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Preparation method of hydroxymethylated lignin

A technology of hydroxymethylation and lignin, which is applied in the field of preparation of hydroxymethylated lignin, can solve the limitation of large-scale industrial production of hydroxymethylated lignin and the improvement of yield, generation of a large amount of waste liquid, complicated treatment, etc. problems, to save the steps of product post-processing, reduce the amount of waste liquid, and achieve the effect of easy operation

Active Publication Date: 2019-03-29
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

[0004] In order to solve the above-mentioned problems that the post-treatment of the hydroxymethylation process of lignin is complicated, a large amount of waste liquid is produced in the production process, and the large-scale industrial production of hydroxymethylated lignin and the improvement of the yield are limited, the present invention provides a water Method for preparing hydroxymethylated lignin by thermal method

Method used

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  • Preparation method of hydroxymethylated lignin
  • Preparation method of hydroxymethylated lignin
  • Preparation method of hydroxymethylated lignin

Examples

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Effect test

Embodiment 1

[0025] Add 12g of wheatgrass lignin, 0.12g of NaOH solid, and 3.0g of 37% formaldehyde solution into the hydrothermal reaction kettle, stir evenly, seal the reaction kettle, then raise the temperature to 80°C, keep it warm for 60min, cool to room temperature, and wash the product , suction filtration, and drying to obtain hydroxymethylated lignin. The yield of hydroxymethylated lignin obtained in this example was 68%.

Embodiment 2

[0027] Add 12g of wheatgrass lignin, 0.42g of NaOH solid, and 3.0g of 37% formaldehyde solution into the hydrothermal reaction kettle, stir evenly, seal the reaction kettle, then raise the temperature to 80°C, keep it warm for 120min, cool to room temperature, and wash the product , suction filtration, and drying to obtain hydroxymethylated lignin. The yield of hydroxymethylated lignin obtained in this example was 70%.

Embodiment 3

[0029] Add 12g of wheatgrass lignin, 0.42g of NaOH solid, and 3.0g of 37% formaldehyde solution into the lining of the hydrothermal reaction kettle, stir evenly, seal the reaction kettle, then raise the temperature to 100°C, keep the temperature for 120min, cool to room temperature, and test the product Washing, suction filtration, and drying to obtain hydroxymethylated lignin. The yield of hydroxymethylated lignin obtained in this example was 86%.

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Abstract

The invention discloses a preparation method of hydroxymethylated lignin. The method comprises the following steps: adding certain amounts of lignin, a formaldehyde solution and a solid base into a hydrothermal reactor, performing uniform stirring, sealing the reactor, heating the reactor to a specific temperature, carrying out a reaction for a period of time, cooling the obtained reaction productto room temperature, and carrying out washing, suction filtration and drying on the product to obtain the hydroxymethylated lignin. The method for preparing the hydroxymethylated lignin by a hydrothermal process has the advantages of easiness in operation, simplicity in post-treatment, no acidification precipitation step, facilitation of further high-value utilization of the hydroxymethylated lignin, and good application prospect.

Description

technical field [0001] The invention relates to the technical field of organic chemical industry, in particular to a method for preparing hydroxymethylated lignin. Background technique [0002] Lignin (Lig) is a natural polymer material with a three-dimensional network structure. Its molecular structure is mainly composed of three types: Composed of phenylpropane structural units, there are a large number of benzene ring structures in the structure, and it contains polar groups such as hydroxyl, carbonyl, and carboxyl, which provide a theoretical basis for its further functionalization. However, in the actual functionalization process, lignin has a large steric hindrance and fewer reactive sites, resulting in low reactivity and difficulty in effective functionalization. In order to improve the reactivity of lignin, lignin needs to be modified. Modification methods mainly include hydroxymethylation, phenolization and demethylation, among which hydroxymethylation is one of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08H7/00
CPCC08H6/00
Inventor 李锦春宗旭宋艳张鑫邹国享赵彩霞
Owner CHINA PETROLEUM & CHEM CORP
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