Preparation method of alkali lignin-based dye dispersant

A dye dispersant and alkali lignin technology, applied in the field of preparation of alkali lignin-based dye dispersants, can solve the problems of low dispersion grade, poor high temperature stability, strong fiber contamination, etc., and achieve high dispersion grade and high temperature stability. Good, low fiber contamination effect

Pending Publication Date: 2021-11-16
QILU UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Low dispersion level, poor high temperature stability, and strong staining on fibers are disadvantages, so domestic lignin dispersants are mostly used as filling dispersants

Method used

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  • Preparation method of alkali lignin-based dye dispersant
  • Preparation method of alkali lignin-based dye dispersant
  • Preparation method of alkali lignin-based dye dispersant

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preparation example Construction

[0016] A preparation method of an alkali lignin-based dye dispersant, using alkali lignin in the pulp and paper industry as a raw material, comprising the following steps:

[0017] Using alkali lignin in the pulp and paper industry as raw material, purify alkali lignin by using organic solvent and acid precipitation method, and use a new alkylation system 1,6-dibromohexane / dimethylformamide to regulate alkali lignin molecules , to obtain molecularly regulated alkali lignin (CAL). Separation of medium and high molecular weight (3000-13000g / mol) alkali lignin (CAL) by ultrafiltration h ). at cal h CAL h :K 2 CO 3 =5:3 (w / w) Add potassium carbonate solid and place it in a three-necked flask, according to CAL h : DMF = 1: 5 (w: v) after mixing, put it in a water bath and heat it until it reaches 70-100 ° C, according to CAL h : 1,4-butane sultone=1:0.05~0.35 Add 1,4-butane sultone, and make the mixture sulfonate under stirring for 1~4h respectively. Pour the mixture into a...

Embodiment 1

[0032] Embodiment 1: The preparation of alkali lignin-based dye dispersant is realized through the following steps.

[0033] (1) Organic solvent purification of crude alkali lignin: add acidic dioxane aqueous solution (dioxane / water=9:1, v:v, pH=2). The mixture was stirred at 87°C for 2 hours, then centrifuged to remove the precipitate. The supernatant to which sodium bicarbonate was added was kept stirring for 3 hours to neutralize the acid in the solution. After centrifuging again to remove the precipitate, the supernatant was rotovapped under vacuum at 55 °C to remove and recover dioxane.

[0034] (2) Separation and purification of alkali lignin by acid precipitation: the supernatant after vacuum rotary evaporation was added to 2000 mL of hydrochloric acid solution (pH=2), and then centrifuged to obtain a precipitate. The precipitate was freeze-dried to obtain purified alkali lignin (PAL) as a solid powder.

[0035] (3) Alkylation of PAL: Dissolve PAL in dimethylformami...

Embodiment 2

[0042] Embodiment 2: The preparation of alkali lignin-based dye dispersant is realized through the following steps.

[0043] (1) Organic solvent purification of crude alkali lignin: add acidic dioxane aqueous solution (dioxane / water=9:1, v:v, pH=2). The mixture was stirred at 87°C for 2 hours, then centrifuged to remove the precipitate. The supernatant to which sodium bicarbonate was added was kept stirring for 3 hours to neutralize the acid in the solution. After centrifuging again to remove the precipitate, the supernatant was rotovapped under vacuum at 55 °C to remove and recover dioxane.

[0044] (2) Separation and purification of alkali lignin by acid precipitation: the supernatant after vacuum rotary evaporation was added to 2000 mL of hydrochloric acid solution (pH=2), and then centrifuged to obtain a precipitate. The precipitate was freeze-dried to obtain purified alkali lignin (PAL) as a solid powder.

[0045] (3) Alkylation of PAL: Dissolve PAL in dimethylformami...

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Abstract

The invention belongs to the field of alkali lignin utilization in pulping and papermaking industry, and relates to a preparation method of an alkali lignin-based dye dispersant. The method comprises the following steps: purifying alkali lignin, and carrying out molecular weight regulation and ultrafiltration in a 1, 6-dibromohexane / dimethylformamide system to obtain high molecular weight alkali lignin; and sulfonating the high molecular weight alkali lignin by using 1, 4-butanesultone to obtain the alkali lignin-based dye dispersant. The alkali lignin-based dye dispersant is prepared by taking alkali lignin in the pulping and papermaking industry as a raw material, firstly regulating and controlling the alkali lignin by adopting a novel alkylation system of 1, 6-dibromohexane / dimethylformamide, and then sulfonating the regulated and controlled alkali lignin by using 1, 4-butanesultone. The prepared alkali lignin-based dye dispersant is high in dispersion grade, high in high-temperature stability and low in contamination to fibers, and all indexes reach or exceed the indexes of first-grade sodium lignin sulfonate dispersants in HGT 3507-2008.

Description

technical field [0001] The invention belongs to the field of alkali lignin utilization in the pulp and paper industry, and in particular relates to a preparation method of an alkali lignin-based dye dispersant. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] Lignin is the largest natural source of aromatic compounds, accounting for 15-40wt% of wood, and is the second largest biomass resource in the plant kingdom after cellulose. Currently only about 2% of lignin is used to produce high value-added products, and most of it is only used as cheap fuel. Lignin is mainly derived from the pulp and paper industry. As a by-product of pulping, the world's annual output is about 5...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B67/46
CPCC09B67/009
Inventor 田中建吉兴香姜潇张凤山吕高金马浩
Owner QILU UNIV OF TECH
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