阅读说明：本技术 一种高纯度二氯三乙醚的提纯加工方法 (Purification processing method of high-purity dichlorotriethanol ) 是由 瞿军 陆文辉 于 2020-12-11 设计创作，主要内容包括：本发明提供了一种高纯度二氯三乙醚的提纯加工方法,包括：离心过滤、一级初步蒸馏以及二级减压蒸馏等步骤。本发明提供了一种高纯度二氯三乙醚的提纯加工方法,减少二氯三乙醚中的杂质,降低了二氯三乙醚中水份的含量,从而有效提升二氯三乙醚浓度,增强了二氯三乙醚效果。(The invention provides a purification processing method of high-purity dichlorotriethanol, which comprises the following steps: centrifugal filtration, primary distillation, secondary reduced pressure distillation and the like. The invention provides a purification processing method of high-purity dichlorotriethanol, which reduces impurities in the dichlorotriethanol and reduces the content of water in the dichlorotriethanol, thereby effectively improving the concentration of the dichlorotriethanol and enhancing the effect of the dichlorotriethanol.)

1. The purification processing method of high-purity dichlorotriethanol is characterized by comprising the following steps:

(1) and centrifugal filtration: collecting crude dichlorotriethanol solution, pouring the dichlorotriethanol solution into a centrifuge, centrifuging and filtering to obtain supernatant

(2) Primary distillation: putting the supernatant obtained by centrifugal filtration into a first distillation tower, stirring the solution in the first distillation tower by using the rotation of a stirring shaft in the first distillation tower, and introducing hot oil heated in a hot oil heater into a hollow stirring shaft and a hollow jacket of the first distillation tower by using a rotary joint on the stirring shaft and the jacket of the first distillation tower to distill the solution in the first distillation tower to obtain a condensate;

(3) and secondary reduced pressure distillation: putting the condensate after the primary distillation into a secondary distillation tower, stirring the solution in the second distillation tower by the rotation of a stirring shaft in the second distillation tower, introducing hot oil output from an oil outlet end of the rotary joint on the stirring shaft of the first distillation tower into a rotary joint on the stirring shaft of the second distillation tower, introducing hot oil into a jacket of the first distillation tower into a jacket of the second distillation tower for distillation, starting a vacuum device during the distillation process, reducing the internal air pressure of the second distillation tower, carrying out reduced pressure distillation on the second distillation tower to obtain condensate, and condensing to obtain the high-purity triethyl dichlorohydrin solution.

2. The method as claimed in claim 1, wherein the rotation speed of the centrifuge in step (1) is 900-1100r/min, and the centrifugation time is 6-12 min.

3. The method as claimed in claim 1, wherein the heating in step (2) is performed by raising the temperature at 2-4 ℃ per minute, and the final heating temperature is maintained at 105-115 ℃.

4. The method for purifying dichlorotriethanol as claimed in claim 1, wherein the distillation time in step (2) is 1-2 h.

5. The method for purifying dichlorotriethanol as claimed in claim 1, wherein the heating in step (3) is carried out by raising the temperature by 2-4 ℃ per minute and the final heating temperature is maintained at 50-60 ℃.

6. The method of claim 1, wherein the pressure in the first distillation column in step (3) is controlled to be 10 to 86 kpa.

7. The method for purifying dichlorotriethanol as claimed in claim 1, wherein the distillation time in step (3) is 1-2 h.

Technical Field

The invention mainly relates to the technical field of purification of dichlorotriether, in particular to a purification processing method of high-purity dichlorotriether.

Background

Dichlorotriethanol is a chemical substance with the formula C6H12CL2O2, often obtained from the reaction between diethylene glycol and thionyl chloride.

