Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for preparing chromatographic pure dichloromethane

A dichloromethane, chromatographically pure technology, applied in the field of chemical reagents, to achieve the effects of stable operation, high product purity, and simple process

Inactive Publication Date: 2011-06-15
天津市康科德科技有限公司
View PDF1 Cites 8 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the deficiencies of the existing production technology and provide a method for preparing chromatographically pure dichloromethane. This method can effectively remove a small amount of impurities such as chloroform, ethanol, ether and water in the raw materials that are difficult to remove and have low content. , to prepare chromatographically pure dichloromethane that satisfies liquid chromatography analysis

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for preparing chromatographic pure dichloromethane
  • Method for preparing chromatographic pure dichloromethane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A preparation method of chromatographically pure dichloromethane, the steps are as follows:

[0023] (1) Adsorption: Put the industrial-grade methylene chloride raw material liquid into the adsorption column, in which the adsorption column is 1.5m in length, 3.5cm in inner diameter, and contains basic alumina with a particle size of 0.15-0.30mm. The flow rate flows through the adsorption column for adsorption and removal of impurities;

[0024] In this step, basic alumina and dichloromethane are fully contacted and adsorbed to remove a small amount of organic impurities, such as a small amount of impurities such as chloroform, ethanol, ether, etc. The purity of the raw material dichloromethane is 99.5%.

[0025] (2) Drying: The adsorbed dichloromethane flows through a drying column equipped with desiccant 4A molecular sieve. The specification of the column is the same as that of the adsorption column. The min flow rate flows through the drying column for drying, and th...

Embodiment 2

[0029] A preparation method of chromatographically pure dichloromethane, the steps are as follows:

[0030] (1) Adsorption: The industrial-grade dichloromethane raw material solution is poured into the adsorption column, in which the adsorption column is 1.5m long, with an internal diameter of 3.5cm, and silica gel with a particle size of 0.15-0.30mm inside, and the dichloromethane flows through it at a flow rate of 80mL / min. Adsorption column for adsorption and removal of impurities;

[0031] In this step, silica gel and methylene chloride are fully contacted and adsorbed to remove a small amount of organic impurities.

[0032] (2) Drying: The absorbed dichloromethane flows through a calcium hydride drying column equipped with a desiccant. The specification of the column is the same as that of the adsorption column. The flow rate flows through the drying column for drying, and the water content after drying is controlled at ≤0.02%;

[0033] (3) Rectification: Put the dried ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
Apertureaaaaaaaaaa
Login to View More

Abstract

The invention relates to a method for preparing chromatographic pure dichloromethane. The method comprises the following steps: using an adsorbent to remove few impurities such as chloroform, ethanol, ethyl ether and the like, using a desiccant to remove water and finally carrying out rectification according to set process conditions to further remove the impurities, thus finally obtaining the chromatographic pure dichloromethane product. The method has the following advantages and positive effects: the process steps are as follows: adopting alkaline alumina or silica gel as the adsorbent to remove the organic impurities in the raw material, then using a 4A molecular sieve desiccant to remove water and finally carrying out rectification according to set process conditions, thus obtaining the high performance liquid chromatographically pure dichloromethane product with purity being more than 99.9%, pesticide residues being more than 90% and yield being more than 95%; and the method has simple process, is convenient to operate and has the advantages of high product purity, stable operation and suitability for scale production compared with the existing methods.

Description

technical field [0001] The invention belongs to the field of chemical reagents, and relates to a preparation method of a special organic solvent for high-performance liquid chromatography, in particular to a preparation method of chromatographically pure dichloromethane. Background technique [0002] High-performance liquid chromatography reagents are high-purity organic reagents specially used for liquid chromatography analysis and pesticide residue detection. [0003] The preparation methods of liquid chromatography reagents in my country are rarely reported due to technical confidentiality reasons. Although a few manufacturers have this product, the quality level varies greatly, and the application is very unstable. Many scientific research units still rely on imports. Therefore, It is still blank in this field. It can be seen that the development of high-performance liquid chromatography reagents in my country lags behind the development needs of current scientific resear...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07C19/03C07C17/38
Inventor 宋金链张玉芝
Owner 天津市康科德科技有限公司
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com