Novel method for efficiently synthesizing dibenzoylmethane

A technology for dibenzoylmethane and methyl benzoate, which is applied in the field of novel and efficient synthesis of dibenzoylmethane, can solve the problems of high cost of raw materials, many by-products, low yield of dibenzoylmethane, etc., and achieves condensation The effect of short reaction period, less by-products and cost reduction

Inactive Publication Date: 2020-02-21
SHANDONG RUIFENG CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The preparation method of dibenzoylmethane in the prior art has high cost of main raw materials, long condensation reaction cycle, many by-products, low yield of dibenzoylmethane, solvent can not be fully recycled and has a negative effect on improving thermoplastic resin. Problems with poor photothermal stability

Method used

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  • Novel method for efficiently synthesizing dibenzoylmethane
  • Novel method for efficiently synthesizing dibenzoylmethane
  • Novel method for efficiently synthesizing dibenzoylmethane

Examples

Experimental program
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Effect test

Embodiment 1

[0087] Prepare dibenzoylmethane of the present invention according to the following steps

[0088] ① . Synthesis of methyl benzoate

[0089] Using benzoic acid and methanol as raw materials, using sulfuric acid as a catalyst, it is prepared by esterification and distillation

[0090] a. Esterification process conditions

[0091] Benzoic acid / methanol molar ratio 1:4 ~ 1:6

[0092] The esterification reaction temperature is 70-80°C

[0093] Response time hours 4 to 5

[0094] Put 366g of benzoic acid and 384g of methanol into a three-necked flask, raise the temperature to 70°C-80°C, and wait until the benzoic acid is completely dissolved

[0095] After thawing, concentrated sulfuric acid was added dropwise, and the reaction was refluxed for 4-5 hours. After the reaction is completed, distill and recover the residual methanol to obtain the crude product.

[0096] b. Esterification solution treatment

[0097] The esterification solution from step a is washed with water, al...

Embodiment 2～ Embodiment 5

[0127] According to the method and steps of Example 1, the stearoylbenzoylmethane product of the present invention is prepared according to the formula in Table 1

[0128] Table 1

[0129]

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Abstract

The invention relates to a novel method for efficiently synthesizing dibenzoylmethane. The product (dibenzoylmethane) is non-toxic, tasteless and widely used in PVC (polyvinyl chloride) plastics and ABS (acrylonitrile butadiene styrene) resins. The invention belongs to preparation of compounds containing C0 groups and only connecting carbon or hydrogen atoms, in particular relates to preparation of beta-dione. The method is characterized in that the dibenzoylmethane is prepared from methyl benzoate and acetophenone through a condensation reaction in an alkaline environment. The methyl benzoateis prepared from benzoic acid and methanol as raw materials and sulfuric acid as a catalyst through an esterification reaction. The main raw material, namely the methyl benzoate, of the target product, namely dibenzoylmethane, of the method, is prepared through a self-designed process, a catalyst, namely sodium methoxide, of the condensation reaction, is prepared according to the self-designed process, and technological conditions of the key steps of the condensation reaction for synthesizing the dibenzoylmethane are optimized. The invention provides the method for preparing the dibenzoylmethane with low raw material cost, a short condensation reaction period, few by-products, a high yield of dibenzoylmethane, complete solvent recovery and an excellent capability for improving photothermal stability of a thermoplastic resin. The condensation yield is 85%, and the crystallization yield is 95%.

Description

technical field [0001] The invention is a novel and efficient method for synthesizing dibenzoylmethane. It belongs to the preparation of compounds containing CO groups, only connected to carbon or hydrogen atoms, especially the preparation of β-diketones. Background technique [0002] Dibenzoylmethane is an important light and heat stabilizer for thermoplastics with β-diketone structure. The product is non-toxic and odorless, and is widely used in PVC plastics and ABS resins. At present, light stabilizers are mainly hindered amines, benzotriazoles and benzophenones. Efficient, multi-functional and non-toxic are the development directions of stabilizer products suitable for thermoplastic resin molding processing. Following the trend of environmental protection, the production of polluting and toxic stabilizers should be reduced. The production and promotion of β-diketone additives should be developed and increased. [0003] Compared with commonly used varieties, dibenzoylm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/45C07C49/784
CPCC07C45/455C07C67/08C07C69/78C07C49/784
Inventor 张振国王滨焦淑元
Owner SHANDONG RUIFENG CHEM
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