According to the method for purifying o-diethyl ether provided in patent document CN201410808194.8, the product is obtained by taking catechol and sodium hydroxide solution as reactants, ethyl chloride or ethyl bromide as etherifying agents, ethanol as a solvent, reacting in an autoclave to obtain a crude o-diethyl ether product, using water as a solvent, adding water into a reaction kettle, adding the crude o-diethyl ether product under stirring, heating until the o-diethyl ether is completely melted, dropwise adding hydrochloric acid into the reaction kettle under sufficient stirring, dissolving part of impurities in the crude o-diethyl ether product in water to form an aqueous solution layer, a non-water-soluble flocculent impurity layer and an o-diethyl ether layer from bottom to top, and separating out the o-diethyl ether to obtain a pure product with the purity of not less than 99% and the water content of not more than 0.5%. The method uses clean, environment-friendly and low-price water to replace the traditional organic solvent, not only saves the cost and is environment-friendly, but also has simple purification method and high yield in the purification process, and the o-diethyl ether obtained by purification has high purity and low water content and better meets the export requirement.

However, the above-mentioned ether purification method has drawbacks, for example, although the above-mentioned purification method can improve the yield in the purification process, the conventional purification method usually adopts a precipitation method or a distillation method, the precipitation method is simple in operation, but it takes a long time and is inefficient, and the distillation method can reduce the impurities in the crude solution of dichlorotriethylether but does not reduce the water content in the solution.

Disclosure of Invention

The invention mainly provides a purification processing method of high-purity dichlorotriethanol, which is used for solving the technical problems in the background technology.

The technical scheme adopted by the invention for solving the technical problems is as follows:

a purification processing method of high-purity dichlorotriethanol comprises the following steps:

(1) and centrifugal filtration: collecting crude dichlorotriethanol solution, pouring the dichlorotriethanol solution into a centrifuge, centrifuging and filtering to obtain supernatant

(2) Primary distillation: putting the supernatant obtained by centrifugal filtration into a first distillation tower, stirring the solution in the first distillation tower by the rotation of a stirring shaft in the first distillation tower, standing for 1h, introducing heated hot oil into a hot oil heater through a rotary joint on the stirring shaft and a first distillation tower jacket, and distilling the solution in the first distillation tower to obtain a condensate;

(3) and secondary reduced pressure distillation: putting the condensate after the primary distillation into a secondary distillation tower, stirring the solution in the second distillation tower by the rotation of a stirring shaft in the second distillation tower, introducing hot oil output from an oil outlet end of the rotary joint on the stirring shaft of the first distillation tower into a rotary joint on the stirring shaft of the second distillation tower, introducing hot oil into a jacket of the first distillation tower into a jacket of the second distillation tower for distillation, starting a vacuum device during the distillation process, reducing the internal air pressure of the second distillation tower, carrying out reduced pressure distillation on the second distillation tower to obtain condensate, and condensing to obtain the high-purity triethyl dichlorohydrin solution.

Further, the rotation speed of the centrifuge in the step (1) is 900-.

Further, the heating method adopted in the step (2) is to raise the temperature by 2-4 ℃ per minute, and the final heating temperature is kept at 105-115 ℃.

Further, the distillation time in the step (2) is 1-2 h.

Further, the heating mode adopted in the step (3) is that the temperature is raised by 2-4 ℃ per minute, and the final heating temperature is kept at 50-60 ℃.

Further, the pressure in the first distillation column in the step (3) is controlled to be 10 to 86 kpa.

Further, the distillation time in the step (3) is 1-2 h.

Compared with the prior art, the invention has the beneficial effects that:

firstly, the invention firstly adopts a centrifuge to carry out centrifugal filtration on the crude dichlorotriether ether solution, thereby effectively removing impurities in the crude dichlorotriether ether solution, leading the dichlorotriether ether solution to be relatively clear and reducing the subsequent impurity removal time.

Secondly, the distillation method of the dichlorotriethanol solution adopts a distillation mode of firstly reducing the pressure after the normal pressure, thereby avoiding the gasification of low boiling point substances in the first distillation tower and the increase of the pressure, possibly causing the explosion of a reduced pressure distillation tower, simultaneously preventing the cracking of effective substances in the dichlorotriethanol solution, and further improving the quality of the finally obtained high-purity dichlorotriethanol solution.

Thirdly, the external jacket and the internal stirring shaft of the first distillation tower and the second distillation tower are simultaneously heated, so that the solution in the first distillation tower and the solution in the second distillation tower are fully contacted with a heat source, and the heating efficiency is improved.

