JPS5899111A - Method and device for refining of carbon disulfide - Google Patents

Abstract

PURPOSE:To produce refined carbon disulfide with good energy efficiency by treating crude gaseous carbon disulfide contg. sulfur by using a special free sulfur separator, an activated carbon adsorption tower, and a gas-liquid contact type hydrogen sulfide removing tower. CONSTITUTION:In a fan or blade type separator 3, the free sulfur on the crude gaseous carbon disulfide introduced through a pipe 1 is removed (a symbol 3 is a receiver for sulfur), then the gas is introduced into an activated carbon adsorption tower 4 where the gaseous sulfur and a trace of remaining free sulfur are removed. Thereafter, the gas is fed into a hydrogen sulfide removing tower 7 (a symbol 7' is an introducing port) provided with packed layers 9, 9' and a heating means 10 and is brought into contact with the liquid carbon disulfide which is sprayed from a dropping means 8 to condense and liquefy the gas. The liquefied gas is discharged as refined carbon disulfide through a pipe 11. On the other hand, hydrogen sulfide and part of carbon desulfide vapor are fed from the tower top 12 to a cooler 13, where only the carbon disulfide is liquefied. The liquefied carbon disulfide is fed through a pipe 15 and a pump 16 to a dropping device 8, and the hydrogen sulfide is discharged to the outside of the system.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method and apparatus for purifying carbon disulfide.

Conventionally, a carbon source and sulfur were reacted at high temperature, and the entire amount of crude carbon disulfide gas emitted from the reactor was condensed in a cooler to obtain crude carbon disulfide, which was used, for example, in Utility Model Publication No. 1837-17.
Using a distillation column such as that disclosed in No. 553, dissolved sulfur or hydrogen sulfide, carbonyl sulfide (CO
It is common to obtain purified carbon disulfide by removing gases such as S). However, by condensing the entire amount and distilling the entire amount in this manner, a large amount of thermal energy is consumed even if some thermal energy is recovered by electric heat exchange or the like.

The main component of refining crude carbon disulfide is to achieve an evaporation residue of 0.007% or less (Japanese Industrial Standards), and removal of sulfur content is the most important. As a result of intensive studies on this problem, the inventors of the present invention have found that the removal of sulfur contained in crude carbon disulfide can be carried out extremely efficiently using a fan or blade type separator and activated carbon adsorption. It was discovered that carbon sulfide and water sulfide can be effectively separated using a reaction column with a lid, and the present invention is brought to fruition.

That is, in the purification of crude carbon disulfide containing sulfur, the present invention extracts free sulfur from bulk gas from disulfide coal,
Next, the crude carbon disulfide gas is brought into contact with activated carbon to adsorb and remove remaining free sulfur and gaseous sulfur, and the crude carbon disulfide gas is further brought into contact with liquid carbon disulfide to condense and liquefy and form one condensed wave. This is a carbon disulfide cassava method characterized by bringing crude carbon disulfide into contact with carbon disulfide vapor to release dissolved hydrogen sulfide.

Additionally, the present invention includes a fan or grade cap free sulfur separator, an activated carbon adsorption tower, and a gas-liquid contact layer for desulfurization.
The desulfurizing ice tower has an inlet for crude carbon disulfide gas from which free sulfur and gaseous sulfur have been removed in the middle stage, and an inlet in the upper stage K11.
Provided is a carbon disulfide purification device, characterized in that it has a dripping device for carbon disulfide and a hydrogen sulfide slope outlet, and further has a droplet for liquid carbon disulfide and a heating means for generating gas at the lower stage. do.

In the present invention, crude disulfide #l! ! The cable contains sulfur and sulfide water as impurities, and these must be removed. Looking at these impurities, sulfur has a lot of free particulates and gaseous ones, and hydrogen sulfide has a lot of gaseous ones, so it is necessary to efficiently remove free particulates and gaseous impurities.

First, as a result of studying the separation of free sulfur, we found that free sulfur can be efficiently separated from crude disulfide leg bulk gas using a fan or blade type separator.9 The separator can be used in one or multiple stages as required. do it.

Crude carbon disulfide from which free sulfur has been removed contains mold, a quantity of free sulfur, and gaseous sulfur, which must be removed. Activated carbon is extremely effective in removing these sulfur contents. Other adsorbents do not have sufficient adsorption capacity, and if adsorption is performed immediately on activated carbon without using the fan or blade separator mentioned above, free sulfur will cover the activated carbon and lose its adsorption capacity. Separation of free sulfur must be carried out before the removal of free and gaseous sulfur by activated carbon to the required level. The activated carbon used here may be one that is normally commercially available, and can be desorbed and reused by a conventional method.

For activated charcoal! The P-adsorbed crude carbon disulfide gas contains sulfide water, which must be extracted. The present inventors have developed a new method for removing hydrogen sulfide. That is, to separate hydrogen sulfide from the bulk gas of carbon disulfide and sulfide water, first, the warm gas K11 carbon disulfide is brought into contact with each other, the carbon disulfide gas is condensed and liquefied, and hydrogen sulfide, which is difficult to liquefy, is separated. . When liquefied carbon disulfide contains a small amount of dissolved sulfide water, it is preferable to remove it even further. For this purpose, carbon disulfide gas is supplied to the cased nine disulfide coal, and when it is brought into contact with liquefied carbon disulfide and heat is applied, dissolved hydrogen sulfide is expelled by K. As will be described later, the carbon disulfide contained in the 16NiK layer can be used by partially heating the carbon disulfide product, but it can also be supplied from a separate supply line.

