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Process for preparing diisobutyl phthalate by electro-catalytic degradation of lignin in fixed bed reactor

A technology of diisobutyl phthalate and fixed bed reactor, which is applied in chemical industry, electrolysis process, electrolysis components, etc., can solve the problems of industrial production cost increase, long reaction cycle, expensive catalyst, etc., and achieve good results The effect of industrial application value, mild reaction conditions, and easy operation of process technology

Active Publication Date: 2013-12-25
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Process for preparing diisobutyl phthalate by electro-catalytic degradation of lignin in fixed bed reactor
  • Process for preparing diisobutyl phthalate by electro-catalytic degradation of lignin in fixed bed reactor
  • Process for preparing diisobutyl phthalate by electro-catalytic degradation of lignin in fixed bed reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

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

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

[0042] (4) Turn on the circulating pump 4 to inject 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 for extraction and layering , the lower liquid, that is, the extracted reaction solution, flows into the sto...

Embodiment 2～8

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

[0051] The impact of table 1 current density on the concentration of diisobutyl phthalate

[0052] project Current density (mA / cm 2 ) DIBP concentration (mg / L) Example 2 10 0.9 Example 3 15 4.8 Example 4 20 0.27 Example 5 25 5.7 Example 6 30 1.15 Example 7 35 1.2 Example 8 40 4.35

Embodiment 9～11

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

[0055] The impact of table 2pH value on the concentration of diisobutyl phthalate

[0056] project pH value DIBP concentration (mg / L) Example 9 11 5.55 Example 10 12 1.65 Example 11 13 5.7

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Abstract

The invention relates to a method for preparing diisobutyl phthalate by electrochemically degrading lignin. According to the method, a three-dimensional fixed bed reactor is formed by using Ti / SnO2-Sb2O3-Fe(NO3)3 / PbO2 as a working electrode, a copper mesh electrode as an auxiliary electrode, filled nutshell activated carbon as a third electrode and a standard saturated calomel electrode as a reference electrode. Electro-catalytic degradation of the lignin is combined with an integrated process for continuous electro-catalytic degradation and solvent extraction separation, so that degraded products can be separated from a lignin alkali solution rapidly. By combining the electro-catalytic degradation of the lignin with the integrated process for continuous electro-catalytic degradation and solvent extraction separation, reaction conditions are mild; process technology is simple and can be operated easily; byproduct-lignin of a paper-making factory is used relatively well; and a fine chemical product-diisobutyl phthalate is obtained; and the method has relatively good industrial application values.

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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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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