Isosorbide preparation method

A technology of isosorbide and sorbitol solution, applied in the direction of organic chemistry, etc., can solve the problems of high cost of isosorbide, high requirements for reaction equipment, environmental pollution, etc., reduce reaction equipment parameters, reduce production costs, avoid The effect of high power consumption

Active Publication Date: 2018-06-05
FUTASTE PHARM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, most of the domestic preparation methods of isosorbide use processes such as vacuum distillation and organic solvent extraction and crystallization. The process is complicated, the requirements for reaction equipment are high, resources are wasted, and environmental pollution is serious, resulting in high production costs of isosorbide.

Method used

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  • Isosorbide preparation method

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Experimental program
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Effect test

Embodiment 1

[0026] This isosorbide preparation method step is as follows:

[0027] 1) solid sorbitol is dissolved in water, is made into the solution that mass fraction is 10%; Add phosphorus modified HZSM-5 molecular sieve in sorbitol solution, the addition amount of phosphorus modified HZSM-5 molecular sieve is sorbitol solution dry matter 15% by weight; at 150 ° C, stirring for 3 hours under the condition that the nitrogen filling pressure is 3Mpa, and dehydration reaction is carried out to obtain a solid-liquid mixture;

[0028] 2) The solid-liquid mixture is filtered to remove insolubles to obtain the filtrate, which is detected by HPLC, and the purity of isosorbide in the liquid is 77%, as shown in figure 1 and shown in Table 1;

[0029] 3) The filtrate is decolorized with activated carbon, the amount of activated carbon added is 1% of the dry matter weight of the solution, kept at 80° C. for 40 min, and filtered to obtain the filtrate;

[0030] 4) Ion-exchange the filtrate throug...

Embodiment 2

[0036] This isosorbide preparation method step is as follows:

[0037] 1) liquid sorbitol is diluted with water to Brix and be 30% solution; In sorbitol solution, add phosphorus-modified HZSM-5 molecular sieve, the addition of phosphorus-modified HZSM-5 molecular sieve is 8% of sorbitol solution dry matter weight ; Stirring for 5 hours at 220°C under nitrogen filling pressure of 7Mpa, performing dehydration reaction to obtain a solid-liquid mixture;

[0038] 2) Filtrating the solid-liquid mixture to remove insoluble matter to obtain a filtrate, which is detected by HPLC, and the purity of isosorbide in the liquid reaches 81%;

[0039] 3) The filtrate is decolorized with activated carbon, the amount of activated carbon added is 5% of the dry matter weight of the solution, kept at 70° C. for 30 min, and filtered to obtain the filtrate;

[0040] 4) Ion-exchange the filtrate through D301 anion resin, 001×7 cation resin, and D301 anion resin in sequence to obtain an ion-exchange l...

Embodiment 3

[0044] This isosorbide preparation method step is as follows:

[0045] 1) solid sorbitol is dissolved in water, is made into the solution that mass fraction is 50%; Add phosphorus modified HZSM-5 molecular sieve in sorbitol solution, the addition amount of phosphorus modified HZSM-5 molecular sieve is sorbitol solution dry matter 2% by weight; at 300°C, stirring for 7 hours under the condition of nitrogen filling pressure of 10Mpa, dehydration reaction to obtain a solid-liquid mixture;

[0046] 2) Filtrating the solid-liquid mixture to remove insoluble matter to obtain a filtrate, which is detected by HPLC, and the purity of isosorbide in the liquid reaches 78%;

[0047] 3) The filtrate is decolorized with activated carbon, the amount of activated carbon added is 10% of the dry matter weight of the solution, kept at 60° C. for 20 min, and filtered to obtain the filtrate;

[0048] 4) Ion-exchange the filtrate through D301 anion resin, 001×7 cation resin, and D301 anion resin i...

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Abstract

The invention discloses an isosorbide preparation method. The method comprises the following steps: 1) adding a phosphorus modified HZSM-5 molecular sieve into a sorbitol solution, and carrying out adehydration reaction to obtain a solid-liquid mixture; 2) filtering the solid-liquid mixture so as to obtain the filtrate; 3) performing actived carbon decoloration on the filtrate, and filtering again so as to obtain the filtrate; 4) performing ion exchange on the filtrate by virtue of D301 anion resins, 001*7 cation resins and D301 anion resins respectively so as to obtain ion exchange liquid; 5) concentrating the ion exchange liquid into Brix being 75-90%, and performing primary cooling crystallization; and centrifuging to obtain a crude isosorbide crystal; and 6) adding water into the crude isosorbide crystal, heating and dissolving to enable the Brix to be 70-85%, performing secondary cooling crystallization, centrifuging and drying, thereby obtaining the product isosorbide crystal. Compared with the prior art, the method disclosed by the invention has the advantages that the isosorbide produced by the method is high in yield, the number of by-products is few and the stability ishigh, so that the isosorbide preparation process is simplified, and the cost is reduced.

Description

technical field [0001] The invention relates to the technical field of isosorbide processing, in particular to a preparation method of isosorbide. Background technique [0002] Isosorbide is a dehydrated derivative of sorbitol. Due to its functional and structural properties, it is widely used in medicine and chemical industry. For medicine, it has strong drug properties and can be used to treat It is an excellent antihypertensive drug and diuretic for intracranial hypertrophy, and can also be used as a pharmaceutical intermediate to prepare specific drugs for treating coronary heart disease. For industry, it can be applied to the synthesis of new highly analytical materials. In addition, it also has a lot of applications in the fields of electronics and national defense, such as comonomer synthesis and modification of commercial polymers, which are used to improve the high temperature performance and impact performance of polymers, and improve the transparency and degradat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04
CPCC07D493/04
Inventor 孙鲁邱学良付丽云邵竞锋
Owner FUTASTE PHARM CO LTD
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