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Device for evaporative crystallization and crystallization method of ethyl maltol

A technology of ethyl maltol and evaporative crystallization, applied in evaporative separation crystallization, solution crystallization, organic chemistry, etc., can solve the problems of low production efficiency, large product quality differences, and many steps, and achieve the promotion of precipitation and regular distribution of flow field orderly effect

Active Publication Date: 2019-03-26
ZHEJIANG NHU CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Many steps, high demand for equipment, large investment, low production efficiency, high energy consumption, and difficult to control crystal particle size
The batch crystallization operation also has the problem of large product quality differences between different batches

Method used

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  • Device for evaporative crystallization and crystallization method of ethyl maltol
  • Device for evaporative crystallization and crystallization method of ethyl maltol
  • Device for evaporative crystallization and crystallization method of ethyl maltol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] This embodiment adopts as figure 1 The shown device for evaporative crystallization carries out the crystallization operation, specifically according to the following steps:

[0080] (1) The ethyl maltol crude product with a purity of 87% was dissolved in water, decolorized and filtered to obtain a raw material solution of ethyl maltol with a concentration of 14% by mass, and the temperature was 35°C.

[0081] (2) Turn on the heater 4, pump the raw material liquid of ethyl maltol from the raw material liquid inlet pipe 1, and transport it to the heater 4 through the second circulation pump 3, and the temperature of the raw material liquid rises to 62°C. The heated raw material liquid continuously flows into the evaporation vessel 6 at a rate of 240kg / h.

[0082] (3) Control the vacuum degree of evaporation container 6 to be 0.065MPa, make raw material liquid enter boiling state after entering evaporation container 6, ethanol evaporation rate is maintained at 157kg / h, s...

Embodiment 2

[0087] This embodiment adopts as figure 2 The shown device for evaporative crystallization carries out the crystallization operation, specifically according to the following steps:

[0088] (1) The ethyl maltol crude product with a purity of 87% was dissolved in an ethanol solvent, decolorized and filtered to obtain a raw material solution of ethyl maltol with a concentration of 14% by mass, and the temperature was 35°C.

[0089] (2) Turn on the heater 4, pump the raw material liquid of ethyl maltol from the raw material liquid inlet pipe 1, and transport it to the heater 4 through the second circulation pump 3, and the temperature of the raw material liquid rises to 62°C. The heated raw material liquid continuously flows into the evaporation vessel 6 at a rate of 240kg / h. The diameter of the upper end of the channel 18 is 5 mm, the ratio of the diameter of the lower end of the channel 18 to the diameter of the upper end of the channel 18 is 1.8:1, and the opening ratio of t...

Embodiment 3

[0095] On the basis of embodiment 2, the flow rate of the first circulating pump 13 of step (3) is set to 417kg / h, and the ratio control of the flow rate of the flow of the first stream and the flow of the second stream is 0.4, step ( 5) The flow rate of the first circulating pump 13 is controlled at 384kg / h, and the ratio of the flow rate of the first stream to the second stream is controlled to be 0.4; all the other conditions are the same as in Example 2. The resulting filter cake was dried to obtain white ethyl maltol crystalline particles with a purity of 97.8%. The crystallization yield was 89.5% based on the amount of feed, and the 60-mesh pass rate of ethyl maltol crystalline particles was 85.8%. , The pass rate of 80 mesh is 32%, and the pass rate of 120 mesh is 0.5%.

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Abstract

The invention provides a device for evaporative crystallization. The device for evaporative crystallization comprises an evaporative container and a crystallization container and also comprises a first circulation unit and a second circulation unit, wherein the first circulation unit comprises a first branch pipe, a first circulation pump and a first circulation feeding pipe which are connected insequence; the second circulation unit comprises a second branch pipe, a second circulation pump, a heater and a second circulation feeding pipe which are connected in sequence; the first circulationfeeding pipe and the second circulation feeding pipe are connected with the evaporative container. The invention also provides a crystallization method of ethyl maltol. The method provided by the invention has the beneficial effects that the additional first circulation loop is arranged, first crystal is guided into the evaporative container again as a crystal core to grow to obtain larger secondparticles and induce to obtain more and more-uniform second particles.

Description

technical field [0001] The invention relates to the field of chemical process improvement, in particular to a device for evaporative crystallization and a crystallization method of ethyl maltol. Background technique [0002] Maltol belongs to food flavor ingredients and flavor enhancers, which can enhance and harmonize the aroma of products and cover up bad flavors. Adding it to poultry and livestock feed additives can greatly increase the palatability of the feed and enhance the appetite of poultry and livestock, so it has extremely high research and development value and has a large market demand. [0003] At present, the following methods are mainly used for the crystallization of ethyl maltol: [0004] a) Sublimation crystallization, for example, Chinese invention application CN201510395551.7 discloses a sublimation process of ethyl maltol crystallization that reduces energy consumption. In the sublimation kettle, the temperature of the electric heating kettle is contr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D9/02C07D309/40
CPCB01D9/0031C07D309/40
Inventor 马啸陈志荣张玉红朱全东刘金龙李传鹏何博张相如鲁光银田路飞
Owner ZHEJIANG NHU CO LTD
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