Method for preparing acetylacetone acid molybdenum

A technology of molybdenum acetylacetonate and acetylacetone, which is applied in the chemical field, can solve the problems of ammonium nitrate explosive, large environmental pollution, and ammonia water is easy to volatilize, and achieve the effects of less environmental pollution, less side reactions, and avoiding self-polymerization

Inactive Publication Date: 2008-02-06
ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, organic alkali ammonia water has been used, and ammonia water is volatile, difficult to control, highly irritating, and pollutes the environment greatly, so it is difficult to be widely used in industry; ammonia water and HNO 3 The generated ammonium nitrate is explosive and dangerous during production; HNO 3 As a strong oxidizing acid, it will partially oxidize the product and affect the yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Molybdenum trioxide 28.8g (0.2mol), sodium carbonate 31.8g (0.3mol), 200ml water, stir to dissolve, add antioxidant BHA (butyl hydroxyanisole) 1.5g, water bath heat up to 60 ° C, then add acetylacetone dropwise 40g (0.4mol), the dropping time is controlled at 2h, and the pH is adjusted to 3-4 with 8% sulfuric acid (about 200ml) after the dropping, and pale yellow crystals are precipitated, and then stirred at 50°C for 1.5h. Cool to 0°C, stand still for 1 hour, filter with suction, wash the filter cake with water until the pH is neutral, and finally wash the filter cake with 50ml of ethanol, and dry it under reduced pressure at 50°C to obtain light yellow crystal molybdenum acetylacetonate, 60g, yield 92%.

Embodiment 2

[0015] Molybdenum trioxide 28.8g (0.2mol), sodium hydroxide 10g (0.25mol), 80ml water, stir to dissolve, add antioxidant TBHQ (tert-butyl hydroquinone) 0.86g, water bath heats up to 40 ℃, then add dropwise Add 40 g (0.4 mol) of acetylacetone, and the dropping time is controlled within 2 hours. After the dropping, use 6% hydrochloric acid (about 200 ml) to adjust the pH to 3. Light milky white crystals of molybdenum acetylacetonate are precipitated, and then keep stirring at 40°C for 2 hours. Cool to -5°C, filter with suction, wash the filter cake with water until the pH is neutral, finally wash the filter cake with 50ml of ethanol, dry it under vacuum at 50°C, 61g, yield 93.5%.

Embodiment 3

[0017] 50g (0.347mol) of molybdenum trioxide, 48g (0.347mol) of potassium carbonate, 250ml of water, stir to dissolve, add 1.0g of anti-oxidation BHT (dibutylhydroxytoluene), heat the water bath to 70°C, and then add 69.4g of acetylacetone dropwise (0.694mol), the dropping time was controlled at 1h, and the pH was adjusted to 3 with 10% hydrochloric acid (about 250ml) after the dropping, and yellow crystals of molybdenum acetylacetonate were precipitated, and then kept stirring at 70°C for 2h. Cool to -5°C, filter with suction, wash the filter cake with water until the pH is neutral, and finally wash the filter cake with 50ml of ethanol, dry it under reduced pressure at 50°C, 102g, yield 90%.

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Abstract

The invention discloses a preparation process for molybdenum acetylacetonate. In the prior art, the acetylacetone is easy to be oxidized in the air and polymerized under refluence, so the unreacted molybdenum trioxide and by-products exist in the product, the product is impure and has low yields. In the invention, the molybdenum trioxide is dissolved into the weak-base inorganic alkaline solution, then the antioxidant is added into the solution, the temperature rises to forty to seventy Celsius system, the acetylacetone is dripped into the solution, then the non-oxidizing inorganic acid is added to adjust the solution to the weak acid, then the temperature is preserved until the crystal of molybdenum (II) 2,4-pentanedionate hydrate is precipitated; then the procedure of cooling, filtering, fulling is done to remove the adhesive acetylacetone from the filter cake. The invention is reacted with the molybdenum trioxide under low temperature, thereby the invention avoids the self-polymerization of the acetylacetone, and has less side reactions, high yields as well as high purity.

Description

technical field [0001] The invention relates to the field of chemistry, in particular to a method for preparing molybdenum acetylacetonate. Background technique [0002] Molybdenum acetylacetonate is a relatively important organic compound of molybdenum, which is mainly used to prepare oxymolybdenum compounds of Schiff bases. Using molybdenum acetylacetonate to catalyze the rearrangement of methylbutynol to pentenal, and its catalyzed rearrangement of dihydrodehydrolinalool to prepare dihydrocitral. Using molybdenum acetylacetonate as an oxidation catalyst, phenanthrene can be oxidized to phenanthrenequinone in liquid phase. Molybdenum acetylacetonate is loaded with styrene and can be used as a catalyst for the quantitative epoxidation of cyclohexene with tert-butyl hydroperoxide to synthesize epoxycyclohexane. It is also the catalyst for the synthesis of tris(pentafluorophenyl)molybdenum borate main ingreadient. Molybdenum acetylacetonate is more and more widely used as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/77C07C49/92C07F11/00
Inventor 陈建辉
Owner ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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