Method for extracting lignin sulfonate using waste liquid from boiling canapina fiber or paper making

A technology of lignosulfonate and papermaking waste liquid, which is applied in the directions of lignin derivatives, chemical instruments and methods, processing wastewater treatment, etc. The quality needs to be improved, the energy consumption of evaporation and concentration is large, etc., to achieve the effect of complete acid precipitation sulfonation reaction, full extraction and utilization, and low production cost

Inactive Publication Date: 2007-11-14
武汉海德天物新材料有限公司
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Problems solved by technology

However, this method cannot remove impurities or other residues in pulping black liquor; its evaporation an

Method used

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Experimental program
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Effect test

preparation example Construction

[0020] B. Preparation of lignosulfonate solution:

[0021] Take 25-50 parts by weight of the lignin concentrate, place it in the reactor, turn on the stirring, add 5-15 parts by weight of 10% sulfuric acid, react at 60-80°C for 2 to 4 hours, and then add 10 sulfite ~30 parts by weight, 2~6 parts by weight of ferric chloride or copper sulfate, react at 80~100℃ for 3~5 hours, adjust the PH value of 7~8, and obtain lignin sulfonic acid with 20~40% solid content Salt solution. The sulfuric acid can be waste sulfuric acid from chemical plants.

[0022] In step A, the process of microfiltration or ultrafiltration can use three-layer filter membranes, and the pore diameters of the filter membranes are 50, 30, and 20 microns, respectively. It is also possible to use only one or two layers of filter membrane, the minimum pore size of the filter membrane is 20 microns to ensure that the molecular weight of the lignin intercepted is 8000-100000, and the pressure in the microfiltration proces...

Embodiment 1

[0024] Put the boiling waste liquid of the ramie production plant at a temperature of 40℃ and a pressure of 1.5MPa / cm 2 Under the conditions of, the three-layer filter membrane with pore size of 50, 30, and 20 microns is used for microfiltration. The molecular weight of the lignin retained by the filter membrane is 8000-100000, and a lignin concentrate with a solid content of about 30% is obtained. ;

[0025] Take 30 parts by weight of the lignin concentrate with a solid content of 30%, place it in the reactor, turn on the stirring, add 10 parts by weight of 10% sulfuric acid, react at 70°C for 3 hours, and then add 20 parts by weight of sodium sulfite. 4 parts by weight of ferric chloride, reacted at 90° C. for 4 hours, adjusted the pH value of 7-8 to obtain a lignosulfonate solution with a solid content of 20-40%.

[0026] The concentrated liquid is sent to a drying tower for drying to obtain brown-yellow lignosulfonate powder.

Embodiment 2

[0028] Put the waste liquid from the paper mill at a temperature of 20℃ and a pressure of 1.0MPa / cm 2 Under the conditions of, the two-layer filter membrane with the filter membrane pore size of 30 and 20 microns respectively is used for microfiltration, and the molecular weight of the lignin retained by the filter membrane is 8000-100000 to obtain a lignin concentrate with a solid content of about 40%;

[0029] Take 20 parts by weight of the lignin concentrate with a solid content of 40%, place it in the reactor, turn on the stirring, add 5 parts by weight of 10% sulfuric acid, react at 70°C for 3 hours, and then add 10 parts by weight of sodium sulfite. 2 parts by weight of ferric chloride, reacted at 80°C for 3 hours, adjusted the pH value of 7-8 to obtain a lignosulfonate solution with a solid content of 20-40%.

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Abstract

This invention relates to a method of using boied hemp or papermaking waste liquor to extract lignosulphonate. Firstly boied hemp or papermaking waste liquor proceed microfiltration and hyperfiltration; take lignin concentrated solution 25 to 50 parts by weight, put at reactor; unlock whipper, add 10% sulfuric acid 5 to 15 parts by weight, at 60 to 80 deg take reaction for 2 to 4hours, then add sulfite 10 to 30 parts by weight, ferric chloride or bluestone 2 to 6 parts by weight, at 80 to 100deg take reaction for 3 to 5hours, adjust pH value 7 to 8, gain lignosulphonate solution. The lignosulphonate has many active group, possess good surface activity and hydrophile-lipophile balance, good solubility and dispersibility, higher yield and good quality.

Description

Technical field [0001] The invention relates to a method for extracting polymer compounds, in particular to a method for extracting lignosulfonate by using hemp or papermaking waste liquid. Background technique [0002] There are a large number of usable resources-lignin in the waste liquid discharged from the textile and paper industries in our country, but most of our enterprises have not recycled it. According to data, about 0.3 to 0.5 tons of lignin are discharged for every ton of refined dried hemp or 1 ton of paper produced. According to statistics, tens of millions of tons of alkali lignin are discharged into rivers and lakes in my country's textile and paper industry every year, causing a great waste of lignin resources, while also polluting the environment and destroying the ecological balance. Chinese Patent Publication Number: CN1454069, Publication Date: August 6, 2003, Title of Invention: "Method for Producing Lignosulfonate at Normal Temperature and Pressure" propos...

Claims

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Application Information

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IPC IPC(8): C07G1/00C02F1/44C02F103/28C08H7/00
Inventor 李学平鲁爱国
Owner 武汉海德天物新材料有限公司
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