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Method of preparing hydronol

A technology of isosorbide and sorbitol, which is applied in the field of isosorbide preparation from biomass raw materials, can solve the problems of reduced reaction rate, narrow operating temperature range, and difficult removal of ions, and achieves simple reaction operation process, obvious catalytic effect, and easy Effects of Separation and Recycling

Inactive Publication Date: 2009-07-29
青州市瑞鑫再生资源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are some common deficiencies in these production processes: kettle reaction, which requires dehydration under certain pressure or vacuum conditions, is not suitable for continuous production; inorganic acid as a catalyst has higher requirements for catalytic reactors, long life but easy to generate dark by-products Product, although the ion exchange resin produces few by-products, its service life is short; the operating temperature range is narrow, high temperature can easily lead to sorbitol decomposition or product carbon deposition, and low temperature can easily cause the water generated by the reaction to be unable to be removed in time to reduce the reaction rate; Separation often requires organic solvents such as toluene or xylene to participate in distillation and recrystallization, and a small amount of inorganic acid ions in the product are difficult to remove
[0004] Along with the inconvenience that inorganic acid catalyst brings in production, some relevant replacement catalysts have appeared gradually, the most notable is exactly solid acid catalyst, as HY and HZSM-5 molecular sieve (USP 6013812 and 7420067), but these molecular sieves can obtain The yield of isosorbide is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 64.4gZrOCl 2 ·8H 2 O was dissolved in 500ml of water, 28% ammonia water was added dropwise until the pH of the solution was 8.4, suction filtered and washed with deionized water until Cl-free - Existence, resulting Zr(OH) 4 The filter cake was dried in an oven at 120°C for 24 hours, and then calcined at 500°C for 5 hours to obtain ZrO 2 .

[0019] Take 7.3972g ZrO 2 Add 6.7mL 1M H 3 PO 4 , add a little water, heat in a water bath at 80°C, immerse and stir until evaporated to dryness, dry at 100°C, then heat to 600°C within 3 hours, and calcined at 600°C for 4 hours to obtain PO with a molar ratio of P / Zr=1:9 4 3- / ZrO 2 catalyst. Lower the temperature and cool down, crush the tablets into pieces and sieve with 30-50 meshes.

[0020] The above 30-50 mesh P / Zr=1:9 PO 4 3- / ZrO 2 2.0 g of the catalyst is loaded into the constant temperature section of the tubular fixed-bed reactor, and the rest is filled with quartz sand. After the system checks the seal, whe...

Embodiment 2

[0022] Get the ZrO prepared according to the example 1 method 2 Add 15.0mL 1M H to 7.3972g 3 PO 4 , add a little water, heat in a water bath at 80°C, immerse and stir until evaporated to dryness, dry at 120°C, then heat to 600°C within 3 hours, and calcined at 600°C for 6 hours to obtain PO with P / Zr=2:8 4 3- / ZrO 2 catalyst. Lower the temperature and cool down, crush the tablets into pieces and sieve with 30-50 meshes.

[0023] The above 30-50 mesh P / Zr=2:8 PO 4 3- / ZrO 2 2.0 g of the catalyst is loaded into the constant temperature section of the tubular fixed-bed reactor, and the rest is filled with quartz sand. After the system checks the seal, when the volumetric space velocity is 6h -1 N 2 The temperature of the catalytic bed is raised to 250°C under the gas flow rate, and then 10% sorbitol solution is injected into the system. After gasification, the reaction is carried out through the catalytic bed. After the reaction mixture is cooled by an ice-water bath an...

Embodiment 3

[0025] Get the 7.3972g ZrO prepared according to the example 1 method 2 Add 25.7 mL of 1M H 3 PO 4 , add a little water, heat in a water bath at 80°C, immerse and stir until evaporated to dryness, dry at 100°C, then heat to 650°C within 3 hours, and calcined at 650°C for 4 hours to obtain PO with P / Zr=3:7 4 3- / ZrO 2 catalyst. Lower the temperature and cool down, crush the tablets into pieces and sieve with 30-50 meshes.

[0026] The above 30-50 mesh P / Zr=3:7 PO 4 3- / ZrO 2 2.0 g of the catalyst is loaded into the constant temperature section of the tubular fixed-bed reactor, and the rest is filled with quartz sand. After the system checks the seal, when the volumetric space velocity is 1h -1 N 2 The temperature of the catalytic bed is raised to 350°C under the gas flow rate, and then 15% sorbitol solution is injected into the system. After gasification, the reaction is carried out through the catalytic bed. The liquid collected after 2 hours of reaction was sampled...

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PUM

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Abstract

The invention discloses a preparation method of isobide. Sorbierite is used as raw material and H3PO4 modified tetravalent metal oxides are used as catalyst to prepare the isobide by the dehydration reaction. The method has the advantages of simple operation process, low production cost, little environmental pollution, easy separation and recovery. The used modified catalyst has obvious catalytic effect. The selectivity of the isobide reaches as high as 63.49 percent, and the yield reaches as high as 62.23 percent. With strong practicality, the method is novel and can satisfy the industrialization requirements.

Description

technical field [0001] The invention relates to the field of chemical technology, in particular to a 3 PO 4 The modified tetravalent metal oxide is used as a catalyst, and the method for preparing isosorbide by adopting biomass raw materials. Background technique [0002] Isosorbide is a dehydrated derivative of D-sorbitol. In medicine, sorbitol is an excellent antihypertensive drug and diuretic for the treatment of intracranial hypertrophy. After dehydration, the hydroxyl group becomes an ether bond, and its fat solubility is greatly increased. Already completely different from sorbitol, absorbed immediately after oral administration is an effective osmotic oral dehydration diuretic. Isosorbide has been used clinically in foreign countries, but in China it is only used as an intermediate for the synthesis of anti-anginal drugs isosorbide dinitrate and isosorbide mononitrate. Isosorbide is an important raw material and intermediate of span and Tween surfactants in industr...

Claims

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Application Information

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IPC IPC(8): C07D493/04B01J21/06B01J23/14B01J27/16A61P9/12A61P7/10
Inventor 黄和余定华顾铭燕
Owner 青州市瑞鑫再生资源科技有限公司
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