CN105693461A

CN105693461A - Preparation method of chromatographic grade dichloromethane

Info

Publication number: CN105693461A
Application number: CN201410692734.0A
Authority: CN
Inventors: 陈曙; 王家濬
Original assignee: Tianjin Kermel Chemical Reagent Co Ltd
Current assignee: Tianjin Kermel Chemical Reagent Co Ltd
Priority date: 2014-11-26
Filing date: 2014-11-26
Publication date: 2016-06-22

Abstract

The invention provides a preparation method of chromatographic grade dichloromethane. The method concretely comprises the following steps: 1, taking fruit shell active carbon DV11, drying and dehydrating the fruit shell active carbon DV11, cooling the dried and dehydrated fruit shell active carbon DV11, and filling a glass column with the cooled fruit shell active carbon DV11; and 2, allowing industrial grade dichloromethane to go through the glass column from top to bottom to carry out column chromatography adsorption treatment in order to obtain the chromatographic grade dichloromethane. The method has the advantages of high purity of the chromatographic grade dichloromethane, simple and reasonable process, high qualified rate of the above product, and suitableness for needs of large-scale industrial production.

Description

A kind of preparation method of chromatographic grade dichloromethane

Technical field

The preparation method that the present invention relates to a kind of chemical reagent, the preparation method of especially a kind of chromatographic grade dichloromethane。

Background technology

Dichloromethane (CH₂Cl₂) it is non-combustible low boiling point solvent, except for organic synthesis, it is also widely used as cellulose acetate film forming, Triafol T reels off raw silk from cocoons, oil dewaxing, aerosol and antibiotic, vitamin, steroid produce in solvent, and metal surface enamelled coating cleaning and degreasing and remover；For the refrigeration of fumigation of grain and low-pressure refrigeration machine and air-conditioning device, in polyether-type urethane foams produces, it is used as auxiliary blowing agent, and is used as the foaming agent of extruding polysulfones type foam plastics；As solvent, extractant, mutagenic agent, study for plant genetic；There is good dissolving power, it it is conventional industrial solvent poisonings low boiling point solvent little, non-flame properties, a lot of resins, paraffin and fat all had good solvability, it is mainly used as in paint stripper, oil dewaxing solvent, the extractant of determination system of thermal unstable material, Pilus Caprae seu Ovis and extracts lanoline and from Cortex cocois radicis, extract the solvent of the extractant of edible oil, tri acetic acid fiber ester cinematographic film, be also widely used in acetate fiber, the manufacture of vinyl chloride fibers, processing and extinguishing chemical, cryogen, hexamethylenamine etc. and manufacture；For electronics industry, it is commonly used for cleaning degreaser；Owing to boiling point is extremely low, it is the solvent of flame retardancy and is widely used, except the cleaning solvent making aero-engine, precision optical machinery etc., also can make the remover of coating, yet suitably can mix with other solvents, for various industrial washings；Also serve as setilose solvent, dentistry local anesthetic, cryogen and extinguishing chemical etc., be the common solvent of the conventional eluant of chromatography and extract and separate；Solvent as resin and plastics industry。The production method of present stage dichloromethane is more, but highly purified realization is comparatively difficult, and therefore, the new technology finding a kind of preparative hplc level dichloromethane has highly important production practices meaning。

Summary of the invention

The technical problem to be solved is in that the preparation method providing a kind of chromatographic grade dichloromethane。

For solving above-mentioned technical problem, the technical scheme is that

A kind of preparation method of chromatographic grade dichloromethane, concrete preparation process is as follows:

(1), after taking active fruit shell carbon DV11 drying and dehydrating and cooling down, load in glass column；

(2) from top to bottom through glass column, technical grade dichloromethane is done Adsorption to process, obtain chromatographic grade dichloromethane。

Preferably, the preparation method of above-mentioned chromatographic grade dichloromethane, in described step (1), active fruit shell carbon DV11 is purchased from brilliance timber mill, Beijing。

Preferably, the preparation method of above-mentioned chromatographic grade dichloromethane, in described step (1), drying and dehydrating is to adopt centrifugation to be dried in drying oven after carrying out dehydration, and baking temperature is 120 130 DEG C。

The invention has the beneficial effects as follows:

The preparation method of above-mentioned chromatographic grade dichloromethane, gained chromatographic grade dichloromethane purity is high, technique advantages of simple, and conforming product rate is high, is suitable for the needs that large-scale industrial produces。

Detailed description of the invention

Below in conjunction with specific embodiment, technical scheme of the present invention is further described。

Embodiment 1

(1) taking after active fruit shell carbon DV11 (purchased from brilliance timber mill, Beijing) carries out dehydration by centrifugation and be dried in drying oven, baking temperature is 125 DEG C, is loaded in glass column by the active fruit shell carbon DV11 after drying and dehydrating cooling；

Embodiment 2

(1) taking after active fruit shell carbon DV11 (purchased from brilliance timber mill, Beijing) carries out dehydration by centrifugation and be dried in drying oven, baking temperature is 120 DEG C, is loaded in glass column by the active fruit shell carbon DV11 after drying and dehydrating cooling；

Embodiment 3

(1) taking after active fruit shell carbon DV11 (purchased from brilliance timber mill, Beijing) carries out dehydration by centrifugation and be dried in drying oven, baking temperature is 130 DEG C, is loaded in glass column by the active fruit shell carbon DV11 after drying and dehydrating cooling；

Embodiment 4

(1) taking after active fruit shell carbon DV11 (purchased from brilliance timber mill, Beijing) carries out dehydration by centrifugation and be dried in drying oven, baking temperature is 127 DEG C, is loaded in glass column by the active fruit shell carbon DV11 after drying and dehydrating cooling；

In above-described embodiment 1-4, raw material is meet AR raw material in industrial goods, and after long-term storage and filtration experiment, content 99.5% → 98.7%, free chlorine >=0.0005% acidity >=0.05% outward appearance shoals Huang；

Detection foundation is company standard Q/12HB4234-2009 content >=99.8% acidity≤0.03mmol/100g (in H+) free chlorine≤0.0001%；

Absorbance standard 240nm≤0.30,245nm≤0.15,260nm≤0.05；

Four embodiments feed intake and detects data result in Table 1。

Table 1

The above-mentioned detailed description preparation method of this kind of chromatographic grade dichloromethane carried out with reference to embodiment; it is illustrative rather than determinate; can according to restriction scope list several embodiments; therefore without departing from changing and modifications under present general inventive concept, should belong within protection scope of the present invention。

Claims

1. the preparation method of a chromatographic grade dichloromethane, it is characterised in that: concrete preparation process is as follows:

2. the preparation method of chromatographic grade dichloromethane according to claim 1, it is characterised in that: in described step (1), active fruit shell carbon DV11 is purchased from brilliance timber mill, Beijing。

3. the preparation method of chromatographic grade dichloromethane according to claim 1, it is characterised in that: in described step (1), drying and dehydrating is to adopt centrifugation to be dried in drying oven after carrying out dehydration, and baking temperature is 120 130 DEG C。