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Method for preparing 2,6-ditert-butyl-4-methylphenol by lignin pyrolysis

A technology of di-tert-butyl and methyl phenol, which is applied in the fields of chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve problems such as relatively expensive prices, achieve simple production process, improve utilization efficiency, and save costs Effect

Active Publication Date: 2019-01-04
BEIJING UNION UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These synthetic methods all use chemical products as raw materials, and the price is relatively expensive.

Method used

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  • Method for preparing 2,6-ditert-butyl-4-methylphenol by lignin pyrolysis
  • Method for preparing 2,6-ditert-butyl-4-methylphenol by lignin pyrolysis
  • Method for preparing 2,6-ditert-butyl-4-methylphenol by lignin pyrolysis

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preparation example Construction

[0030] 1) Preparation of molecular sieves doped with metal ions: 10ml of phosphoric acid and 10g of alumina were placed in 90g of water, and 2.4g of silicon dioxide and salts of different metal ions (titanium, iron, vanadium, copper, zinc, Nickel, cobalt and bismuth ion) 1 to 5 grams, the coordination reagent sodium edetate of 4.2 grams (also can use other polynitrogen, oxygen coordination reagent) and 14 grams of n-propylamine, after mixing and stirring for 12 hours, High-pressure reaction for 48 hours, washing, suction filtration, drying for 24 hours, then activation in a muffle furnace at 350°C for 3 hours, cooling, and grinding.

[0031] Among them, the salt of metal ions is soluble chloride salt, nitrate or sulfate of titanium, iron, vanadium, copper, zinc, cobalt, bismuth or nickel, such as: titanium sulfate, ferric chloride, vanadium trichloride, sulfuric acid Copper, zinc chloride, cobalt chloride and bismuth nitrate, nickel chloride.

[0032] Wherein, the complexing ...

Embodiment 1

[0036] A method for catalytic thermal cracking of lignin, comprising the steps of:

[0037]1) Preparation of molecular sieve doped with iron ions: 10ml of phosphoric acid and 10g of alumina were placed in 90g of water, after dissolving, 2.4g of silicon dioxide and 1g of ferric chloride were added under constant stirring, and 4.2g of ethylenediaminetetra Sodium acetate and 14 grams of n-propylamine, mixed and stirred for 12 hours, reacted under high pressure for 48 hours, washed, suction filtered, dried for 24 hours, then activated in a muffle furnace at 350°C for 3 hours, cooled, and ground to obtain a doped iron ion with a weight content of about 0.25% SAPO-34 molecular sieves.

[0038] 2) Cracking reaction of lignin: Weigh one gram of molecular sieve catalyst and one gram of lignin in a weight ratio of 1:1, mix them evenly, put them into a quartz reactor, install the reaction device, and pass inert gas nitrogen for 30 minutes to remove oxygen. Heat to 350°C and react for 10...

Embodiment 2

[0040] A method for catalytic thermal cracking of lignin, comprising the steps of:

[0041] 1) Preparation of molecular sieve doped with copper ions: 10ml of phosphoric acid and 10g of alumina were placed in 90g of water, after dissolving, 2.4g of silicon dioxide, 2g of copper sulfate and 4.2g of ethylenediaminetetraacetic acid were added under constant stirring Sodium and 14 grams of n-propylamine, mixed and stirred for 12 hours, reacted under high pressure for 48 hours, washed, suction filtered, dried for 24 hours, then activated in a muffle furnace at 350°C for 3 hours, cooled, and ground to obtain a doped copper ion weight content of about 0.25 % SAPO-34 molecular sieve.

[0042] 2) Cracking reaction of lignin: weigh 3 grams of molecular sieve catalyst and 1 gram of lignin in a weight ratio of 3:1, mix them evenly, put them in a quartz reactor, install the reaction device, and pass inert gas nitrogen for 30 minutes to remove oxygen , heated to 350°C and reacted for 10 min...

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Abstract

The invention relates to a method for preparing 2,6-ditert-butyl-4-methylphenol by lignin pyrolysis. The method comprises the following steps: mixing a metal-ion-doped molecular sieve catalyst and lignin, placing in a quartz reactor, feeding an inert gas for deoxidizing, heating and performing a pyrolytic reaction, enabling the lignin to be pyrolyzed, cooling and collecting a reaction production,to obtain a liquid mixture with fragrance, through column chromatography separation, freezing and crystallizing, to obtain a white crystal. The method is capable of, through controlling types of metalions in the catalyst and content in the catalyst, in a relative low temperature, using the cheap lignin as a raw material, high-selectively producing an antioxidant of the 2,6-ditert-butyl-4-methylphenol, and through processes of the simple column chromatography separation and the crystallization and the like later, acquiring a product with high purity. The method is simple in production process,and capable of improving utilization efficiency of industrial papermaking wastes and the lignocellulose raw material, saving cost, and suitable for large-scale production.

Description

technical field [0001] The invention relates to a method for preparing 2,6-di-tert-butyl-4-methylphenol by pyrolysis of lignin, which specifically relates to the preparation of antioxidant 2,6-di-tert-butyl-4 by thermal catalytic cracking reaction of lignin -methylphenol. Background technique [0002] 2,6-di-tert-butyl-4-methylphenol (abbreviation: BHT), its structure is shown in the general formula I, the English name is 2,6-Di-tert-butyl-4-methyl-phenol, commonly known as anti-aging Antioxidant BHT, Antioxidant BHT, Antioxidant 264. Soluble in common organic solvents. BHT has the advantages of strong antioxidant capacity, good heat resistance and stability, no specific odor, and no color reaction with metal ions, so it is used as a main food additive and antioxidant at home and abroad. BHT is widely used as an antioxidant in edible oils, cosmetics, pharmaceuticals, rubber and petroleum products, and can effectively prevent organic compounds and polymeric materials from ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/54C07C39/06
CPCC07C37/004C07C37/54C07C39/06
Inventor 刘白宁蒋丹程艳铃周考文李晓宇王欣竹张佳音崔天宇
Owner BEIJING UNION UNIVERSITY