Crystallization method with a fine crystal elimination

A crystallization and fine-crystal technology, applied in solution crystallization, crystallization purification/separation, organic chemistry, etc., can solve the problems of small crystal size and frequent crystallizer cleaning, and achieve the effect of good technical effect

Active Publication Date: 2013-12-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is that the existing crystallization method has small crystal size and frequent cleaning of the crystallizer, and a novel crystallization method with fine grain elimination is provided

Method used

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  • Crystallization method with a fine crystal elimination
  • Crystallization method with a fine crystal elimination
  • Crystallization method with a fine crystal elimination

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028]The crystallization method of band fine grain elimination described in the present invention produces p-xylene

[0029] like figure 2 Said, the mixed xylene raw material 12 contains 90% p-xylene, and the flow rate is 14864kg / h. The mixed xylenes are crystallized in tank crystallizer 1, and the crystallization temperature is -14.5°C. Crystal clear mother liquor 8 flows out from the crystallizer top in the kettle type crystallizer 1, and crystal clear mother liquor 8 is divided into two shares, and the crystal clear mother liquor 9 that the first share accounts for 50% by weight is discharged, and the crystal clear mother liquor that the second share accounts for 50% by weight 10 into the middle groove 11. The magma 2 in the kettle crystallizer 1 flows out from the bottom of the crystallizer, and is separated by a solid-liquid separator 3 to obtain p-xylene crystals 4 and crystallization and filtration mother liquor 5 . The p-xylene crystal 4 is discharged as a product...

Embodiment 2

[0031] The crystallization method of band fine grain elimination described in the present invention produces p-xylene

[0032] use as image 3 In the crystallization method with fine crystal elimination, the second crystallization and filtration mother liquor 7 accounting for 91% by weight is returned to the kettle crystallizer 1, and the operating temperature of the sleeve crystallizer 13 is -4.2°C, and the rest of the operations are The conditions are the same as in Example 1, and the results are listed in Table 1.

Embodiment 3

[0034] The crystallization method of band fine grain elimination described in the present invention produces p-xylene

[0035] use as figure 2 The described crystallization method with fine crystal elimination, wherein, the crystal clear mother liquor 8 is divided into two shares, the first crystal clear mother liquor 9 accounting for 33% by weight is discharged, and the second crystal clear mother liquor 10 accounting for 67% by weight enters the middle In the tank 11; the crystallization and filtration mother liquor 5 is divided into two shares, the crystallization and filtration mother liquor 6 accounting for 14% by weight of the first share is discharged, and the crystallization and filtration mother liquor 7 of the second share of 86% by weight enters the middle tank 11; the casing type crystallizer The operating temperature of 13 is-1.4 ℃; The weight ratio of crystallization clear mother liquor 8 and crystallization filtration mother liquor 6 is 0.68: 1;

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Abstract

The invention relates to a crystallization method with a fine crystal elimination, which mainly solves the problems of small crystal granularity and frequent crystallizer cleaning in the prior art. The invention is characterized in that crystallized clear mother liquor in a kettle-type crystallizer flows out from the upper part of the crystallizer, the crystallized clear mother liquor is divided into two streams, a first stream I of the crystallized clear mother liquor which takes account for 5-95% of weight is discharged, a second stream II of the crystallized clear mother liquor which takes account for 5-95% of weight enters in an intermediate groove; crystal slurry in the kettle-type crystallizer flows out from the lower part of the crystallizer and separated by a solid-liquid separator to obtain crystals, and crystallized and filtered mother liquor; crystals as products are discharged, the crystallized and filtered mother liquor is divided into two streams, a first stream I of the crystallized and filtered mother liquor which takes account for 5-95% of weight is discharged, a second stream II of the crystallized and filtered mother liquor which takes account for 5-95% of weight enters in the intermediate groove or directly returns to the kettle-type crystallizer; the raw material enters into the intermediate groove, the material in the intermediate groove is performed heat exchange through a tubular type crystallizer and returned to the kettle-type crystallizer; wherein the weight ratio of the crystallized clear mother liquor to the crystallized and filtered mother liquor is 0.1:1-10:1. The technical scheme better solves the problems, and can be used in industrial crystallization production.

Description

technical field [0001] The invention relates to a crystallization process with fine grain elimination. Background technique [0002] The kettle-type crystallizer is a type of crystallizer commonly used in industry. It uses the refrigerant in the jacket to exchange heat and cool the raw material, so that the product is crystallized from the raw material. The heat transfer efficiency of indirect heat exchange is low, and crystal scars are easy to form on the cooling surface, and the formed crystal scars will further reduce the heat transfer efficiency. Therefore, the production capacity of the kettle crystallizer is not high, and its production capacity is limited by the exchange rate of the crystallizer. thermal area. In order to further increase the production capacity of the kettle crystallizer, a casing crystallizer with a scraper is usually set outside the kettle crystallizer. The purpose of setting up the sleeve-type crystallizer is to provide more heat exchange area f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D9/02C07C15/08C07C7/14
Inventor 陈亮肖剑钟禄平卢咏琰郭艳姿
Owner CHINA PETROLEUM & CHEM CORP
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