A way of separating ethylene oxide from a mixture containing ethylene oxide

 

(57) Abstract:

Describes a way of separating ethylene oxide from a mixture containing ethylene oxide, comprising distilling the mixture in the column and the outlet of pure ethylene oxide in the liquid or gaseous state from the upper part of the column and through the side outlet located in the strengthening of the column, and the cubic product, while in case of violation of the operational mode for distillation serves a means of extinguishing, characterized in that the distillation is carried out in a column at an absolute pressure of from 2 to 10 bar and temperatures from 20 to 180oC, and the mixture passed through several successive zones with structured gaskets from sheet metal or layers of nozzles which are placed inside the column and of which at least one zone is connected to a source of water serving as miscible with ethylene oxide liquid extinguishing agents, and the means of extinguishing served in a zone or zones with increasing 0.01-4 bar operating pressure in the column, equal to 2-10 bar. 7 C.p. f-crystals, 1 Il.

The invention relates to the technology of production of ethylene oxide, in particular to a method for separation of ethylene oxide from a mixture containing an oxide of these is ay distillation initial mixture, allotment received the cubic product and distillate, condensing the distillate and recycling the condensate to the distillation, and the initial mixture, distillate, CBM product and recycled condensate is passed through outside the distillation column layers packings with a specific surface area 250-700 m2/m3and a height equal to 0.3 to 20 times the diameter of the distillation column, and in case of violation of the operating mode, to prevent hazardous situations for distillation serves inert gas as the extinguishing media from a source to which the distillation column is connected in height (see patent USSR 1118288, CL 07 D 303/04, 07.10.84 year).

The disadvantage of this method is the placement of layers of nozzles outside of the distillation column, connecting the source of extinguishing agents to the column and not to the layers of the nozzles, and the lack of regulation regarding violation of the operating mode.

The objective of the invention is to develop a way of separating ethylene oxide from a mixture containing ethylene oxide, which provides increased security process.

The problem is solved in the method of separation of ethylene oxide from a mixture containing ethylene oxide, including distillation ex is by and through the side outlet, located in the strengthening of the column, and the cubic product, while in case of violation of the operational mode for distillation serves a means of quenching due to the fact that the distillation is carried out in a column at an absolute pressure of from 2 to 10 bar and temperatures from 20 to 180oC, and the mixture passed through several successive zones with structured gaskets from sheet metal or layers of nozzles which are placed inside the column and of which at least one zone is connected to a source of water serving as miscible with ethylene oxide liquid extinguishing agents, and the means of extinguishing served in a zone or zones with increasing 0.01-4 bar operating pressure in the column, equal to 2-10 bar.

The original mix is mainly the result of the synthesis of ethylene oxide and along with ethylene oxide also contains residual water. Other components in this particular case can be, for example, ethylene glycol, oligoethyleneglycols, aldehydes, such as formaldehyde or acetaldehyde, or methane.

In addition, the proposed method allows the distillation of such mixtures, which along with the ethylene oxide is, for example, methanol, glycols, mono-,ordinary be directed at refining the initial mixture contains from 1 to 90 wt.%, preferably from 30 to 70 wt.% ethylene oxide and 90 to 10 weight. %, particularly preferably from 70 to 30 wt.% water. Additionally, the mixture may contain from 0 to 10 wt.%, preferably from 0 to 5 wt.% of ethylene glycol and from 0 to 10 wt.%, particularly preferably from 0 to 5 wt.% acetaldehyde. The sum of the contents of the components in the mixture is 100 weight%.

The proposed method is carried out in a distillation column of conventional design mainly from the strengthening part. For these purposes fit standard well-known distillation columns, for example, those described in Ullmann, "Encyclopedia of Industrial Chemistry", 5th ed., Tom B3, page 4-824-94 or "Klaus Sattler, Thermische Trennverfahren: Grundlagen, Auslegung, Apparate", publisher Chemie, 1988, pp. 25-27.

The data is well-known distillation columns modified to the needs of the proposed method, i.e., equipped with the above-mentioned areas and source water as a liquid extinguishing agents.

As nozzles are suitable, for example, the well-known metal and ceramic ring process, rings Pella or rings of Bialecka that perform the function of isolating material.