The present invention will be explained in detail below with reference to the drawings and specific embodiments.

Drawings

FIG. 1 is a schematic structural view of the present invention;

in the figure: 1. a centrifuge; 2. a first distillation column; 3. a hot oil heater; 4. a secondary distillation column; 5. a vacuum device.

Detailed Description

In order to facilitate an understanding of the invention, the invention will now be described more fully hereinafter with reference to the accompanying drawings, in which several embodiments of the invention are shown, but which may be embodied in different forms and not limited to the embodiments described herein, but which are provided so as to provide a more thorough and complete disclosure of the invention.

It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may be present, and when an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present, as the terms "vertical", "horizontal", "left", "right" and the like are used herein for descriptive purposes only.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, and the knowledge of the terms used herein in the specification of the present invention is for the purpose of describing particular embodiments and is not intended to limit the present invention, and the term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.

Examples are given.

Example 1

A purification processing method of high-purity dichlorotriethanol comprises the following steps:

(1) and centrifugal filtration: collecting crude dichlorotriethanol solution, pouring the dichlorotriethanol solution into a centrifuge, centrifuging and filtering to obtain supernatant

(2) Primary distillation: putting the supernatant obtained by centrifugal filtration into a first distillation tower, stirring the solution in the first distillation tower by the rotation of a stirring shaft in the first distillation tower, standing for 1h, introducing heated hot oil into a hot oil heater through a rotary joint on the stirring shaft and a first distillation tower jacket, and distilling the solution in the first distillation tower to obtain a condensate;

(3) and secondary reduced pressure distillation: putting the condensate after the primary distillation into a secondary distillation tower, stirring the solution in the second distillation tower by the rotation of a stirring shaft in the second distillation tower, introducing hot oil output from an oil outlet end of the rotary joint on the stirring shaft of the first distillation tower into a rotary joint on the stirring shaft of the second distillation tower, introducing hot oil into a jacket of the first distillation tower into a jacket of the second distillation tower for distillation, starting a vacuum device during the distillation process, reducing the internal air pressure of the second distillation tower, carrying out reduced pressure distillation on the second distillation tower to obtain condensate, and condensing to obtain the high-purity triethyl dichlorohydrin solution.

The rotating speed of the centrifuge in the step (1) is 900-.

The heating mode adopted in the step (2) is to raise the temperature by 2-4 ℃ per minute, and the final heating temperature is kept at 105-115 ℃.

The distillation time in the step (2) is 1-2 h.

The heating mode adopted in the step (3) is to heat up 2-4 ℃ per minute, and the final heating temperature is kept at 50-60 ℃.

The pressure in the first distillation column in the step (3) is controlled to be 10 to 86 kpa.

The distillation time in the step (3) is 1-2 h.

The water content of the obtained dichlorotriethanol solution was detected to be 0.1%.

Example 2

A purification processing method of high-purity dichlorotriethanol comprises the following steps:

(1) and centrifugal filtration: collecting crude dichlorotriethanol solution, pouring the dichlorotriethanol solution into a centrifuge, centrifuging and filtering to obtain supernatant

(2) Primary distillation: putting the supernatant obtained by centrifugal filtration into a first distillation tower, stirring the solution in the first distillation tower by the rotation of a stirring shaft in the first distillation tower, standing for 1.5 hours, introducing heated hot oil into a hot oil heater through a rotary joint on the stirring shaft and a first distillation tower jacket, and distilling the solution in the first distillation tower to obtain a condensate;

(3) and secondary reduced pressure distillation: putting the condensate after the primary distillation into a secondary distillation tower, stirring the solution in the second distillation tower by the rotation of a stirring shaft in the second distillation tower, introducing hot oil output from an oil outlet end of the rotary joint on the stirring shaft of the first distillation tower into a rotary joint on the stirring shaft of the second distillation tower, introducing hot oil into a jacket of the first distillation tower into a jacket of the second distillation tower for distillation, starting a vacuum device during the distillation process, reducing the internal air pressure of the second distillation tower, carrying out reduced pressure distillation on the second distillation tower to obtain condensate, and condensing to obtain the high-purity triethyl dichlorohydrin solution.

