Preparation of diisobutyl phthalate by electrocatalytic degradation of lignin in a fixed bed reactor

A diisobutyl phthalate, fixed bed reactor technology, applied in the chemical industry, electrolysis process, electrolysis components and other directions, can solve the problems of increased industrial production cost, expensive catalyst, long reaction period, etc. The effect of industrial application value, mild reaction conditions and simple process technology

Active Publication Date: 2015-10-28
HEBEI UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

For example, the Chinese invention patent (application number: 201110114836) proposes to use solid phthalic anhydride or liquid phthalic anhydride and isobutanol esterification to synthesize DIBP, but the reaction cycle is long, the catalyst is expensive, and the cost of industrial production increases.

Method used

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  • Preparation of diisobutyl phthalate by electrocatalytic degradation of lignin in a fixed bed reactor
  • Preparation of diisobutyl phthalate by electrocatalytic degradation of lignin in a fixed bed reactor
  • Preparation of diisobutyl phthalate by electrocatalytic degradation of lignin in a fixed bed reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] (1) First prepare a 0.5mol / L NaOH solution, take out 20mL of it and dilute it to a 1L volumetric flask to prepare a pH=11 NaOH solution.

[0040] (2) Dissolve 11 g of lignin in 1 L of the NaOH solution prepared in step (1), the lignin concentration is 11 g / L, and pour it into the three-dimensional fixed-bed reactor 8 as an electrolyte, and the remaining lignin alkali solution is introduced into the storage tank 13 middle.

[0041] (3) Connect working electrode 1, auxiliary electrode 2 and reference electrode 5 to TD-3691A potentiostat 9 (Tianjin Zhonghuan Electronic Instrument Co., Ltd.) with wires respectively.

[0042] (4) Turn on the circulating pump 4 to drive the lignin alkali solution in the storage tank 13 into the three-dimensional fixed-bed reactor 8 through the inlet 11, and the electrolyzed reaction solution flows into the extraction bottle 7 through the outlet 12, extraction, and layering. , the lower layer liquid, that is, the extracted reaction liquid, fl...

Embodiment 2～8

[0050] In Examples 2-8, under the conditions of reaction time of 4h, pH=13, and lignin concentration of 11g / L, the effects of different current densities on the product DIBP concentration (see Table 1), other operation steps are the same as those in Example 1.

[0051] Table 1 Effect of current density on the concentration of diisobutyl phthalate

[0052] project

Embodiment 9～11

[0054] Examples 9-11 have a reaction time of 4h and a current density of 25mA / cm 2 , the effect of different pH values ​​on the concentration of product DIBP under the condition of lignin concentration of 11g / L (see Table 2), and other operation steps are the same as those in Example 1.

[0055] Table 2 The effect of pH value on the concentration of diisobutyl phthalate

[0056] project

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Abstract

The invention is a method for electrochemically degrading lignin to prepare diisobutyl phthalate. The method uses Ti / SnO 2- Sb 2 o 3 -Fe(NO 3 ) 3 / PbO 2 As the working electrode, the copper mesh electrode is used as the auxiliary electrode, the loaded activated carbon is used as the third electrode, and the standard saturated calomel electrode is used as the reference electrode to form a three-dimensional fixed-bed reactor for electrocatalytic degradation of lignin, combined with continuous electrocatalytic degradation The integrated process of separation with solvent extraction enables the degradation products to be separated from the lignin alkali solution quickly. The present invention combines the integrated process of continuous electrocatalytic degradation and solvent extraction separation with electrocatalytic degradation of lignin, which has mild reaction conditions, simple and easy-to-operate process technology, and better development and use of lignin, a by-product of paper mills, to obtain The fine chemical product diisobutyl phthalate has good industrial application value. <pb pnum="1" / >

Description

technical field [0001] The invention relates to providing a method for preparing diisobutyl phthalate by electrocatalytically degrading lignin alkali solution in a fixed-bed reactor, and belongs to the technical field of biomass energy chemical industry. Background technique [0002] Lignin is one of the most potential renewable organic resources on earth, and it mainly exists in woody plants and herbaceous plants. Lignin is a kind of aromatic polymer with complex structure in plant cells, mainly containing three basic structural units (guaiacyl propyl, syringyl propyl and p-hydroxyphenyl propyl), S.R.Collinson, W.Thielemans et al. (Coordination Chemistry Reviews, 2010, 254:1854-1870) deduced the chemical structural formula of lignin based on rapid pyrolysis as shown in the following formula. [0003] [0004] my country's forest resources are not very rich, but the annual output of crop straw is huge, about 500-600 million tons. As a by-product of the paper industry, t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C25B3/02B01D11/04C07C69/80C25B3/23
CPCY02P20/10
Inventor 黎钢彭莹杨芳张松梅
Owner HEBEI UNIV OF TECH
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