Method for preparing isosorbide taking supported heteropoly acid as catalyst

A technology for immobilizing heteropolyacids and isosorbide, which is applied in the chemical industry, can solve the problems of reduced reaction rate, difficulty in removing ions, short life, etc., and achieves the effects of simple reaction operation process, easy separation and recovery, and low production cost

Inactive Publication Date: 2010-04-07
NANJING UNIV OF TECH
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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 the production, gradually appeared some relevant replacement catalysts, the most notable is exactly solid acid catalyst, as HY and HZSM-5 molecular sieve (USP 6013812 and 7420067), but under the catalysis of these molecular sieves The yield of isosorbide obtained is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Dissolve 30g of phosphotungstic acid in 100mL of water, stir and add 10g of SiO 2 , after stirring at room temperature for 24 hours, the temperature was raised to 60°C, stirred and dried to obtain a slurry, then transferred to a vacuum drying oven at 40°C for 24 hours to obtain a solid powder, and calcined at 300°C for 3 hours.

[0026] Crush the powder into tablets and sieve through 30-50 meshes to obtain SiO 2 Supported phosphotungstic acid catalyst.

[0027] 30-50 mesh SiO 2 Load 0.5g of phosphotungstic acid catalyst into the constant temperature section of the tubular fixed-bed reactor, and fill the rest with quartz sand. After the system checks the seal, the N 2 Under flow protection, the temperature of the catalyst bed was programmed to 250°C, and then 10% sorbitol solution was pumped into the system (the liquid hourly space velocity was 2.4h -1 ), reacted through the catalytic bed after gasification, the reaction mixture was cooled by an ice-water bath and ga...

Embodiment 2

[0029] Dissolve 30g of silicotungstic acid in 100mL of water, stir and add 10g of SiO 2 , after stirring at room temperature for 24 hours, the temperature was raised to 60°C, stirred and dried to obtain a slurry, then transferred to a vacuum drying oven at 40°C for 24 hours to obtain a solid powder, and calcined at 300°C for 3 hours.

[0030] Crush the powder into tablets and sieve through 30-50 meshes to obtain SiO 2 Supported silicotungstic acid catalyst.

[0031] 30-50 mesh SiO 2 Load 0.5g of silicotungstic acid catalyst into the constant temperature section of the tubular fixed-bed reactor, and fill the rest with quartz sand. After the system checks the seal, the N 2 Under flow protection, the catalytic bed layer is heated up to 250°C, and then 10% sorbitol solution is pumped into the system (the liquid hourly space velocity is 4.8h -1 ), reacted through the catalytic bed after gasification, the reaction mixture was cooled by an ice-water bath and gas-liquid separation...

Embodiment 3

[0033] Dissolve 30g of phosphotungstic acid in 50mL of water, stir and add 10g of ZrO 2 , after stirring at room temperature for 24 hours, the temperature was raised to 50°C, stirred and dried to obtain a slurry, then transferred to a vacuum drying oven at 30°C for 48 hours to obtain a solid powder, and calcined at 300°C for 3 hours.

[0034] Crush the powder into tablets and sieve through 30-50 meshes to obtain ZrO2 Supported phosphotungstic acid catalyst.

[0035] 30-50 mesh ZrO 2 Load 0.5g of phosphotungstic acid catalyst into the constant temperature section of the tubular fixed-bed reactor, and fill the rest with quartz sand. After the system checks the seal, the N 2 Under flow protection, the catalytic bed layer is heated up to 280°C, and then 10% sorbitol solution is pumped into the system (the liquid hourly space velocity is 2.4h -1 ), reacted through the catalytic bed after gasification, the reaction mixture was cooled by an ice-water bath and gas-liquid separation...

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Abstract

The invention discloses a method for preparing isosorbide by taking supported heteropoly acid as a catalyst. Sorbitol from a biological radical is used as a raw material to prepare the isosorbide directly through dehydration reaction. The method comprises the following steps: putting the catalyst into a constant temperature section of a fixed-bed reactor; introducing a reactant sorbitol solution into a reactor, and performing reaction through a catalyst bed after gasification; and separating a mixture obtained after the reaction to obtain the isosorbide. The method has simple operation process of the reaction, low production cost and light environmental pollution; the selectivity and yield of the isosorbide reaches up to 75.2 percent and 71.4 percent respectively, and the catalyst is easy to separate and recycle; and the method is a novel method which meets industrial demands and has strong practicality.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a method for preparing isosorbide from biomass raw materials. Background technique [0002] Isosorbide is a secondary dehydrated derivative of D-sorbitol, which is absorbed immediately after oral administration. It is an effective osmotic oral dehydration diuretic and an excellent antihypertensive drug for the treatment of intracranial hypertrophy. In foreign countries, isosorbide has been used clinically, but in China it is only used as an intermediate for the synthesis of anti-anginal drugs isosorbide dinitrate and isosorbide mononitrate. The research focus in recent years is to use it as a comonomer to synthesize modified commercial polymers, such as PET, polyether, polyester, polyurethane, polycarbonate, etc. Adding it to PET can increase the glass transition temperature of the polymer and increase the strength of the polymer. It can also be used in packaging bott...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04B01J31/16B01J31/18
Inventor 黄和孙鹏余定华唐振辰
Owner NANJING UNIV OF TECH
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