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Catalyst and preparation method, hydrotreating method of vanillin tar

A technology for catalytic hydrogenation and hydrotreating, which is applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc. The effect of solid waste generation

Active Publication Date: 2022-07-12
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Related patents focus on how to effectively recover 5-formyl vanillin, and how to convert it into high value-added products: vanillin, ortho-vanillin, but 5-formyl vanillin is only vanillin Part of the tar, the relevant patents do not directly solve the problem of vanillin tar recovery. On the other hand, the separation of 5-formyl vanillin from tar requires complicated processes such as extraction and crystallization, and the industrialization feasibility is not high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 5

[0028] In Example 5, different batches of phenol hydroxylated tars were used from those in Examples 1-4. The composition of vanillin tar: 16% vanillin, 47% 5-formyl vanillin, 20% vanillin di-focus Oil and 17% phenolic tar containing aldehyde groups.

[0029] The analytical method and calculation process adopted in the implementation process of the technical solution of the present invention are as follows:

[0030] The product concentration was analyzed by liquid chromatography, and the standard curve method was used for accurate quantification.

[0031] Liquid chromatography model: Shimadzu LC-20AT high performance liquid chromatograph;

[0032] Column model: Waters XSelect HSS T3;

[0033] Detection wavelength: 233nm

[0034] Mobile phase: acetonitrile / water (containing 0.1% phosphoric acid in water) = 35 / 65

[0035] The hydrocracking reaction performance of vanillin tar was measured using guaiacol selectivity and effective tar recovery:

[0036] Guaiacol selectivity=gu...

Embodiment 1

[0040] Weigh 10g of titanium dioxide and dissolve it in a 20ml aqueous solution in a round-bottomed flask, add 0.1g palladium nitrate dihydrate solid, 0.1g platinum nitrate solid, 0.01g cesium carbonate solid under constant stirring, continue stirring for 2 hours, and then close the stirring, After standing for 4 hours, the excess aqueous solution was removed by rotary evaporation, dried overnight for 12 hours, calcined at 400 °C for 4 hours, and finally reduced at 300 °C for 2 hours under a hydrogen atmosphere to obtain cesium salt-modified Pd / TiO 2 , Pt / TiO 2catalyst. 0.05 g of the titanium dioxide supported catalyst prepared above, 10 g of ethanol and 5 g of tar were added to the reaction kettle, and the air in the reaction kettle was replaced by hydrogen for 5 times. Under the conditions of temperature 100 ° C, pressure 1 MPa, and stirring speed 500 rpm, the reaction was carried out for 2 h, and then cooled. After reaching room temperature, the reaction solution was taken...

Embodiment 2

[0042] Weigh 10g of titanium dioxide and dissolve it in a 100ml aqueous solution in a round-bottomed flask, add 0.3g palladium nitrate dihydrate solid, 0.3g platinum nitrate solid, 0.03g cesium carbonate solid under constant stirring, continue stirring after 6 hours, close the stirring, After standing for 12 hours, the excess aqueous solution was removed by rotary evaporation, dried overnight for 12 hours, calcined at 500 °C for 6 hours, and finally reduced at 400 °C for 5 hours under a hydrogen atmosphere to obtain cesium salt-modified Pd / TiO 2 , Pt / TiO 2 catalyst. Take 0.2 g of the titanium dioxide supported catalyst prepared above, 20 g of ethanol and 5 g of tar into the reaction kettle, replace the air in the reaction kettle with hydrogen 5 times, at a temperature of 150 ° C, a pressure of 2 MPa, and a stirring speed of 800 rpm, react for 5 h, and cool to room temperature. , take out the reaction solution, filter out the catalyst, the filtrate is the hydrocracking reactio...

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Abstract

The invention relates to a catalyst, a preparation method and a hydrotreating method of vanillin tar. The catalyst comprises a cesium-containing compound, Pd / TiO 2 and Pt / TiO 2 The hydrotreating method of vanillin tar is as follows: in ethanol solvent, using vanillin tar as reaction raw material, directly catalyzing hydrocracking to recover guaiacol. The method is simple to operate, green and environmentally friendly. On the one hand, the residual vanillin and 5-aldehyde-based vanillin by-products in the vanillin tar are cracked and recovered, and at the same time, tars such as vanillin dimerization and deep oxidation are added again. Hydrogen cracking into high value-added guaiacol products. It not only reduces the treatment cost of solid waste, but also has better economic benefits.

Description

technical field [0001] The invention belongs to the technical field of catalytic hydrogenation, and in particular relates to a catalyst, a preparation method and a hydrotreating method of vanillin tar. Background technique [0002] Vanillin is one of the largest flavor and fragrance products, with a current global demand of about 27,000t, mainly used in food additives, feed additives, pharmaceutical intermediates and other fields. China is a big producer of vanillin, and about 70% of the world's production capacity is concentrated in China. At present, the mainstream process route for vanillin production is glyoxylic acid method, which is synthesized by three-step reaction of guaiacol and glyoxylic acid through condensation, oxidation and decarboxylation, followed by rectification and crystallization to produce high-quality vanillin products. The glyoxylic acid method has the disadvantage of poor selectivity in the condensation step. The purity of the crude vanillin product...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/58C07C41/18C07C43/23
CPCB01J23/58C07C41/18C07C43/23
Inventor 付松李俊平丁大康孟祥南张晨黎晓峰黎源
Owner WANHUA CHEM GRP CO LTD
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