The rotating speed of the centrifuge in the step (1) is 900-.

The heating mode adopted in the step (2) is to raise the temperature by 2-4 ℃ per minute, and the final heating temperature is kept at 105-115 ℃.

The distillation time in the step (2) is 1-2 h.

The heating mode adopted in the step (3) is to heat up 2-4 ℃ per minute, and the final heating temperature is kept at 50-60 ℃.

The pressure in the first distillation column in the step (3) is controlled to be 10 to 86 kpa.

The distillation time in the step (3) is 1-2 h.

The water content of the obtained dichlorotriethanol solution was detected to be 0.08%.

Example 3

A purification processing method of high-purity dichlorotriethanol comprises the following steps:

(1) and centrifugal filtration: collecting crude dichlorotriethanol solution, pouring the dichlorotriethanol solution into a centrifuge, centrifuging and filtering to obtain supernatant

(2) Primary distillation: putting the supernatant obtained by centrifugal filtration into a first distillation tower, stirring the solution in the first distillation tower by the rotation of a stirring shaft in the first distillation tower, standing for 2 hours, introducing heated hot oil into a hot oil heater through a rotary joint on the stirring shaft and a first distillation tower jacket, and distilling the solution in the first distillation tower to obtain a condensate;

(3) and secondary reduced pressure distillation: putting the condensate after the primary distillation into a secondary distillation tower, stirring the solution in the second distillation tower by the rotation of a stirring shaft in the second distillation tower, introducing hot oil output from an oil outlet end of the rotary joint on the stirring shaft of the first distillation tower into a rotary joint on the stirring shaft of the second distillation tower, introducing hot oil into a jacket of the first distillation tower into a jacket of the second distillation tower for distillation, starting a vacuum device during the distillation process, reducing the internal air pressure of the second distillation tower, carrying out reduced pressure distillation on the second distillation tower to obtain condensate, and condensing to obtain the high-purity triethyl dichlorohydrin solution.

The rotating speed of the centrifuge in the step (1) is 900-.

The heating mode adopted in the step (2) is to raise the temperature by 2-4 ℃ per minute, and the final heating temperature is kept at 105-115 ℃.

The distillation time in the step (2) is 1-2 h.

The heating mode adopted in the step (3) is to heat up 2-4 ℃ per minute, and the final heating temperature is kept at 50-60 ℃.

The pressure in the first distillation column in the step (3) is controlled to be 10 to 86 kpa.

The distillation time in the step (3) is 1-2 h.

The water content of the obtained dichlorotriethanol solution was measured to be 0.12%.

The specific operation mode of the invention is as follows:

firstly, collecting crude dichlorotriethanol solution, pouring the dichlorotriethanol solution into a centrifuge, carrying out centrifugal filtration to obtain supernatant, then placing the supernatant obtained by centrifugal filtration into a first distillation tower, stirring the solution in the tower by using the rotation of a stirring shaft in the first distillation tower, standing for 2 hours, introducing heated hot oil into a hollow stirring shaft and a jacket through a rotary joint on the stirring shaft and the first distillation tower jacket in a hot oil heater, distilling the solution in the first distillation tower to obtain condensate, finally placing the condensate subjected to primary distillation into a second distillation tower, stirring the solution in the tower by using the rotation of the stirring shaft in the second distillation tower, simultaneously introducing the hot oil output from an oil outlet end of the rotary joint on the stirring shaft of the first distillation tower into the rotary joint on the stirring shaft of the second distillation tower, introducing the hot oil into the first distillation tower jacket for distillation through the second distillation tower jacket, in the process, the vacuum device is started to reduce the internal air pressure of the second distillation tower, so that the second distillation tower carries out reduced pressure distillation to obtain condensate, and the condensate is condensed to obtain the high-purity dichlorotriethyl ether solution.

The invention is described above with reference to the accompanying drawings, it is obvious that the invention is not limited to the above-described embodiments, and it is within the scope of the invention to adopt such insubstantial modifications of the inventive method concept and solution, or to apply the inventive concept and solution directly to other applications without modification.