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Preparation method of stearoylbenzoylmethane

A technology of stearoylbenzoylmethane and fatty benzoylmethane, which is applied in the field of preparation of stearoylbenzoylmethane, can solve the problem of affecting the synthesis efficiency of stearoylbenzoylmethane, the low purity of finished products, and the preparation of stearoylbenzoylmethane. High temperature and other problems, to achieve the effect of short production cycle, high yield, simple wastewater treatment

Pending Publication Date: 2022-06-28
ANHUI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The condensation reaction in the existing process has the problems of long reaction cycle, high preparation temperature, low purity of finished product, many by-products, and large energy consumption
Seriously affect the synthesis efficiency of stearoylbenzoylmethane, affecting its output

Method used

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  • Preparation method of stearoylbenzoylmethane
  • Preparation method of stearoylbenzoylmethane
  • Preparation method of stearoylbenzoylmethane

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0031] Embodiment 1: a kind of preparation method of stearoyl benzoyl methane

[0032] A preparation method of stearoyl benzoyl methane, comprising the steps:

[0033] Step 1: Synthesize dibenzoylmethane, according to the mass ratio, N,N-dimethylformamide: acetophenone: methyl benzoate: sodium tert-butoxide=9:1:3:1, to a 250mL reactor 50mL of N,N-dimethylformamide, 5.64g of sodium tert-butoxide and 15.84g of methyl stearate were added to the mixture, and then the air in the reactor was driven off with nitrogen, and the temperature was heated while maintaining a nitrogen atmosphere and stirring. to 50°C, then slowly drip 5.28g of acetophenone (the rate of dripping is 1.5-3mL / min) under the condition of insulation, after the completion of the dripping of acetophenone, continue the reaction for 3.5 hours, and move the solution after the end of the reaction. Remove the heat source and stop the nitrogen flow;

[0034] Step 2: After treatment, add hydrochloric acid to the reaction...

Embodiment 2

[0043] Embodiment 2: a kind of preparation method of stearoyl benzoyl methane

[0044] A preparation method of stearoyl benzoyl methane, comprising the steps:

[0045]Step 1: Synthesize dibenzoylmethane, by mass ratio, N,N-dimethylformamide: acetophenone: methyl benzoate: sodium tert-butoxide=8:1:3:1, to 2L reactor Add 1L of N,N-dimethylformamide, 56.4g of sodium tert-butoxide and 158.2g of methyl stearate, then use nitrogen to drive out the air in the reactor, and heat up the reactor while maintaining a nitrogen atmosphere and stirring. to 50°C, then slowly drip 52.8g of acetophenone (the rate of dripping is 1.5-3mL / min) under the condition of insulation, after the completion of the dripping of acetophenone, continue the reaction for 3.5 hours, and move the solution after the end of the reaction. Remove the heat source and stop the nitrogen flow;

[0046] Step 2: After treatment, add concentrated hydrochloric acid to the reaction system to neutralize to neutrality, then add...

Embodiment 3

[0048] Embodiment 3: a kind of preparation method of stearoyl benzoyl methane

[0049] A preparation method of stearoylbenzoylmethane, comprising the following steps:

[0050] Step 1: add organic solvent, catalyzer and methyl stearate to the reactor, then use inert gas to drive out the air in the reactor, under the condition of keeping inert atmosphere and stirring, heat up to the reaction temperature, then under the condition of keeping inert atmosphere and stirring Add acetophenone under the conditions, continue to react after the addition of acetophenone, stop heating and stop the inert gas;

[0051] Step 2: adjust the pH value of the reaction system to neutrality, then add distilled water, and stir to separate out the product crystals, and filter to obtain a crude product;

[0052] Step 3: The crude product was added to methanol, stirred and washed at room temperature to obtain the product.

[0053] A preferred embodiment is: the catalyst is a mixture of sodium tert-buto...

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Abstract

The invention relates to a stearoylbenzoylmethane preparation method, which comprises: 1, adding an organic solvent, a catalyst and methyl stearate into a reactor, removing air in the reactor by using an inert gas, heating to a reaction temperature under the conditions of maintaining an inert atmosphere and stirring, adding acetophenone under the condition of heat preservation, and carrying out a reaction for 2-3 h to obtain a reaction product; continuously reacting after the acetophenone is added, stopping heating, and stopping introducing the inert gas; 2, adjusting the pH value of the reaction system to be neutral, then adding distilled water, stirring to separate out product crystals, and filtering to obtain a crude product; and step 3, adding the crude product into methanol, and stirring and washing at room temperature to obtain the product. The yield of the synthesis process reaches 85%, and the purity reaches 98.5%.

Description

technical field [0001] The invention relates to a preparation method of stearoylbenzoylmethane, belonging to the technical field of chemical industry. Background technique [0002] The structural formula of the stearoylbenzoylmethane molecule: [0003] [0004] Stearoylbenzoylmethane (1-phenyleicosane-1,3-dione, Stearoylbenzoylmethane, SBM) is an important light stabilizer and heat stabilizer for thermoplastics with β-diketone structure , is widely used in polyvinyl chloride (PVC) plastics and acrylonitrile-butadiene-styrene (ABS) resins, it can be compounded with a variety of stabilizers, and through the synergy between components, it can effectively improve the The transparency and weather resistance of vinyl chloride products can avoid precipitation and "zinc burning" during processing. It can not only reduce the early coloring of plastic products, but also improve the later stability. Compared with common stabilizers, it has good thermal stability, chemical stabili...

Claims

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Application Information

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IPC IPC(8): C07C45/45C07C45/78C07C45/81C07C49/76
CPCC07C45/455C07C45/78C07C45/81C07C49/76
Inventor 张忠洁卜丽丹勾林陈祥迎
Owner ANHUI UNIVERSITY
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