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Chromatographically pure N,N-dimethylacetamide as well as preparation method and production system thereof

A technology of dimethylacetamide and production system, applied to chromatographically pure N, can solve the problems of high cost, low product purity, low yield and the like, and achieve the effects of low production cost, good quality and high yield

Inactive Publication Date: 2017-11-10
HUBEI ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Chromatographically pure N, N-dimethylacetamide is one of the mobile phases commonly used in liquid chromatography. Various purification processes for N, N-dimethylacetamide have been reported at home and abroad. The purification methods mainly include: including: decolorization , adsorption, rectification, or a combination of decolorization, adsorption, and rectification steps. The disadvantages of these purification methods are that the product purity is not high, does not meet the scientific research requirements, or the yield is not high and the cost is too high

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  • Chromatographically pure N,N-dimethylacetamide as well as preparation method and production system thereof
  • Chromatographically pure N,N-dimethylacetamide as well as preparation method and production system thereof
  • Chromatographically pure N,N-dimethylacetamide as well as preparation method and production system thereof

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Embodiment 1

[0048] The present embodiment provides a kind of chromatographically pure N,N-dimethylacetamide, which adopts figure 1 Shown production system 100, and make according to following preparation method:

[0049] (1) Use industrial-grade N,N-dimethylacetamide as a raw material, transport it to the reaction kettle 002 through the raw material delivery pump 001, turn off the raw material delivery pump 001, start the reaction kettle 002 to stir, turn on the circulation pump 003, and establish the formation reaction In the circulation line between the bottom of the kettle 002, the circulating pump 003, the mixer 004 and the top of the reactor 002, add 1000 g of barium oxide to the 1500 L of N,N-dimethylacetamide in the reactor 002, and the reactor 002 The solution inside circulates and reacts in the circulation pipeline for 2.5 hours.

[0050] (2) Establish a circulation pipeline between the reaction kettle 002, the circulation pump 003 and the activated carbon column 005, and the so...

Embodiment 2

[0056] The present embodiment provides a kind of chromatographically pure N,N-dimethylacetamide, which adopts figure 1 Shown production system 100, and make according to following preparation method:

[0057] (1) Use industrial-grade N,N-dimethylacetamide as a raw material, transport it to the reaction kettle 002 through the raw material delivery pump 001, turn off the raw material delivery pump 001, start the reaction kettle 002 to stir, turn on the circulation pump 003, and establish the formation reaction In the circulation line between the bottom of the kettle 002, the circulation pump 003, the mixer 004 and the top of the reactor 002, add 100 g of barium oxide to the 500 L of N,N-dimethylacetamide in the reactor 002, and the reactor 002 The solution inside is circulated and reacted in the circulation pipeline for 3 hours.

[0058] (2) Establish a circulation pipeline between the reaction kettle 002, the circulation pump 003 and the activated carbon column 005, and the so...

Embodiment 3

[0064] The present embodiment provides a kind of chromatographically pure N,N-dimethylacetamide, which adopts figure 1 Shown production system 100, and make according to following preparation method:

[0065] (1) Use industrial-grade N,N-dimethylacetamide as a raw material, transport it to the reaction kettle 002 through the raw material delivery pump 001, turn off the raw material delivery pump 001, start the reaction kettle 002 to stir, turn on the circulation pump 003, and establish the formation reaction In the circulation line between the bottom of kettle 002, circulation pump 003, mixer 004 and the top of reactor 002, add 2000 g of barium oxide to 3000 L of N, N-dimethylacetamide in reactor 002, and reactor 002 The solution inside circulates and reacts in the circulation pipeline for 2 hours.

[0066] (2) Establish a circulation pipeline between the reaction kettle 002, the circulation pump 003 and the activated carbon column 005, and the solution in the reaction kettle...

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Abstract

The invention discloses chromatographically pure N,N-dimethylacetamide as well as a preparation method and a production system thereof, and relates to the technical field of purification of chemical products. The preparation method for the chromatographically pure N,N-dimethylacetamide comprises the following steps: first, adding barium oxide into raw materials for reacting; then, adsorbing via activated carbon; next, adsorbing via a 4A molecular sieve; finally, rectificating. The preparation method is low in production cost; the prepared chromatographically pure N,N-dimethylacetamide is high in quality and high in yield, and meets the requirements of a chromatographically pure reagent. The production system for the chromatographically pure N,N-dimethylacetamide comprises a reaction kettle, an activated carbon column, a 4A molecular sieve column, a fractionating tower and a finished product tank, wherein the reaction kettle is separately connected with the activated carbon column and the 4A molecular sieve column; the production system is specifically used for preparing the chromatographically pure N,N-dimethylacetamide and realizing large-scale industrial production of the chromatographically pure N,N-dimethylacetamide.

Description

technical field [0001] The invention relates to the technical field of purification of chemical products, and in particular to a chromatographically pure N,N-dimethylacetamide, a preparation method and a production system thereof. Background technique [0002] Chromatographically pure refers to the standard reagents or solvents used in chromatographic analysis. Its UV absorbance at low wavelengths is relatively low. Under chromatographic conditions, only peaks of specified compounds can appear, and impurity peaks cannot appear. The purity requirements are very high. In addition to the high requirements on the content of specified compounds, there are also high requirements on the content of impurities such as dust and water, which belong to the category of high-purity reagents. At present, the domestic chromatographic pure market is mostly monopolized by foreign reagent companies, such as Merck, Sigma, Fisher, Tedia, etc. The high prices of foreign reagent companies will lea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C233/05
CPCC07C231/24C07C233/05
Inventor 覃彩芹文胜郑根稳龚春丽赵正崇程凡董浩
Owner HUBEI ENG UNIV
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