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Method for preparation of 2, 6-dihydroxytoluene

A technology of dihydroxytoluene and methanol, which is applied in the field of preparation of 2,6-dihydroxytoluene, can solve problems such as complex production process, many reaction steps, and difficult production operation, and achieve simple operation, improve product quality, and reduce environmental pollution. pollution effect

Active Publication Date: 2017-04-05
ZHEJIANG DINGLONG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0022] There are many reaction steps in this route, the total yield is low, the production process is relatively complicated, and it is difficult to implement large-scale production operations

Method used

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  • Method for preparation of 2, 6-dihydroxytoluene
  • Method for preparation of 2, 6-dihydroxytoluene
  • Method for preparation of 2, 6-dihydroxytoluene

Examples

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preparation example Construction

[0047] (a) Preparation of collagen fiber loaded metal material:

[0048] Take 15g of skin collagen fiber and place it in a three-necked flask and stir evenly, adjust the pH to 1.8-2.0 with a mixture of formic acid and sulfuric acid, place it in a constant temperature water bath and stir for 2h at a stirring speed of 180r / min, and add 30.0g of Zr (SO 4 ) 2 And a certain amount of nitrate solution, stirring at room temperature for 4h, rotating speed 350r / min, with saturated NaHCO 3 The solution is slowly adjusted to pH 4.0-4.1, heated to 45°C and stirred for 8 hours, filtered after the reaction, washed with water several times, and ventilated and dried at room temperature to obtain metal-laden collagen fibers;

[0049] (b)SO 4 2- / ZrO 2 -M x O y Preparation of solid acid:

[0050] The product prepared above was put into a muffle furnace for temperature-programmed heat treatment, and the temperature was increased to 400, 500, 600, 700, 800 ℃ at a heating rate of 10 ℃ / min, and the fibrou...

Embodiment 1

[0052] The synthetic route of the present invention is as follows:

[0053]

[0054] This reaction adopts a fixed bed reaction mode, and 1.0g of self-made solid acid SO 4 2- / ZrO 2- Ni 2 O 3 The catalyst is put into a cylindrical stainless steel reaction tube with a length of 100 mm and an inner diameter of 4.4 mm, and the vacant part is filled with inert quartz sand. The reaction adopts the following feeding method. The reaction mixture is continuously pumped into the reaction tube at an appropriate feeding rate through a SURPASS 102S / R-20 peristaltic pump, and the reaction product is continuously discharged after condensation, and samples are collected regularly. The collection time is 5.0min, the reaction temperature was controlled by an electric heating temperature control device during the reaction. The specific reaction process is as follows: Mix 220g methanol and 22.0g resorcinol uniformly, and use a peristaltic pump at a methanol space velocity of 0.50h -1 The reaction te...

Embodiment 2

[0056] This reaction adopts a fixed bed reaction mode, and 1.0g of self-made solid acid SO 4 2- / ZrO 2 -La 2 O 3 The catalyst is put into a cylindrical stainless steel reaction tube with a length of 100 mm and an inner diameter of 4.4 mm, and the vacant part is filled with inert quartz sand. The reaction adopts the following feeding method. The reaction mixture is continuously pumped into the reaction tube at an appropriate feeding rate through a SURPASS 102S / R-20 peristaltic pump, and the reaction product is continuously discharged after condensation, and samples are collected regularly. The collection time is 5.0min, the reaction temperature was controlled by an electric heating temperature control device during the reaction. The reaction process is as follows: mix 220g methanol and 22.0g resorcinol uniformly, and use a peristaltic pump at a methanol space velocity of 0.50h -1 The reaction temperature was 350℃, and the reaction product was collected and sampled after condensat...

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Abstract

The invention relates to a method for preparation of 2, 6-dihydroxytoluene. The method comprises (1) methylation reaction: carrying out a methylation reaction process on resorcinol as a raw material, a certain amount of methanol as a solvent and a methylation reagent in the presence of a solid acid as a catalyst in a fixed bed reaction device, (2) distillation: carrying out reduced pressure distillation on the reaction liquid, recovering the solvent and collecting a crude product of 2, 6-dihydroxytoluene, and (3) purification: carrying out recrystallization on the crude product of 2, 6-dihydroxytoluene to obtain a refined product of 2, 6-dihydroxytoluene. The method improves the quality of the product, reduces environmental pollution, reduces a cost, is simple in operation, realizes clean and eco-friendly product production and is suitable for mass production.

Description

Technical field [0001] The invention belongs to the technical field of chemical material preparation, and specifically relates to a method for preparing 2,6-dihydroxytoluene. Background technique [0002] 2,6-Dihydroxytoluene has many important physical and chemical properties. It has very important applications in the chemical industry and is an indispensable chemical raw material. It is used in synthetic resins, dyeing, pigments, dyes, hair dyes, medicine, Pesticides, agrochemicals, photosensitive materials, explosives and other fields, and because of its good disinfection and sterilization functions, in recent years have also been widely used in shampoos, skin care products and other products. [0003] In the 1980s, people began to study the synthesis method of 2,6-dihydroxytoluene. So far, the literature has reported several synthesis methods of 2,6-dihydroxytoluene, mainly: [0004] 1. Using glutaric acid as the starting material, it reacts with acetyl chloride under the cataly...

Claims

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Application Information

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IPC IPC(8): C07C37/16C07C39/08C07C37/70
CPCC07C37/16C07C37/70C07C39/08
Inventor 潘志军许惠钢金宁人叶炯英刘峰顾锋雷张学
Owner ZHEJIANG DINGLONG TECH
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