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Method for continuous production of isosorbide and device used therefor

A technology for isosorbide and sorbitol, which is applied in the field of continuous production of isosorbide, can solve problems such as material consumption, high energy consumption, complicated process, etc., and achieves the effects of low temperature and energy consumption, simplified separation process and good quality of finished products

Active Publication Date: 2016-12-07
长春鸿成生物化工材料技术开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These methods are feasible and advanced, but the process is relatively complicated, and the material consumption and energy consumption are relatively high.

Method used

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  • Method for continuous production of isosorbide and device used therefor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] In the 500mL reactor that is provided with stirrer, add the polyphosphoric acid of 180 grams solid sorbitol and 0.9 gram, each component of reaction device is according to figure 1 Connect as shown, and then evacuate. Maintain a vacuum degree of 200pa and heat at a temperature of 130°C. Under the action of polyphosphoric acid, the molten sorbitol reacts for 1 hour, then the oil bath is heated to 280°C, and the temperatures of the first condenser and the second condenser are controlled to be 60°C and -10°C, a total of 112.6 grams of product were collected in the product tank (yield: 78.0% of theoretical value), with a purity of 99.5%.

[0038]The resulting product had a melting point of 61-62°C.

[0039] HRMS-EI(m / e,%): 146.0578(M + ,5.14),86.0340(C 4 h 6 o 2 ,100),69.0325(C 4 h 5 O, 18.20), 58.0408 (C 3 h 6 O, 13.41), 44.0254 (C 2 h 4 O, 17.57).

[0040] The peak at 146.0578 is the molecular ion peak, and the peak at 86.0340 is the fragment ion generated aft...

Embodiment 2

[0044] In the 500mL reactor that is provided with agitator, add 100 grams of 70% sorbitol aqueous solution and 0.4 gram of polyphosphoric acid, each assembly of reaction device is according to figure 1 Connect as shown, and then evacuate. Maintain a vacuum degree of 300pa, heat at a temperature of 135°C, and carry out the reaction under the action of polyphosphoric acid until the reactor is anhydrous, then the oil bath is heated to 260°C, and the temperatures of the first condenser and the second condenser are controlled respectively At 52°C and -15°C, a total of 44.1 g of product (yield: 78.5% of theoretical value) was collected in the product tank with a purity of 99.6%.

[0045] The obtained product characterization result is similar to Example 1.

Embodiment 3

[0047] In the 500mL reactor that is provided with stirrer, add the polyphosphoric acid of 60 gram solid sorbitol and 0.3 gram, each component of reaction device is according to figure 1 Connect as shown, and then evacuate. Maintain a vacuum degree of 200pa and heat at a temperature of 130°C. Under the action of polyphosphoric acid, the molten sorbitol reacts for 1 hour, then the oil bath is heated to 240°C, and the temperatures of the first condenser and the second condenser are controlled to be 52°C and -15°C, after collecting 15 grams of product in the product tank, add 30 grams of sorbitol to the system through the raw material tank, continue the reaction under the same conditions, collect 30 grams of product, and then add 30 grams of sorbitol to the system The polyphosphoric acid of gram and 0.1 gram still reacts under the same conditions, and a total of 75.2 grams of products are collected (yield: 78.1% of theoretical value), with a purity of 99.5%.

[0048] The obtained...

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Abstract

The invention relates to a method for continuously producing isosorbide, which comprises the following steps: (1) feeding: mixing sorbitol and a catalyst in a reactor; (2) reaction: under reduced pressure, controlling the temperature in the reactor to sequentially initiate first dehydration reaction and second dehydration reaction of the sorbitol so as to generate the isosorbide, and meanwhile, enabling the isosorbide and water to form a gaseous mixture; and (3) condensation separation: controlling the condensation temperature of the condenser to sequentially condense the isosorbide and water in the gaseous mixture from the reactor, thereby obtaining the isosorbide. The invention also relates to a device for the method.In the sorbitol dehydration reaction process, the isosorbide and water are separated in time by distillation, thereby promoting the selective dehydration reaction, simplifying the separation technique and implementing purification of the isosorbide.

Description

technical field [0001] The invention relates to a method for continuous production of isosorbide and a device used therein. Background technique [0002] Isosorbide, the secondary dehydration product of sorbitol, as a new type of bio-based material, is widely used in food, cosmetics, plastics, medicine and other polymerization fields. At present, a research hotspot in the application of isosorbide is to use it as a comonomer for the modification of polymers such as polyether, polyester, polyurethane, and polycarbonate, which can significantly improve the high temperature performance and impact resistance of the polymer. Isosorbide and terephthalic acid are used to polymerize polyester with similar properties to polyethylene terephthalate (PET), which can be used as a substitute for PET polyester, and it has good optical properties, thermal properties, and mechanical properties. properties and dyeability. Isosorbide has great potential in the modification of polymers and th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/04
CPCC07D493/04
Inventor 林英杰段海峰褚腊林
Owner 长春鸿成生物化工材料技术开发有限公司
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