Method and device for continuously producing isosorbide

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

Active Publication Date: 2014-08-13
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

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Problems solved by technology

These methods are feasible and advanced, but the process is relatively complic

Method used

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  • Method and device for continuously producing isosorbide

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0036] Example 1

[0037] In a 500 mL reactor equipped with a stirrer, 180 grams of solid sorbitol and 0.9 grams of polyphosphoric acid were added, and the components of the reaction device were figure 1 Make connections as shown, and then pump down. Maintain a vacuum of 200pa and heat at a temperature of 130°C. Under the action of polyphosphoric acid, the molten sorbitol reacts for 1 hour, and then the oil bath is heated to 280°C, and the temperature of the first condenser and the second condenser are controlled to 60°C and At -10°C, a total of 112.6 grams of product was collected in the product tank (yield: 78.0% of theoretical value), with a purity of 99.5%.

[0038] The resulting product has 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 after ...

Example Embodiment

[0043] Example 2

[0044] In a 500 mL reactor equipped with a stirrer, 100 grams of 70% sorbitol aqueous solution and 0.4 grams of polyphosphoric acid were added, and the components of the reaction device were figure 1 Make connections as shown, and then pump down. Maintain a vacuum of 300pa, heat at a temperature of 135°C, and make the reaction proceed under the action of polyphosphoric acid until the reactor is evaporated without water, then the oil bath is heated to 260°C, and the temperature of the first condenser and the second condenser are controlled respectively At 52°C and -15°C, a total of 44.1 grams of product (yield: 78.5% of theoretical value) was collected in the product tank, with a purity of 99.6%.

[0045] The resulting product characterization results are similar to those of Example 1.

Example Embodiment

[0046] Example 3

[0047] In a 500 mL reactor equipped with a stirrer, 60 grams of solid sorbitol and 0.3 grams of polyphosphoric acid were added, and the components of the reaction device were figure 1 Make connections as shown, and then pump down. Maintain a vacuum of 200 Pa and heat at a temperature of 130°C. Under the action of polyphosphoric acid, the molten sorbitol reacts for 1 hour, and then the oil bath is heated to 240°C. The temperature of the first condenser and the second condenser are controlled to 52°C and At -15°C, after 15 grams of product are collected 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 Grams and 0.1 grams of polyphosphoric acid were still reacted under the same conditions. A total of 75.2 grams of product was collected (yield: 78.1% of the theoretical value) with a purity of 99.5%....

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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 therefor. 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 t...

Claims

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Application Information

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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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