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Comprehensive utilization method of byproduct 5-aldehyde vanillin in vanillin production process

An aldehyde-based vanillin and production process technology, applied in chemical instruments and methods, preparation of carbon-based compounds, preparation of organic compounds, etc., can solve the problem of high comprehensive utilization cost, low proportion of ortho-vanillin, and reaction yield Low problems, to achieve the effects of good economic benefits, fewer synthesis steps, and high reaction yields

Inactive Publication Date: 2013-09-25
SHANGHAI INST OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a vanillin production method to solve the technical problems of low reaction yield, low proportion of ortho-vanillin in the product and high cost of comprehensive utilization in the original 5-formyl vanillin comprehensive utilization method. Comprehensive utilization method of 5-formyl vanillin by-product

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Embodiment 1

[0026] A comprehensive utilization method of by-product 5-formyl vanillin in the production process of vanillin, specifically comprising the following steps:

[0027] (1) Take 800g of the distilled fraction of vanillin, and the content of 5-formyl vanillin reaches 93.1% after testing;

[0028] (2) Add 1.5 g of a dealdehyde catalyst to the 800 g of 5-formyl vanillin crude product obtained in step (1) with a purity of 93.1%, and control the temperature to 190°C for the dealdehyde reaction, while controlling the pressure to 6.0 Kpa carries out vacuum distillation, collects the distillate between boiling point 120~155 ℃ and promptly obtains the mixture 450g of guaiacol, ortho-vanillin and vanillin;

[0029] Described dealdehyde catalyst is the Pt / C that load capacity is 5%, the amount of the dealdehyde catalyst added is 0.19% of 5-formyl vanillin crude product weight;

[0030] In the mixture of ortho-vanillin, vanillin and guaiacol obtained above, the content of ortho-vanillin is...

Embodiment 2

[0036] A comprehensive utilization method of by-product 5-formyl vanillin in the production process of vanillin, specifically comprising the following steps:

[0037] (1), the production of vanillin obtained 1760g of 66% The by-product 5-formyl vanillin is obtained by vacuum distillation under the control pressure of 0.8kpa 920 grams The crude product of 5-formyl vanillin with a purity of 92%;

[0038] (2), obtained in step (1) 920 grams Add 1.2g of dealdehyde catalyst to the crude product of 5-formyl vanillin with a purity of 92%, control the temperature at 182°C for dealdehyde reaction, and control the pressure at 2.0kpa for vacuum distillation at the same time, the collected boiling point is 112-148 The distillate between ℃ promptly obtains the mixture of guaiacol, ortho-vanillin and vanillin 548g altogether;

[0039] Described dealdehyde catalyst is the Pd / C that load capacity is 10%, the amount of the dealdehyde catalyst added is 0.13% of 5-formyl vanillin crude pro...

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Abstract

The invention discloses a comprehensive utilization method of a byproduct 5-aldehyde vanillin in a vanillin production process. The comprehensive utilization method comprises the following steps of: taking the byproduct 5-aldehyde vanillin produced in the vanillin production process as a material, carrying out high-temperature aldehyde removal under existence of dealdehyding catalysts such as Pt / C or Pd / C and the like after proper purification to generate a mixture of ortho vanillin, vanillin and methyl catechol; and respectively obtaining the ortho vanillin, the vanillin and the methyl catechol by rectification. By adopting the comprehensive utilization method of the byproduct 5-aldehyde vanillin in the vanillin production process disclosed by the invention, not only are the three wastes reduced, but also the comprehensive utilization method has good economic benefits by transforming the 5-aldehyde vanillin into the ortho vanillin, the vanillin and the methyl catechol.

Description

technical field [0001] The invention relates to a comprehensive utilization method of by-product 5-formyl vanillin in the production process of vanillin. Background technique [0002] Vanillin is an important food additive and spice product, and its current global demand is between 17,000 and 18,000 tons. At present, vanillin is mainly synthesized by three steps of condensation, oxidation and decarboxylation of guaiacol and glyoxylic acid as raw materials. When guaiacol and glyoxylic acid are condensed, there are three selectivities for simultaneous condensation of ortho, para and ortho-para. These condensation products correspond to ortho-vanillin, vanillin and 5-formyl vanillin (i.e. 3-methoxy-4-hydroxy-5-formylbenzaldehyde). Generally, the proportions of ortho-vanillin, vanillin and 5-formyl vanillin in the primary product are generally about 2%, 93%, and 5%. At present, ortho-vanillin can be used as a raw material for the production of flavone, and vanillin is the mai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/67C07C47/575C07C47/58C07C43/23C07C41/18
Inventor 毛海舫刘年金孙揭阳吴建新王立志
Owner SHANGHAI INST OF TECH
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