system to prevent thermal degradation during processing and application. [0003] Calcium acetylacetonate is a ne...

Claims

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Application Information

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IPC IPC(8): C07C45/77C07C49/92C01F11/02C08K5/00C08L27/06C08L33/04
CPCC07C45/77C07C49/92C01F11/02C08K5/0091C08L27/06C08L2201/08C08L33/04
Inventor 林永祥谷诗荣闵建中代炜
Owner 山东键兴新材料科技有限公司
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