KR20100040467A - A method for recovering organic compounds in ammonium lequor - Google Patents

Abstract

PURPOSE: A method for recovering organic compounds in ammonia liquor is provided to prevent facilities from being broken due to the organic compounds, to easily refine coke oven gas, and to prevent the closure of a process piping and a distillation tower due to the organic compounds. CONSTITUTION: A method for recovering organic compounds in ammonia liquor comprises the following steps: preparing a filtered ammonia liquor by filtering the ammonia liquor; mixing the filter ammonia liquor with a solvent; dissolving the organic compounds, which is contained in the ammonia liquor, in a solvent; extracting the organic compounds which is dissolved in the solvent; distilling the extracted organic compounds; crystallizing a residue remaining in the distillation step by cooling the residue; and collecting the organic compounds by filtering a crystal which is generated in the crystallization step.

Description

A method for recovering organic compounds in ammonium lequor

The present invention relates to a method for recovering organic compounds contained in ordination, and in particular, to efficiently recover benzene, toluene, xylene, naphthalene and various benzene ring type organic compounds contained in ordination (ammonia water) generated in the process of producing coke. The present invention relates to a method for recovering an organic compound contained in ordination so as to prevent closure of the process piping or distillation column by the organic compound in advance and to increase the efficiency of the process.

Generally, coke oven gas (COG; coke oven gas), tar, and water are generated during the coking process using coal, and the tar and water of the product are recovered in a liquid state, and the gaseous coke Oven gas is collected and used as an energy source in steel mills.

The water contains various compounds produced by chemical reactions during the dry distillation process, and is particularly referred to as ordination because it contains a large amount of ammonia.

Meanwhile, the coke oven gas contains some carbon dioxide, sulfur dioxide, and inflow oxygen, which are not utilized as fuels, thereby reducing the amount of heat generated by increasing the volume of the coke oven gas, and being released into the atmosphere, which is caused by air pollution and sulfur dioxide caused by sulfur dioxide. Coke oven gas is subjected to a purification process in order to cause a warming phenomenon, and to solve the above problems.

Benzene, toluene, xylene, naphthalene and various benzene ring type organic compounds exist in the ordination of the chemical by-product plant used for the coke oven gas purification, and conventionally, only some of the organic compounds contained in ordination are present. The method of removing coke oven gas was selected by using a filter. However, in the use of such ordination, benzene, toluene, xylene, and naphthalene are vaporized or sublimed among remaining organic compounds. It is attached to cause a closure, thereby making the normal operation of the equipment difficult to reduce the efficiency of the process, there was a problem that causes the failure of the equipment.

The present invention has been made in view of the problems of the prior art as described above, an object of the present invention is to provide a method for recovering the organic compound contained in the ordination to prevent the closing of the process piping or distillation column by the organic compound in advance. There is.

Another object of the present invention is to solve the problem of equipment failure by the recovery of organic compounds, improve the efficiency of the process, and to provide a method for recovering the organic compounds contained in the ordinal water can be easily purified coke oven gas There is.

It is still another object of the present invention to provide a method for recovering organic compounds contained in ordination, which can be economically obtained by selling recovered organic components and naphthalene as by-products.

The object of the present invention as described above (a) preparing the filtered eye by the ordination supplied through the first and second filtration; (b) mixing the filtration eye and a solvent to dissolve an organic compound contained in the filtration eye in the solvent; (c) extracting the organic compound dissolved in the solvent; (d) distilling the organic compound extracted by the solvent; (e) cooling and crystallizing the residues remaining in the distillation step; (f) is achieved by a method for recovering organic compounds contained in ordination comprising filtering the crystals produced in the crystallization step to recover organic compounds.

Preferably, the solvent in the organic compound dissolving step in the present invention is characterized in that to use quinoline and kerosene, respectively or in the same proportion to each other.

In addition, the solvent in the organic compound dissolving step in the present invention, it characterized in that it contains 3.5% by volume or more based on the filtered ordination.

In addition, the distillation temperature in the organic compound distillation step in the present invention, characterized in that more than 120 ℃ temperature.

According to the present invention described above, by efficiently recovering the organic compound containing naphthalene contained in the ordination generated in the process for producing coke, it is possible to prevent the closing of the process piping or distillation column by the organic compound in advance.

In addition, the problem of equipment failure is solved in advance by the recovery of the organic compound, the efficiency of the process is improved, and the coke oven gas is easily purified, while the recovered organic components and naphthalene are sold as by-products and are economical. You can benefit.

Hereinafter, with reference to the accompanying drawings will be described in detail the configuration and effect of the preferred embodiment of the present invention.

1 is a schematic diagram illustrating a method for recovering an organic compound contained in the ordination according to the present invention, Figure 2 is a graph showing a preferred amount of solvent in the method for recovering the organic compound contained in the ordination according to the present invention. 3 is a graph showing a preferred distillation temperature in the method for recovering the organic compound contained in the ordination according to the present invention.

In addition, Figure 4 is a flow chart of a method for recovering the organic compound contained in the ordination according to the present invention, referring to Figures 1 and 4, first filtered to remove the solid particles in the supplied ordination, 1 Secondary filtration to remove the fine particles in the water after the primary filtration to prepare the filtration eye (S11), by mixing the filtration eye and a solvent in a mixer (mixer) to the above-mentioned organic compound contained in the filtration eye It is dissolved in a solvent (S12).

The mixer is mixed for a sufficient time to extract the solvent, wherein the solvent may be used, or mixed with quinoline recoverable in the process and kerosine generated in the petrochemical process, respectively. .