Through this process, carbon disulfide is reduced to the required level of impurities. Sulfur and sulfide water can also be recovered and reused.

The first [t;i] is one example of an apparatus for carrying out the present invention, and will be described below.

The crude carbon disulfide gas produced by reacting the carbon source and sulfur at high temperature is passed through a cyclone, etc. to reversibly separate powder, sulfur particles, etc., and then passed through a pipe IK to a 7-inch or blade-type separator. sent to. The nine sulfur collected in separator 2 is transferred to receiver 3.
K]l) served. The carbon nine disulfide gas from which free sulfur has been almost completely removed by the separator 2 is then introduced into the activated carbon adsorption tower 4. The activated carbon adsorption tower 4 can be provided with a hopper 5 for supplying active carbon and an activated carbon discharge device 6, as is known in the art. Activated carbon adsorbs and removes trace amounts of remaining free sulfur and gaseous sulfur.

Impurities that are not adsorbed, such as hydrogen sulfide and carbonyl sulfide, remain in the crude disulfide coal gas that has passed through the adsorption tower. The gas is then introduced into the middle inlet of the desulfurizing water bulk tower 7? 'Sent to. The inside of the desulfurizing hydrogen group has a liquid carbon disulfide dropping device 8 on its upper stage, from which the casing carbon disulfide is dropped in a shower or spray state. 'The nine fox carbon disulfide gas is introduced into the tower and comes into contact with it, and the gas is condensed and liquefied. Therefore, it is desirable to provide a round packed bed 9 in the tower to promote gas-liquid contact.The lower stage of the tower is used to stir liquid carbon disulfide droplets, and the lower stage is equipped with heating means 1G for steam generation. have The carbon disulfide accumulated in the liquid reservoir is heated by the heating means 10 to develop and generate the necessary carbon disulfide vapor. This vapor is used as M4-supplied carbon disulfide vapor. It is also possible to provide a heating means of 4 km outside the apparatus shown in FIG. 1 and have an independent structure so that carbon disulfide vapor can be supplied into the column. The supplied carbon disulfide vapor is brought into contact with liquid carbon disulfide dripping or flowing down from the top of the tower. It is desirable to install a packed bed 91 for gas-liquid contact in the column inside the column. In the packed bed 91, condensed and liquefied carbon disulfide and carbon disulfide vapor come into contact and heat the liquid carbon disulfide to drive out dissolved hydrogen sulfide and the like.

In this way, the carbon disulfide stored in the droplets can be of high purity. The carbon disulfide is discharged as a product through a pipe 11. On the other hand, hydrogen sulfide and some carbon nitride vapor are taken out from the top 12 of the desulfurization water bulk tower 70, which is cooled by a cooling device 13, and only the carbon disulfide with a high boiling point is liquefied, and the vibrator 15 and pump 16 are Then, it is circulated to the above-mentioned disulfide caster dripping device 8. It is preferable that the liquid carbon disulfide in this line is not used as a product. Hydrogen sulfide and the like that are not liquefied are removed from the cooling device 13.

As described above, carbon disulfide can be purified according to the present invention with low energy consumption, and its industrial value is highly desirable.

This will be explained below using examples.

In the apparatus shown in Fig. 1, approximately 1 ton of activated carbon (2 liters of 4G carbon) is placed in an activated carbon adsorption tower with a capacity of 2.4 kg.
As a result of operation, the reactor was filled with Rikien (trade name), and a cooler with a capacity of 15 dehydrogen sulfide groups and a cooling section surface film 33d was installed, and 48 G of carbon disulfide was obtained per hour. The required amount of heat is the same as the conventional one, and the evaporation residue in the product carbon disulfide is o,ooos ~ 0.0020'/C8x 100t, and hydrogen sulfide is not detected.

The circulating amount of activated carbon is 20 times a day.-1) Friends.

[Brief explanation of drawings]

Iris is a schematic diagram showing an example of an apparatus for carrying out the present invention. Patent applicant: Kuraray Chemical Co., Ltd. Representative: Patent attorney Tate Honda

Claims (1)

[Claims] (1) In purification 11 of crude carbon disulfide containing sulfur, free sulfur is removed from the carbon disulfide gas. Next, the crude carbon disulfide gas is brought into contact with activated carbon to adsorb and remove remaining free sulfur and gaseous sulfur, and the crude silicon disulfide gas is further brought into contact with liquid carbon disulfide to condense and liquefy, as well as condensation and liquefaction. 9. A method for purifying carbon disulfide, which comprises bringing crude carbon disulfide into contact with carbon disulfide vapor to extract dissolved carbon sulfide. @ 7 or more blades installed free sulfur separator, active member mold deposition tower, gas-liquid contact lid desulfurization tower), the wrinkle desulfurization tower removes free sulfur and gaseous sulfur in the middle stage. Top 1 with an inlet for carbon disulfide gas! 1. A carbon disulfide refining apparatus, comprising a wave body carbon disulfide dropping device and a hydrogen sulfide outlet, and further comprising a liquid carbon disulfide outlet and a heating means for generating steam in the lower stage.