As appropriate structured strips of sheet metal are used so the UP>(Gebr. Sulzer, Winterthur, Switzerland) or Relapak. And are described, for example, in the above source "Encyclopedia of Industrial Chemistry" or the book "Packed Towers in Processing and Envirometal Technology", Reinhard billet, publisher Chemie, Weinheim, 1995, pp. 25-27.

Along with these zones distillation column is also conventional collectors and distributors.

The specific surface of one zone with structured gaskets from sheet metal or layers of nozzles, generally ranges from 100 to 1000 m2preferably from 125 to 750 m2respectively assigned to 1 m3zone.

Column for carrying out the method includes 2-20, preferably 3-15, in particular 4 to 8, and particularly preferably 4-6 zones with structured gaskets from sheet metal or layers of nozzles above specific surface area.

The height of individual zones ranges from 1 to 15 m, preferably from 3 to 8 m

According to a preferred variant of the invention, each area with strips of sheet metal or layers of nozzles connected to a source of extinguishing agents. This source, which is, as a rule, contains the means of extinguishing capacity, which also dopolnenie well-known measurement devices, regulation and control are connected with the column. According to a preferred variant of the invention, sources of extinguishing agents are the above mentioned areas, to use hydrostatic pressure extinguishing agents during the process of quenching.

For optimal distribution of extinguishing agents in the column you can use an ordinary available in the column collectors and distributors.

Used as extinguishing agents water may contain additives (e.g., antifreeze).

Explosive decomposition of gaseous ethylene oxide causes a tenfold increase in pressure compared to the original. In the case of the collapse of liquid ethylene oxide pressure can jump even more in the education released during the decomposition gases. When exceeding the operating pressure in the column on the above amount, preferably 0.1-2 bar, in particular 0.2-1 bar, particularly preferably about 0.5 bar when the extinguishing system. Then after 5-60 seconds, especially after 15 seconds means of extinguishing arrives in the above areas.

During decomposition, which occurs from the top down, the decomposition front moves b is shown characteristics, because this area is subjected to pre-washing by means of quenching and, therefore, the existing conditions do not allow further decomposition of ethylene oxide.

During the collapse, which moves up a clash decomposition front with front quenching, resulting in the process of extinction.

It is preferable to feed to the column while fighting such a quantity of water, which is able to provide in the area of fighting between the two zones above characteristics weight ratio of ethylene oxide : water 80:20, preferably 70:30.

According to a preferred variant of the invention the upper supply tank extinguishing media made with a larger volume than the remaining capacity. If the difference in volume will be approximately 1.5-2 times, guaranteed pass extinguishing media throughout the column, which further intensifies the process of extinguishing.

In the method according to the invention is carried out continuously supplied to the distillation of the initial mixture containing ethylene oxide, is fed to the column at a height of about component from 30 to 80%, preferably 50% of the height of the column, measured from the base of the column. Reflux the number of sostavlyaiete distillation is 10-180oWith, preferably 30-150oC.

Pure ethylene oxide away from the upper part of the column or the same as the lateral flow in the strengthening of the column.

The preferred option of the invention is that of pure ethylene oxide is discharged in a gaseous state from the upper part or in gaseous or liquid state as a side stream.

If you take away on a side line, located in the strengthening of the column, the easier the removal of low-boiling components, such as formaldehyde, from the upper part of the column.

When the distillation of a mixture of ethylene oxide and water drainage, as a rule, occurs in Cuba columns.

When the distillation of a mixture of ethylene oxide, water, and acetaldehyde pure ethylene oxide is removed from the upper part of the column, a mixture of acetaldehyde, ethylene oxide and water - as a side stream in its distant parts, and the water from the cube column.

When the distillation of a mixture of ethylene oxide, water, formaldehyde and acetaldehyde mixture of formaldehyde and ethylene oxide away from the upper part of the column, pure ethylene oxide as a side stream in the strengthening of the column, a mixture of acetaldehyde, ethylene oxide and water - as a side stream in a distant part of the column and vadami. For example, by distillation of a mixture of ethylene oxide and water can draw in the lower part of the column, in a distant part of the column or by heating the initial mixture. When distilling a mixture of ethylene oxide and water is the best heat to serve in distant parts of the column or by heating the initial mixture, because in the original water system ingento have the means of fighting, resisting decomposition of ethylene oxide.

