A kind of preparation method of crystalline isosorbide

A technology for isosorbide and sorbitol, applied in the field of preparation of crystalline isosorbide, can solve the problems of high production cost, high pollution and high energy consumption, and achieve the effects of reducing equipment investment and operating costs and reducing production costs

Active Publication Date: 2019-05-07
南京凯通粮食生化研究设计有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Aiming at the deficiencies in the refining of the above-mentioned isosorbide reaction solution, the present invention provides a simple and practical process for refining and crystallizing the isosorbide reaction solution, which solves the problems of complex purification process, high energy consumption, high production cost and large pollution in the prior art. The problem

Method used

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  • A kind of preparation method of crystalline isosorbide
  • A kind of preparation method of crystalline isosorbide
  • A kind of preparation method of crystalline isosorbide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Using solid sorbitol as a raw material and solid acidic molecular sieve as a catalyst, catalyze the reaction for 4 hours at a pressure of -0.02 to -0.06 MPa, a temperature of 180°C, and a molten state to obtain a reaction liquid.

[0046] The catalytic reaction is carried out in a molten state. After the reaction is completed, pure water is added to dilute the reaction solution until the mass percentage concentration is 50-55% to obtain a diluted solution. At this time, the diluted solution has better fluidity.

[0047] The diluted solution was filtered, and the filtrate and filter residue were collected. The filter residue is the molecular sieve used in the reaction, which is recycled. Molecular sieves can be reused 5-8 times.

Embodiment 2

[0049] The filtrate is decolorized, deionized and separated with a decolorization, deionization and separation mixture device. The decolorization, deionization and separation mixture device consists of the first group of chromatographic systems and the second group of chromatographic systems:

[0050] (1) The first group of chromatographic systems is composed of 1 chromatographic column, and the outlet of chromatographic column 2 and the inlet are connected by booster pump 41, isolation valve 1, connecting pipe 3 and flowmeter 4 54; Described chromatographic column-2 inlet is connected with eluent valve-VWW, material valve-VFF; Described eluent valve-VWW and material valve-VFF are connected with eluent main pipe 11 and material main pipe 12 respectively; Described chromatographic column Outlet 1 is connected with impurity valve VS and feed valve VFS; the feed valve VFS is connected to the feed pipe 121, and then connected to the feed valves VF1~VFn of the second group of chrom...

Embodiment 3

[0065] The isosorbide solution A is concentrated to a percentage concentration of 80-85% to obtain a concentrated solution.

[0066] The concentrated solution is naturally cooled and crystallized, the cooling rate is 1~5°C / h, the amount of seed crystals added is 1%, stirred, cooled to 20~25°C, left standing for 8 hours, then dehydrated and dried to obtain crystalline isosorbide The product has a purity of 98.0-99.5%.

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Abstract

The invention relates to the technical field of isosorbide deep processing, and particularly discloses a preparation method of crystalized isosorbide. The method comprises the steps that solid isosorbide is adopted as a raw material, a solid acid molecular sieve is adopted as a catalyst, a fusion method is adopted for preparing an isosorbide reaction solution; the reaction solution is diluted and filtered to obtain filtrate an d filter residues; the filter residues are adopted as a catalyst to be recycled; the filtrate is an isosorbide mixing solution, a decoloration ion removal and mixture separation device is used for processing the isosorbide mixing solution, and then concentration, normal temperature aqueous phase process crystallization and drying are performed to obtain crystalized isosorbide. The content of the crystalized isosorbide is 98% or above. The preparation method of the crystalized isosorbide has the advantages of being simple in technological process, small in equipment investment, low in operation cost, free of acid-base and activated carbon consumption, and the like.

Description

technical field [0001] The invention relates to the technical field of deep processing of sorbitol, in particular to a preparation method of crystalline isosorbide. Background technique [0002] As a secondary dehydration derivative of sorbitol, isosorbide is a new type of bio-based material and a widely used chemical intermediate. It is known as an important bio-based chemical raw material in the future after polylactic acid. Isosorbide has remarkable medicinal value and is widely used in medicine, food, chemical industry, feed additive and other industries. The polymer of isosorbide has the advantages of high transparency and mechanical strength and can be used to produce degradable polymers, which further expands the application field of isosorbide. In addition, due to the unique chirality of isosorbide, it can be used to prepare liquid crystal materials in the fields of electronics and national defense. Japan has also begun to promote the application of isosorbide poly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/04
CPCY02P20/584
Inventor 李瑛周日尤伍玉碧吴鹏曹媛杜小霞贾红程
Owner 南京凯通粮食生化研究设计有限公司
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