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Method for preparing isosorbitol by dehydration of sorbitol

A technology for isosorbide and sorbitol, applied in the field of chemical preparation, can solve the problems of harsh reaction conditions, low yield of isosorbide, etc., and achieve the effects of mild reaction conditions, easy separation, high practicability and economy

Inactive Publication Date: 2018-10-23
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When using solid acid as a catalyst, the reaction conditions for preparing isosorbide from sorbitol dehydration due to insufficient acidity are relatively harsh, and the yield of isosorbide is low. Therefore, improving the acidity of solid acid catalysts has become one of the research focuses
[0005] WO 3 / ZrO 2 and MoO 3 / ZrO 2 Solid superacids have the advantages of strong acidity, difficult loss of active components, good stability, etc., and have become a research hotspot of solid acid catalysts, but WO 3 / ZrO 2 and MoO 3 / ZrO 2 Solid superacid is applied to the field of catalytic reaction of sorbitol dehydration to isosorbide, no patent report

Method used

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  • Method for preparing isosorbitol by dehydration of sorbitol
  • Method for preparing isosorbitol by dehydration of sorbitol
  • Method for preparing isosorbitol by dehydration of sorbitol

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Taking the preparation of H-15%W / Zr-800 solid acid as an example, the catalyst preparation process is described in detail.

[0021] Zr(OH) 4 Precursor preparation

[0022] 50g ZrOCl 2 ·8H 2 O was dissolved in 450ml water, stirred for 30min, 35mL NH 3 ·H 2 Add ZrOCl dropwise at room temperature with O (25-28%) 2 ·8H 2 O aqueous solution, stirring, while adding dropwise, use a pH meter to measure the pH. When the pH meter reads 9.0, stop adding ammonia water dropwise, stir at room temperature for 1 hour, reflux at 100°C for 10 hours, and filter the obtained white precipitate with deionized water. Wash to free of Cl - , and with AgNO 3 (0.1mol / l) solution detection, drying at 95°C for 10h to obtain Zr(OH) 4 .

[0023] Preparation of WO by Equal Volume Impregnation 3 / ZrO 2

[0024] Dissolve 3g ammonium metatungstate in 24mL water, stir evenly, add 20g Zr(OH) 4 , immerse at room temperature for 24 hours, remove water in a water bath at 80°C, dry at 110°C for 1...

Embodiment 2

[0028] Taking the preparation of Cop-15%W / Zr-800 as an example, the catalyst preparation process is described in detail.

[0029] 30g ZrOCl 2 ·8H 2 Dissolve O in 270ml of water, stir evenly, dissolve 2.2g of ammonium metatungstate in 28mL of water, add ZrOCl dropwise to the ammonium metatungstate solution 2 ·8H 2 O aqueous solution, stirring vigorously at room temperature for 0.5 h, adding NH 3 ·H 2 O (25-28%), while adding dropwise, use a pH meter to measure the pH. When the pH meter reads 9.0, stop the dropwise addition, stir at room temperature for 2 hours, age at 100°C for 24 hours, filter, and wash the obtained white precipitate with deionized water to no Cl -, and with AgNO 3 (0.1mol / l) solution detection, drying at 110°C for 10h, and roasting the dried precipitate in a tube furnace at 800°C for 3h, the calcined catalyst is marked as Cop-15%W / Zr-800, where n represents WO 3 weight percent content.

[0030] Cop-15%W / Zr-800 catalyzes the dehydration process of sorb...

Embodiment 3

[0032] The process of H-20%W / Zr-800 catalyzing the dehydration of sorbitol to prepare isosorbide is as follows: first add 20g sorbitol to the flask, heat it to 210°C, add 1.2g H-20%W / Zr after the sorbitol melts -800, turn on the vacuum pump to decompress the reaction device to 3000Pa, the reaction time is 2h, and the stirring speed is 600r / min. After the reaction, cool to room temperature, add 100ml of water to extract the product, and use high performance liquid chromatography to detect the sample. The conversion of sorbitol was >99%, and the yield of isosorbide was 72%.

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Abstract

The invention provides a method for preparing isosorbitol by dehydration of sorbitol. A catalyst is prepared by a reflux impregnation method or a co-precipitation method, the roasting temperature is 700 to 850 DEG C, and the loading amount of WO3 (tungsten trioxide) or MoO3 (molybdenum trioxide) is 15 to 30wt%. The method has the advantages that the reaction is performed under the conditions of nosolvent and pressure relief, the reaction temperature is 170 to 230 DEG C, the reaction time is 1 to 8h, and the pressure in the container is 1 to 5000Pa; the catalyzing system is used for catalyzingthe sorbitol to dehydrate at high efficiency, and the yield rate of isosorbitol can reach 70% or more; the reaction conditions are mild, the catalyzing efficiency is high, the catalyst is easy to separate and can be recycled, and the like; the higher practicality and economy are realized.

Description

technical field [0001] The invention relates to a preparation method of chemicals, in particular to a method based on WO 3 / ZrO 2 or MoO 3 / ZrO 2 The solid superacid is used as a catalyst, and is applied to the method for preparing isosorbide by dehydrating sorbitol under the condition of no solvent and reduced pressure. Background technique [0002] Isosorbide is a new bio-based chemical that can replace many petrochemicals and is used in pharmaceutical synthesis, polymer materials, polymer modification, electronics and other fields. For example, isosorbide can be used in the field of liquid crystal materials as a monomer or additive, which greatly improves the photoelectric properties of liquid crystal materials; adding isosorbide to polyester can increase the viscosity and improve the glass transition temperature and strength of the polymer; It has good fat solubility and can be quickly absorbed after oral administration, and can be used as an excellent antihypertensi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04B01J23/30B01J23/28
CPCB01J23/002B01J23/28B01J23/30C07D493/04Y02P20/584
Inventor 梁长海张玉莹杜中田李闯陈霄
Owner DALIAN UNIV OF TECH
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