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Method for preparing high value-added phenol products from pulping black liquor

A technology for pulping black liquor with high added value, applied in the field of agricultural and forestry biomass resource utilization and treatment, can solve the problem of limiting the application scope and use value of recycled lignin, poor water solubility and chemical reaction performance, and increasing black liquor treatment. Cost and other issues, to achieve the effect of high-value utilization, increased yield, and reduced processing costs

Active Publication Date: 2017-06-30
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is generally necessary to separate and purify lignin from black liquor, which will increase the cost of black liquor treatment
At the same time, due to the complex molecular structure of lignin and the lack of strong hydrophilic groups, at the same time, there are fewer active sites that can react, resulting in poor water solubility and chemical reaction performance, which further limits the application range and utilization of lignin. use value

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] A method for preparing high value-added phenolic products from pulping black liquor (raw material is eucalyptus), comprising the following steps:

[0039] (1) get 1000ml pulping black liquor and dilute 5 times and adjust pH with sulfuric acid to be 2; Obtain supernatant layer and lignin layer after leaving standstill;

[0040] (2) After discarding the supernatant layer, add sulfonating agent sodium sulfite to the lignin layer solution in step (1), the ratio of sulfonating agent and lignin layer is 12g / 1L; after stirring, the lignin layer solution is transferred to The hydrothermal conversion reaction is carried out in the reaction kettle; the conditions of the hydrothermal conversion reaction are: the reaction temperature is 200°C, and the reaction time is 1h;

[0041] (3) After the reaction is finished, filter the reacted solution, extract the filtrate with chloroform, and evaporate under reduced pressure to obtain high value-added phenolic products.

[0042] The extr...

Embodiment 2

[0045] A method for preparing high value-added phenolic products from pulping black liquor (raw material is poplar), comprising the following steps:

[0046] (1) get 2000ml pulping black liquor and dilute 8 times and adjust pH with sulfuric acid to be 3; Obtain supernatant layer and lignin layer after leaving standstill;

[0047] (2) After discarding the supernatant layer, add sulfonating agent sodium sulfite to the lignin layer solution in step (1), the ratio of sulfonating agent and lignin layer is 18g / 1L; after stirring, the lignin layer solution is transferred to The hydrothermal conversion reaction is carried out in the reaction kettle; the conditions of the hydrothermal conversion reaction are: the reaction temperature is 280°C, and the reaction time is 2h;

[0048] (3) After the reaction is finished, filter the reacted solution, extract the filtrate with ethyl acetate, and evaporate under reduced pressure to obtain high value-added phenolic products.

[0049] The extra...

Embodiment 3

[0052] A method for preparing high value-added phenolic products from pulping black liquor (raw material is bamboo), comprising the following steps:

[0053] (1) get 2000ml pulping black liquor and dilute 10 times and adjust pH with sulfuric acid to be 2; Obtain supernatant layer and lignin layer after leaving standstill;

[0054] (2) After discarding the supernatant layer, add sulfonating agent sodium bisulfite to the lignin layer solution in step (1), the ratio of sulfonating agent and lignin layer is 25g / 1L; The solution is transferred into the reactor for hydrothermal conversion reaction; the conditions of the hydrothermal conversion reaction are: reaction temperature 250°C, reaction time 0.5h;

[0055] (3) After the reaction is finished, the solution after the reaction is filtered, the filtrate is extracted with dichloromethane, and high value-added phenolic products are obtained after evaporation under reduced pressure.

[0056] The extracted solution was qualitatively ...

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Abstract

The invention discloses a method for preparing high value-added phenol products from pulping black liquor. According to the method, the pulping black liquor is directly subjected to hydrothermal conversion after being simply treated, the yield of the phenol products is high, the product selectivity is good and the method has great industrial popularization value. The method comprises steps as follows: (1) the pulping black liquor is diluted by 5-10 times, adjusted with a pH agent until the pH ranges from 2 to 3 and then left to stand, and a supernatant layer and a lignin layer are obtained; (2) a sulfonating agent is added to the lignin layer solution in the step (1) after the supernatant layer is removed and stirred uniformly, and then the lignin layer solution is transferred to a reaction kettle for a hydrothermal conversion reaction; (3) after the reaction ends, a solution obtained after the reaction is filtered, filtrate is extracted with an extracting agent, and the high value-added phenol products are obtained after evaporation under reduced pressure.

Description

technical field [0001] The invention relates to the technical field of utilization and treatment of agricultural and forestry biomass resources, in particular to a method for preparing high value-added phenolic products from pulping black liquor. Background technique [0002] The sewage discharge of the pulp and paper industry accounts for about 10% to 12% of the total sewage discharge in the country. The waste water produced by the paper industry—black liquor—is a serious source of industrial pollution. The treatment of black liquor in pulping and papermaking wastewater is still a major problem in the papermaking industry. Papermaking black liquor contains many chemical substances, and if it is discharged directly, it will cause serious damage to the environment. Therefore, it is of great significance to study the resource utilization of papermaking black liquor. About 1 / 3 of the papermaking black liquor is inorganic, mainly NaOH and SiO 2 etc.; about 2 / 3 are organic matt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D21C11/00
CPCD21C11/00
Inventor 吕高金刘宇刘玉吉兴香杨桂花
Owner QILU UNIV OF TECH
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