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Preparation method of 2-(2-hydroxyethoxy) phenol

A technology of hydroxyethoxyl and phenol, which is applied in the field of preparation of 2-phenol, can solve problems such as difficult long-distance transportation, and achieve the effects of suppressing side reactions, high yield, and high activity

Active Publication Date: 2022-04-19
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, considering the flammable and explosive characteristics of ethylene oxide, it is not easy to transport long distances, and has strong regional characteristics, this process has great limitations.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Dissolve 0.6g of praseodymium nitrate hexahydrate in 20g of water, add 20g of SAPO-11 molecular sieve, stir at room temperature for 6 hours, dry at 110°C for 12h, and then calcinate at 400°C for 4h in an air atmosphere to obtain catalyst A.

[0026] Put 10g of catalyst A in a fixed bed, under N 2 Pretreatment at 300°C for 2 h under atmosphere. Ethylene glycol and catechol are mixed according to a molar ratio of 6:1 to form a raw material liquid, and the raw material liquid is passed into a fixed bed so that the liquid hourly space velocity of catechol is 0.5h -1 , The reaction was carried out under the condition of normal pressure 210°C. After the reaction was stabilized, the product was analyzed by gas chromatography, and the specific results are shown in Table 1 below.

Embodiment 2

[0028] Dissolve 1.0g of praseodymium nitrate hexahydrate in 20g of water, add 20g of SAPO-34 molecular sieve, stir at room temperature for 8 hours, dry at 120°C for 9h, and then calcinate at 450°C for 8h to obtain catalyst B.

[0029] Put 10g catalyst B in the fixed bed, under N 2 Pretreatment at 250°C for 6h under atmosphere. Ethylene glycol and catechol are mixed into a raw material solution according to a molar ratio of 8:1, and the raw material solution is passed into a fixed bed so that the liquid hourly space velocity of catechol is 1.2h -1 , The reaction was carried out under the condition of normal pressure 270°C. After the reaction was stable, the product was analyzed by gas chromatography.

Embodiment 3

[0031] Dissolve 1.8g of praseodymium chloride in 20g of water, add 20g of SAPO-11 molecular sieve, stir at room temperature for 10 hours, dry at 130°C for 8h, and then calcinate at 500°C for 10h to obtain catalyst C.

[0032] Put 10g of catalyst C in a fixed bed, under N 2 Pretreatment at 200°C for 7h under atmosphere. Ethylene glycol and catechol are mixed into a raw material solution according to a molar ratio of 10:1, and the raw material solution is passed into a fixed bed so that the liquid hourly space velocity of catechol is 2.0h -1 , The reaction was carried out under the condition of normal pressure 300°C. After the reaction was stable, the product was analyzed by gas chromatography.

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PUM

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Abstract

The invention discloses a preparation method of 2-(2-hydroxyethoxy) phenol, which is characterized in that catechol and ethylene glycol are used as raw materials, a praseodymium-loaded SAPO molecular sieve is used as a catalyst, and a product can be efficiently obtained. The reaction activity and selectivity are high, long-time continuous operation can be achieved, and stable operation can reach 3000h.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of 2-(2-hydroxyethoxy)phenol. Background technique [0002] 2-(2-hydroxyethoxy)phenol can be used as a drug intermediate, mostly used in the synthesis of doxazosin. The current synthesis processes are mainly divided into three categories: the first is the ethylene carbonate method, in which catechol and ethylene carbonate are dissolved in DMF solution and reacted at 170°C for 2 hours under the catalysis of tetra-n-butylammonium fluoride to obtain product. However, the cost of the catalyst in this method is high and cannot be recycled. The second method is the 2-chloroethanol method. 2-chloroethanol and catechol are added to the mixed solution of potassium hydroxide and 2-methoxyethanol, and reacted for 48 hours at 100°C under a nitrogen atmosphere to obtain 2-(2- hydroxyethoxy) phenol. However, since 2-chloroethanol will produce high...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/09C07C43/23B01J29/85
CPCC07C41/09B01J29/85B01J2229/18C07C43/23Y02P20/52
Inventor 范立耸王锐刘振峰初晓东丁大康边新建王漭刘释水李俊平曹文健马德森冯民昌温道宏郑京涛曹鹤
Owner WANHUA CHEM GRP CO LTD
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