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Method for preparing nano-sized carbon black by lignin at large scale

A technology of nano-carbon black and lignin, applied in nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, can solve problems such as rising raw material oil prices, complex and time-consuming processes, and compressed profit margins, etc., to achieve Great price advantage, simple and controllable process

Active Publication Date: 2017-03-15
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Moreover, with the consumption of these non-renewable resources, the price of raw oil will continue to rise, further compressing profit margins, which will bring great difficulties to carbon black production enterprises
(2) Environmental pollution and greenhouse gas emissions
However, this method needs to use a large amount of strong acid as a solvent, the process is complicated and time-consuming, which is not conducive to large-scale production of carbon black, and the prepared carbon black particle size is greater than 200nm
There are no literature and patent reports on the large-scale preparation of carbon black particles with a primary particle size of less than 100nm by using lignin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Purification: Disperse 100 g of alkali lignin in 400 g of water, add sodium hydroxide to adjust the pH value of the solution to 12 and stir mechanically. After the alkali lignin is fully dissolved, the cellulose and insoluble impurities in the lignin solution are separated and removed by suction filtration to obtain a purified lignin solution.

[0033] (2) Oxidation: Adjust the pH value of the purified lignin solution to 6.5 with 1% sulfuric acid, then add 16 g of hydrogen peroxide, heat to 55° C. and stir the oxidation reaction for 1 hour to obtain the oxidized lignin solution.

[0034] (3) Pre-reaction: adjust the pH of the oxidized lignin solution to 10 with NaOH, heat up to 65° C., add 25 g of epichlorohydrin, and react for 3 hours to obtain a modified lignin solution.

[0035] (4) Condensation: adjust the pH value of the modified lignin solution to 12 with NaOH, raise the temperature to 90° C., add 20 g of formaldehyde, and perform condensation reaction for 1 h...

Embodiment 2

[0041](1) Purification: Disperse 100 g of alkali lignin in 400 g of water, add sodium hydroxide to adjust the pH value to 12 and stir mechanically. After the alkali lignin is fully dissolved, the cellulose and insoluble impurities in the lignin solution are separated and removed by suction filtration to obtain a purified lignin solution.

[0042] (2) Oxidation: Adjust the pH value of the purified lignin solution to 9 with 1% sulfuric acid, then add 5 g of hydrogen peroxide, heat and stir at 60° C., and oxidize for 30 minutes.

[0043] (3) Pre-reaction: adjust the pH value of the oxidized lignin solution to 9 with NaOH, raise the temperature to 80° C., add 2 g of phenol and 20 g of formaldehyde, and react for 2 hours to obtain a modified lignin solution.

[0044] (4) Condensation: Use NaOH to adjust the pH value of the modified lignin solution to 12, and conduct a condensation reaction at 92°C for 1 hour, then add 5 g of epichlorohydrin, and continue the reaction for 0.5 hours ...

Embodiment 3

[0050] (1) Purification: Disperse 100 g of sodium lignosulfonate in 400 g of water, add sodium hydroxide to adjust the pH to 11 and stir mechanically. After the sodium lignosulfonate is fully dissolved, the cellulose and insoluble impurities in the lignin solution are separated and removed by suction filtration to obtain a purified lignin solution.

[0051] (2) Oxidation: Adjust the pH value of the purified lignin solution to 6.5 with 1% sulfuric acid, then add 5 g of hydrogen peroxide, heat and stir at 55° C., and oxidize for 60 minutes.

[0052] (3) Pre-reaction: Use NaOH to adjust the pH value of the oxidized lignin solution to 12, and raise the temperature to 55° C., add 2 g of resorcinol glycidyl ether and 18 g of formaldehyde, and react for 3 hours to obtain the modified lignin solution. prime solution.

[0053] (4) Condensation: Use NaOH to adjust the pH value of the modified lignin solution to 12, and conduct a condensation reaction at 92°C for 1 hour to obtain a lign...

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Abstract

The invention relates to a method for preparing nano-sized carbon black by lignin at a large scale. The method is characterized by comprising the following steps: purification, oxidization, pre-reaction, condensation, washing, paste preparation and heat treatment. According to the method disclosed by the invention, water serves as a reaction medium, the technological process is simple and controllable, the particle size of a product can be adjusted and controlled by adjusting a high-temperature carbonization technological parameter in the chemical reaction and the heat treatment, and the method is suitable for large-scale industrial production. Additionally, the average particle size of primary particles of the carbon black prepared by the method disclosed by the invention can be 100nm or lower, and the carbon black can be applied to the fields of reinforcement for rubber, plastic filling, and so on.

Description

technical field [0001] The invention relates to a preparation method of nano-carbon black, in particular to a method for large-scale preparation of nano-carbon black by utilizing lignin, and belongs to the technical field of chemical production methods. Background technique [0002] Carbon black has excellent properties such as reinforcement, conductivity, UV protection, antistatic, and dyeing, and is widely used in rubber, plastics, inks, coatings, and other fields. Especially in the rubber industry, compared with other fillers, carbon black has obvious reinforcing effect and cost-effective advantages. Almost all rubber products need to be filled with carbon black, and the amount usually accounts for 20%-50% of the total rubber products. The rubber industry is an indispensable important industry for my country's economy and national defense construction, and the carbon black consumed can account for more than 90% of the total output of carbon black. With the development o...

Claims

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Application Information

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IPC IPC(8): C09C1/50B82Y40/00B82Y30/00
CPCB82Y30/00B82Y40/00C09C1/50
Inventor 蒋灿
Owner WUHAN INSTITUTE OF TECHNOLOGY
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