Catalyst for preparing 1,2-glycol by epoxy compound through hydration as well as preparation method and application thereof

A technology of epoxy compounds and catalysts, which is applied in the direction of physical/chemical process catalysts, hydrolysis preparation, molecular sieve catalysts, etc., can solve the problems of high energy consumption, high water ratio, etc., and achieve the effect of low cost, simple preparation process and strong acidity

Inactive Publication Date: 2014-07-16
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The invention can solve the problems of high water ratio, high energy consumption and environmental pollution in the traditional diol preparation process. The catalyst has strong acidity and excellent stability. In the reaction of direct hydration of epoxy compound to prepare diol, it can be used at close to room temperature (40°C) and a low water ratio (for example, the molar ratio of water to epoxy compound is 2) can be catalyzed to achieve excellent catalytic activity and diol selectivity

Method used

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  • Catalyst for preparing 1,2-glycol by epoxy compound through hydration as well as preparation method and application thereof
  • Catalyst for preparing 1,2-glycol by epoxy compound through hydration as well as preparation method and application thereof
  • Catalyst for preparing 1,2-glycol by epoxy compound through hydration as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The preparation process of the 4%Sn-Beta catalyst used in the present embodiment comprises the following steps:

[0026] 1) A certain amount of Beta molecular sieve raw powder (SiO 2 / A 2 o 3 =25) mixed with concentrated nitric acid, concentrated hydrochloric acid or oxalic acid solution in a three-necked flask, heated to reflux and stirred for 20 h in an oil bath reactor at 100°C. Wherein, the feeding ratio of Beta molecular sieve former powder and acid solution is 1: 20 (g / mL);

[0027] 2) After fully cooling the solid-liquid mixture after reflux and stirring, add deionized water to it to dilute to a certain concentration, and after vacuum filtration, wash the obtained filter cake with a large amount of deionized water to neutrality, and then It is placed in a blast drying oven at 100°C for 12 hours at a constant temperature;

[0028] 3) Weigh a certain amount of solid powder in step 2) and the required amount of dimethyl tin dichloride organic precursor in the gl...

Embodiment 2

[0038] In this example, the acid used to treat the raw powder of molecular sieve is nitric acid. The influence of different periods of nitric acid treatment on the hydration performance of 4% Sn-Beta catalyst on the hydration performance of catalytic epoxy cyclohexane under the treatment temperature of 100°C was investigated. The catalytic performance evaluation is shown in Table 2. :

[0039] Table 2 The influence of nitric acid treatment for different time periods on the process of preparing cyclohexanediol by hydration of epoxycyclohexane

[0040]

[0041] The results of catalytic performance evaluation show that: with the increase of nitric acid treatment time, the conversion rate of epoxycyclohexane and the selectivity of the target product are correspondingly improved. When the acid treatment time reaches 20h, the maximum yield of diol is 83.6%. , continue to prolong the acid treatment time, there is no obvious promotion effect on the reaction effect.

Embodiment 3

[0043] This example investigates the influence of different organometallic precursors on the hydration performance of catalytic cyclohexane, and other reaction conditions are the same as those described in Example 2. The catalytic performance evaluation results are shown in Table 3:

[0044] Table 3 Effects of different organometallic precursors on the process of preparing cyclohexanediol by hydration of epoxycyclohexane

[0045]

[0046] The results of catalytic performance evaluation show that different catalytic active centers show obvious differences in the catalytic performance of the reaction. The 4%Sn-Beta catalyst prepared by tin roasting has the best catalytic activity and also exhibits excellent catalytic selectivity.

[0047] Implementation Column 4:

[0048] The purpose of this example is to investigate the influence of the percentage content of tin on the hydration performance of catalytic cyclohexane, and other reaction conditions are the same as those describ...

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Abstract

The invention relates to a catalyst for preparing a 1,2-glycol by epoxy compound through hydration as well as a preparation method and an application thereof. A beta zeolite molecular sieve is used as a raw material and then is subjected to acid treatment, and active centered metal is introduced through roasting; and the preparation method comprises the steps of mixing the beta zeolite molecular sieve after acid treatment with an organometallic compound precursor according to the proportion, and roasting. The method can solve the problems of high water ratio, high energy consumption and environment pollution caused by a production process in the traditional process; and the catalyst carrier is cheap and easily available, the preparation process of the catalyst is simple and has good stability, and the catalyst has excellent catalytic activity and the good selectivity in the glycol preparation process by the epoxy compound under a mild condition, and can be applied to glycol industrial production through epoxy compound hydration.

Description

technical field [0001] The invention relates to a catalyst for preparing 1,2-diol by hydration of an epoxy compound, a preparation method and application thereof, in particular to a catalyst and an application method for preparing 1,2-diol by direct hydration of an epoxy compound as a raw material. Background technique [0002] As an important organic chemical raw material, 1,2-diol is mainly used in the synthesis of polyester resin, antifreeze, cosmetics, photographic materials, lubricants, pharmaceutical intermediates and various fine chemicals. In industry, the direct catalytic hydration of epoxy compounds to prepare 1,2-diols is one of the most promising routes. Therefore, in recent years, the development of efficient water-resistant catalysts has always been a hot spot in this research direction, and it is also a difficult problem to be overcome by many scientific research institutions and enterprises at home and abroad. [0003] In recent decades, a series of catalyst...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/70C07C29/10C07C33/26C07C31/42C07C35/14C07C31/20
Inventor 关乃佳唐波李兰冬武光军戴卫理
Owner NANKAI UNIV
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