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Block polyether compound modified lignin and preparation method and uses thereof

A technology of block polyether and lignin, applied in the directions of lignin derivatives, chemical instruments and methods, chemical/physical processes, etc., can solve problems such as difficulties, and achieve the effects of improving utilization rate, reducing consumption and reducing pollution

Inactive Publication Date: 2008-04-09
JIANGSU QIANGLIN BIO ENERGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The lignin polymer monomer obtained by this invention has olefins or substituted olefins, and it is still very difficult to apply to polymer materials.

Method used

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  • Block polyether compound modified lignin and preparation method and uses thereof
  • Block polyether compound modified lignin and preparation method and uses thereof
  • Block polyether compound modified lignin and preparation method and uses thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Separation and purification of lignin:

[0028] Take 100 parts by mass of crude alkali lignin, make it into a 10% mass fraction aqueous solution, adjust the pH of the solution to 12 with 10% mass fraction of NaOH, until all the lignin is dissolved, and centrifuge at 6000r / rain for 5min to remove insoluble impurities Afterwards, the solution was heated to 60°C, adjusted to pH 3 with 20% mass fraction of sulfuric acid, left to stand, the supernatant was removed, the precipitate was washed with water, centrifuged at 6000r / rain for 10min, the precipitate was washed to neutral, and the precipitate was washed at 105 After drying at ℃, it was ground into powder, and 70 parts by mass of purified lignin was obtained by weighing, which was sealed and stored for future use. The chemical composition of the obtained purified lignin is as follows: the mass fraction of lignin is 95%, the mass fraction of total sugar is 2.70%, the mass fraction of ash is 1.70%, and the molar concentrat...

Embodiment 2

[0030] Purification of lignosulfonate

[0031] Take 100 parts by mass of crude lignosulfonate, make it into an aqueous solution with a mass fraction of 50%, add 8 mass fractions of sulfur, stir and react at 230°C for 30min, stop heating, quickly cool the reactant to room temperature, add 30 mass fractions of sulfur Dilute with water, add 2 mass fractions of 10% sulfuric acid, acidify for 10 minutes, add 50 mass fractions of ethyl acetate for extraction, stop stirring, let stand to separate layers, take the upper organic phase, evaporate the ethyl acetate solvent, and extract the remaining solid The product was vacuum-dried at room temperature 1KPa for 10 hr, the dried purified lignin was ground into powder, and 80 parts by mass of purified lignin were obtained by weighing, which was sealed and stored for future use. The chemical composition of the obtained purified lignin is as follows: the mass fraction of lignin is 98%, the mass fraction of ash is 1.70%, and the mass molar c...

Embodiment 3

[0033] The preparation method of block polyether compound modified lignin:

[0034] A. Before adding raw materials, the pressure-resistant reactor is evacuated to a vacuum degree of 2-4KPa, filled with nitrogen to normal pressure, and repeated 2-3 times to remove the oxygen in the pressure-resistant reactor;

[0035] B. Take 100 parts by mass of purified lignin, 0.5 to 3 parts by mass of alkali catalyst, and 30 to 80 parts by mass of aromatic hydrocarbon solvent, and put them into a pressure-resistant reactor; after feeding, feed nitrogen protection, seal the pressure-resistant reactor and stir, and heat up To 90-120°C, when the reaction pressure is 0.3-1.0MPa, divide 30-80 mass parts of ethylene oxide and 30-80 mass parts of propylene oxide into 4-8 groups;

[0036] C. After passing in one group of ethylene oxide each time and reacting for 30-60 minutes, then passing in one group of propylene oxide for 30-60 minutes;

[0037] D. Repeat step C until all ethylene oxide and pro...

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Abstract

The invention discloses a block polyether compound modified lignin and a preparation method, which includes the following steps: a pressure-resistant reactor is firstly carried out the vacuum pumping, the nitrogen is added to the normal pressure, the oxygen is removed, after that, 100 weight parts of the purified lignin, 0.1 to 5 weight parts of base catalyst, and 20 to 100 weight parts of aromatics solvent are taken; the nitrogen is introduced for protection after the feeding, the pressure-resistant reactor is confined and stirred, 10 to 100 weight parts of ethylene oxide and propylene oxide are divided into 2 to 10 equal parts at 80 to 150 DEG C and 0.3 to 1.0 MPa, one equal part of ethylene oxide is introduced during each time of reaction for reaction for 30 to 60 minutes, one equal part of propylene oxide is then introduced for reaction for 30 to 60 minutes, after that, one equal part of ethylene oxide is introduced for reaction, the reaction is stopped after 2 to 10 times of such cyclic reactions, the heating is also stopped, and the mixture is cooled down to the room temperature, then the stirring is stopped, the nitrogen is introduced to enable the pressure-resistant reactor to achieve the normal temperature, finally the product is obtained by removing the distillation fractions with the low boiling points by vacuum distillation. The product can be used as a surfactant and can also be applied to the manufacture of rigid polyurethane foam materials.

Description

technical field [0001] The invention belongs to the field of lignin modification, and in particular relates to a lignin modified polymer and its preparation method and application. Background technique [0002] Lignin widely exists in seed plants, and the amount in nature is very large. Only about 6% of lignin in my country is utilized. As a by-product of wood hydrolysis industry and paper industry, lignin has become one of the main sources of pollution in the paper industry because it is not fully utilized, not only causing serious environmental pollution, but also causing a major waste of resources. Lignin is mainly composed of three elements: carbon, hydrogen, and oxygen. It is generally recognized that lignin is a cross-linked natural phenolic polymer compound formed by phenylpropyl (C9) units connected by C-O bonds or C-C bonds. Because it contains a large number of phenolic and alcoholic hydroxyl groups, the general formula is often recorded as R-OH. The pulping indu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07G1/00B01F17/50C08G65/00C08H7/00C09K23/50
Inventor 周永红刘欣刘红军胡立红张猛
Owner JIANGSU QIANGLIN BIO ENERGY
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