In addition, when the amount of the solvent is based on the amount extracted in the extractor to be described later, it is possible to extract 95% or more of the organic compound by mixing at least 3.5% by volume with respect to the filtered eye, the reason for the experimental example 1 to be described later Through (see FIG. 2).

In addition, when quinoline and kerosene are used in addition to quinoline or kerosene alone, quinoline and kerosene are preferably mixed at a ratio of 1: 1, and quinoline or kerosene alone, quinoline and kerosene are mixed. There is no big difference in the extraction amount of the organic compound according to the use, this was also proved through Experimental Example 1 to be described later.

After the step (S12), through the extractor to extract the organic compound dissolved in the solvent (S13), purified ordination separated from the bottom of the extractor is utilized in the process.

Thereafter, the organic compound extracted by the solvent is distilled through a steam tower (S14), the distillation column temperature is preferably to have a temperature of 120 ℃ or more, which is necessary as a temperature condition to achieve a distillation recovery of 95% or more , The recovery rate is significantly reduced below 120 ℃ (see Figure 3).

After the step (S14), the remaining residue is cooled to crystallize (S15), the crystals produced in the crystallization step is filtered to recover the organic compound (S16), the distilled solvent is condensed and reused, the present invention Through each of the above steps to recover the organic compound contained in the ordination.

Hereinafter, the preferred solvent mixture amount in the organic compound dissolution step and the preferred distillation temperature conditions in the distillation step through Experimental Example 1 and Experimental Example 2 are as follows.

Experimental Example  One

In Experimental Example 1, as an experimental example for determining the volume ratio of a solvent used for solvent extraction of organic compounds contained in ordination, quinoline and kerosene were respectively mixed or mixed, and then the amount contained in the solvent and extracted was tested. Enough time was mixed for the extraction of the solvent and the extraction time was tested at the same time, in the process of the present invention was carried out based on 20 ℃ at room temperature for 5 minutes to extract sufficient mixed solvent. As a result, the volume% of the extracted amount is summarized and shown in FIG. 2.

As shown in Figure 2, the amount of solvent used to extract the organic compounds contained in the ordination should contain at least 3.5% by volume of more than 95% can be extracted, using quinoline and kerosene as a solvent or quinoline and kero, respectively It can be seen that there is no difference even when the mixture is used, and the amount of the solvent added is 3.5% by volume or more to be extracted, which is a preferable condition of the present invention.

Experimental Example  2

In Experimental Example 2, a distillation method is used to separate organic compounds extracted by solvents (quinoline and kerosene). The organic compounds are benzene, toluene, xylene, naphthalene and various benzene ring type organic compounds. To recover, highly vaporizable organic compounds are recovered at the top of the distillation column, and residues such as polymers and naphthalene contained in the solvent discharged from the bottom of the distillation column are cooled in a cooler to recover the crystallized material, and the rest is reused as a regenerated solvent. do.

Therefore, it is necessary to set distillation temperature conditions, and the relationship test between distillation temperature, polymer, naphthalene content, and solvent amount was carried out. In order to derive these conditions, the distillation temperature is set and the distillation time is 20 minutes, so the solvent organic compound recovery rate is calculated based on this and is shown in FIG. 3.

In order to reuse the solvent in FIG. 3, it is very important in the process to distill and use the solvent. In order to secure a recovery rate of 90% or more of the organic compound in the solvent containing the organic temperature, the temperature condition is possible at 120 ° C or higher. If the temperature is lower than 120 ° C., the recovery rate of organic compounds is reduced to less than 90%. Therefore, in the present invention, the distillation temperature at 120 ° C. or higher can increase the recovery rate of organic compounds, which is a preferable condition of the invention.

As described above, the method for recovering the organic compound contained in the ordination according to the present invention has been described with reference to the illustrated drawings. However, the present invention is not limited by the embodiments and drawings disclosed herein and is within the technical spirit of the present invention. Of course, various modifications may be made by those skilled in the art.

1 is a schematic diagram illustrating a method for recovering an organic compound contained in ordination according to the present invention;

2 is a graph showing a preferred amount of solvent addition in the method for recovering organic compounds contained in ordination according to the present invention;

3 is a graph showing a preferred distillation temperature in the method for recovering the organic compound contained in the ordination according to the present invention,

4 is a flowchart of a method for recovering organic compounds contained in ordination according to the present invention.

Claims (4)

In the recovery method of organic compounds contained in the ordination generated in the coke manufacturing process, (a) preparing filtered ophthalmology through first and second filtration of the supplied ordination; (b) mixing the filtration eye and a solvent to dissolve an organic compound contained in the filtration eye in the solvent; (c) extracting the organic compound dissolved in the solvent; (d) distilling the organic compound extracted by the solvent; (e) cooling and crystallizing the residues remaining in the distillation step; (f) recovering the organic compound contained in the ordination comprising the step of recovering the organic compound by filtering the crystals produced in the crystallization step. The method of claim 1, The solvent in the organic compound dissolution step, A method for recovering organic compounds contained in ordination, wherein quinoline and kerosene are mixed with each other or in the same proportion. 3. The method of claim 2, The solvent in the organic compound dissolution step, A method for recovering organic compounds contained in ordination, characterized in that 3.5% by volume or more of the filtered ordination is contained. The method of claim 1, Distillation temperature in the organic compound distillation step, A method for recovering organic compounds contained in ordination, characterized by a temperature of 120 ° C. or higher.

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