Preparation method of high-oil-absorption and biodegradable lignin-based microporous molecular sieve

A microporous molecular sieve and biodegradation technology, which is applied in the field of preparation of biodegradable lignin-based microporous molecular sieves with high oil absorption rate, can solve the problem of low primary oil absorption rate, water absorption, oil absorption performance interference, low three-dimensional network chemical cross-linking structure and other problems, to achieve the effect of uncomplicated treatment method, wide application range and simple recovery treatment process

Active Publication Date: 2015-03-25
蒋吉平
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Conventional resin oil-absorbing materials are acrylic resins and olefin resin materials, and their structures are characterized by low three-dimensional network chemical cross-linking structures. There is a problem of competitive adsorption between water and oil in the treatment of oil pollution on the sea surface caused by oil spills from tankers. , resultin

Method used

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  • Preparation method of high-oil-absorption and biodegradable lignin-based microporous molecular sieve
  • Preparation method of high-oil-absorption and biodegradable lignin-based microporous molecular sieve
  • Preparation method of high-oil-absorption and biodegradable lignin-based microporous molecular sieve

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Example Embodiment

[0032] Example 1

[0033] Under the reaction temperature of 90℃, dissolve 1g of lignin in 50g of pyridine / dioxane mixture (pyridine:dioxane=1:10, mass ratio), add dropwise appropriate amount of acetic anhydride reagent (acetic anhydride and The molar ratio of the hydroxyl groups in the lignin is 1:2), and the stirring is continued to cause the hydroxyl groups in the lignin to undergo an acetylation reaction with acetic anhydride. The reaction time is 2h. The product is cooled to room temperature, filtered, washed with water three times, and dried to obtain acetyl lignin. Under the condition of reaction temperature 70℃, dissolve acetyl lignin in pyridine / triethoxychlorosilane mixed solution (pyridine:triethoxychlorosilane=1:5, mass ratio), in which triethoxychlorosilane The molar ratio to the hydroxyl group in acetyl lignin is 1:1. Continue to stir to make the hydroxyl group in the acetyl lignin react with triethoxychlorosilane. The reaction time is 12 hours. After the product ...

Example Embodiment

[0035] Example 2

[0036] Refer to Example 1 to prepare acetyl lignin, and then dissolve the acetyl lignin in a mixture of pyridine / triethoxychlorosilane (pyridine:triethoxychlorosilane=1:10) at a reaction temperature of 70°C. The molar ratio of triethoxychlorosilane to hydroxyl groups in acetyl lignin is 1:1. Continue to stir to make the hydroxyl group in the acetyl lignin react with triethoxychlorosilane, and the reaction time is 10 hours. After the product is cooled to room temperature, filtered, washed with water three times, and dried to obtain silyl acetyl lignin. Add the silyl acetyl lignin to the 4A type microporous molecular sieve suspension (mass concentration 10%) dissolved in N,N-dimethylformamide (DMF) at room temperature, in which the hydroxyl group and silyl acetyl lignin in the molecular sieve The molar ratio of ethoxy groups is 1:1. N 2 Under protection, the temperature is raised to 150℃ and the reaction is refluxed for 36 hours. After the product is cooled to...

Example Embodiment

[0038] Example 3

[0039] Refer to Example 1 to prepare acetyl lignin, and then dissolve the acetyl lignin in a pyridine / triethoxychlorosilane mixed solution (pyridine:triethoxychlorosilane=1:3) at a reaction temperature of 70°C, wherein The molar ratio of triethoxychlorosilane to hydroxyl groups in acetyl lignin is 1:1. Continue to stir to make the hydroxyl group in the acetyl lignin react with triethoxychlorosilane. The reaction time is 12 hours. After the product is cooled to room temperature, filtered, washed with water three times, and dried to obtain silyl acetyl lignin. Add silyl acetyl lignin to a suspension of type 5A microporous molecular sieve (mass concentration 5%) dissolved in xylene at room temperature. The molar ratio of the hydroxyl group in the molecular sieve to the ethoxy group in the silyl acetyl lignin is 1: 1. N 2 Under protection, the temperature is raised to 140℃ and the reaction is refluxed for 24 hours. After the product is cooled to room temperature...

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Abstract

The invention discloses a preparation method of a high-oil-absorption and biodegradable lignin-based microporous molecular sieve. The method can be used for synthesizing a high-oil-absorption and biodegradable lignin-based microporous molecular sieve, and is simple in preparation process. The method comprises the following steps: 1) synthesis of acetyl lignin: dissolving lignin in a mixing liquid of pyridine and an organic solvent, dropwise adding an acetic anhydride reagent so that an acetylation reaction is achieved between the alcoholic hydroxyl group in the lignin and acetic anhydride, so as to obtain the acetyl lignin; 2) synthesis of silyl acetyl lignin: dissolving the acetyl lignin in a mixing liquid of pyridine and triethoxy chlorosilane so that a synthesis reaction is achieved between the phenolic hydroxyl group in the acetyl lignin and triethoxy chlorosilane, so as to obtain the silyl acetyl lignin; and 3) preparing the microporous molecular sieve by virtue of copolymerization: adding the silyl acetyl lignin to a microporous molecular sieve suspension dissolved in the organic solvent for copolymerization, thus obtaining a solid matter which is the high-oil-absorption and biodegradable lignin-based microporous molecular sieve.

Description

technical field [0001] The invention relates to a preparation method of a molecular sieve, in particular to a preparation method of a biodegradable lignin-based microporous molecular sieve with a high oil absorption rate. Background technique [0002] Lignin is a complex multi-ring structure and three-dimensional network polymer organic matter (see the following structural formula, referred to as LIG). There are functional groups such as alcoholic hydroxyl group (a), phenolic hydroxyl group (b) and carboxyl group on the molecule, which is conducive to the modification of polymer structure. . In nature, the reserve of lignin is second only to cellulose, and it is regenerated at a rate of tens of billions of tons every year. The pulp and paper industry separates about 150 million tons of cellulose from plants every year, and at the same time obtains about 50 million tons of lignin by-products, but so far, more than 90% of the lignin is directly discharged into rivers as "blac...

Claims

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Application Information

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IPC IPC(8): C08H7/00C09K3/32
Inventor 顾晓利孙岚刘国振周康姚建峰阚春
Owner 蒋吉平
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