According to a particularly preferred variant of the invention carry out the distillation in a column equipped with a jacket, and the space between the casing and the jacket is filled with inert gas such as carbon dioxide or nitrogen, preferably nitrogen. This event provides additional protection from external sources of ignition that can trigger an explosive decomposition of ethylene oxide.

The proposed method allows the continuous separation of ethylene oxide from a mixture containing ethylene oxide, while ensuring that the spontaneous decomposition of ethylene oxide immediately taken under control, preventing the destruction of distillers by an explosion. Purity ethylene oxide, obtained by the proposed method is very high udaetsya ethylene oxide, which contains not more than 30 ppm of acetaldehyde, and water not more than 60 parts per million.

Suitable for carrying out the method distillation column shown in the drawing, in which the positions have the following meanings:

1 - distillation column,

2 - zone structured gaskets from sheet metal or layers of nozzles,

3 - line filing of the original mixture,

4, a secondary cooling cycle,

5 - supply line to the cooling agent,

6 - line removal of the cooling agent,

7 - water supply line as extinguishing media,

8 - source extinguishing media,

9 - line feed pair,

10 - line exhaust side stream containing, for example, acetic aldehyde in a mixture of water and ethylene oxide,

11 - line removal of the cubic product, such as water,

12 - line removal of the target product, ethylene oxide,

13 - line flue gas,

14 - line nitrogen supply,

15 - the supply line of industrial water.

In addition, the distillation column is equipped with another not shown in the drawing shirt that protects the column 1 and the vessel 8 from the weather and external sources of ignition and serving to control the leak. Preemy the method is illustrated by the following example.

Example

The process is carried out in a large industrial plant for the production of ethylene oxide comprising presented on the drawing distillation column has an internal areas with structured gaskets from sheet metal with a specific surface area of 250 m2/m3, each of which is connected to the tank 8 to the external source of water as an extinguishing media, in which there is an atmosphere of inert gas, for example nitrogen. In distillation column operating at an absolute pressure of 3.4 bar, the temperature in the head part 46oWith and reflux 2:1, serves a mixture containing about 65 wt.% ethylene oxide, about 35 wt.% water and about 400 h/mill. aldehydes. From the upper part of the column divert pure ethylene oxide content of 10 h/mill. water and 20 h/mill. aldehydes and from a cube of water. In the lower part of the away side stream representing a mixture of ethylene oxide, water and aldehydes.

In case of exceeding the working pressure is about 0.5 bar will begin to operate the extinguishing system to prevent hazardous situations. In addition to the water in the column 1 may be supplied inert gas, for example nitrogen.

1. The way vydelenijami ethylene oxide in the liquid or gaseous state from the upper part of the column and through the side outlet, located in the strengthening of the column, and the cubic product, while in case of violation of the operational mode for distillation serves a means of extinguishing, characterized in that the distillation is carried out in a column at an absolute pressure of from 2 to 10 bar and temperatures from 20 to 180oC, and the mixture passed through several successive zones with structured gaskets from sheet metal or layers of nozzles which are placed inside the column and of which at least one zone is connected to a source of water serving as miscible with ethylene oxide liquid extinguishing agents, and the means of extinguishing served in a zone or zones with increasing 0.01-4 bar operating pressure in the column, equal to 2-10 bar.

2. The method according to p. 1, characterized in that the distillation is subjected to a mixture containing ethylene oxide and water.

3. The method according to p. 1, characterized in that the distillation is subjected to a mixture that contains 10-90 weight. % ethylene oxide and 90-10 weight. % of water.

4. The method according to p. 1, characterized in that the specific surface area of one zone with structured gaskets from sheet metal ranges from 100 to 1000 m21 m3zone.

5. The method according to p. 1, otlichny.

6. The method according to p. 1, characterized in that the distillation is carried out in a column in which there are several areas with structured gaskets from sheet metal.

7. The method according to p. 1, characterized in that the distillation is carried out in a column, which contains 2-20 areas with structured gaskets from sheet metal.

8. The method according to p. 1, characterized in that each zone with structured gaskets from sheet metal or layers of nozzles is connected to a separate source of liquid extinguishing agents.

 

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