CN101041446A - Treatment method of waste potassium carbonate solution in the process of producing hydrogen peroxide by anthraquinone method - Google Patents

Abstract

The invention relates to a method for treating waste potassium carbonate solution containing a large amount of anthraquinone degradation products generated in the process of preparing hydrogen peroxide by an anthraquinone process. Firstly, adding a waste potassium carbonate solution into a concentration pot, heating and concentrating, and collecting steam while heating to obtain condensed water. Adding methanol into the pot and stirring to obtain alcohol precipitation slurry; putting the alcohol precipitation slurry into a rotary device, and filtering the alcohol washing slurry to obtain alcohol precipitation filter residues and alcohol precipitation filtrate; carrying out alcohol washing and filtering on the alcohol precipitation filter residue by using methanol to obtain an alcohol washing filter cake and an alcohol washing filtrate; and (3) carrying out vacuum drying on the alcohol washing filter cake to obtain solid potassium carbonate with the potassium carbonate content of about 95.3%. Rectifying the alcohol precipitation filtrate to obtain rectification residual liquid and rectification methanol, and burning the rectification residual liquid of the condensed water and the alcohol precipitation filtrate by using a coal gas-making furnace. The recovery rate of the potassium carbonate in the treatment method is 85 percent, and no waste liquid is discharged in the whole treatment process.

Description

Treatment method of waste potassium carbonate solution in the process of producing hydrogen peroxide by anthraquinone method

technical field

The invention relates to a method for recovering resources in the treatment of industrial waste residues, in particular to a method for recycling, treating and utilizing waste potassium carbonate solution containing a large amount of anthraquinone degradation products produced in the process of producing hydrogen peroxide by an anthraquinone method.

Background technique

Hydrogen peroxide is used as a bleaching agent in the textile and paper industry, as an oxidizing agent and epoxy oxidizing agent in green chemical synthesis, and as a disinfectant and bactericide in the food and pharmaceutical industries. The anthraquinone method is the mainstream production process of hydrogen peroxide. In the production of hydrogen peroxide by the anthraquinone method, 2-ethylanthraquinone is used as the carrier, and heavy aromatic hydrocarbons and trioctyl phosphate are used as mixed solvents to prepare a solution of a certain composition (called a working solution). When potassium carbonate is processing the hydrogen peroxide working fluid, some of the water-soluble degradation products in the working fluid will be dissolved in the potassium carbonate solution, so that the organic matter in the potassium carbonate solution will continue to increase. When the organic matter in the potassium carbonate solution accumulates to a certain extent, it is not suitable for continuous recycling. Therefore, the original process uses a part of the potassium carbonate solution after the working fluid is processed to be mixed with the newly prepared pure potassium carbonate solution, and then returned to the working fluid treatment system for use, and the other part is discharged regularly. Not only waste resources, but also cause serious environmental pollution.

Contents of the invention

The purpose of the present invention is to overcome the problems of wasting resources and polluting the environment in the prior art, and provide a treatment method for waste potassium carbonate solution in the process of producing hydrogen peroxide by anthraquinone method, so as to reclaim resources from waste liquid, protect the environment, and improve society. economic benefits.

For reaching above-mentioned object, the technical scheme that the present invention adopts is: a kind of processing method of waste potassium carbonate solution in the production hydrogen peroxide process of anthraquinone method, comprises the steps:

(1) Material concentration: the waste potassium carbonate solution is heated, evaporated and concentrated, and the concentration is increased to 60-95%;

(2) Alcohol analysis: add low-molecular alcohol and stir to obtain alcohol analysis slurry;

(3) Filtration: filter the alcohol analysis slurry to obtain alcohol analysis filter residue and alcohol analysis filtrate;

(4) Alcohol washing and filtering: Alcohol washing and filtering are carried out on the alcohol analysis filter residue to obtain an alcohol washing filter cake and an alcohol washing filtrate.

The method for treating waste potassium carbonate solution in the process of producing hydrogen peroxide by the above-mentioned anthraquinone method includes a vacuum drying step: vacuum drying the alcohol-washed filter cake to obtain solid potassium carbonate.

In the above-mentioned treatment method of waste potassium carbonate solution in the process of producing hydrogen peroxide by anthraquinone method, the steps of filtering, washing with alcohol and vacuum drying are completed in a rotary device with functions of filtering, washing and vacuum drying.

The method for treating waste potassium carbonate solution in the process of producing hydrogen peroxide by the above-mentioned anthraquinone method involves rectifying the alcohol analysis filtrate to obtain rectification raffinate and low-molecular alcohol.

In the above method for treating waste potassium carbonate solution in the process of producing hydrogen peroxide by anthraquinone method, in the material concentration step, the concentration of waste potassium carbonate solution is increased to 85-95%.

The method for treating waste potassium carbonate solution in the process of producing hydrogen peroxide by anthraquinone method comprises the step of dissolving and dealcoholizing: washing the filter cake by dissolving the alcohol with water, evaporating the solution to separate low-molecular alcohols, and obtaining potassium carbonate solution.

The treatment method of waste potassium carbonate solution in the process of producing hydrogen peroxide by anthraquinone method, when the solution is evaporated to separate low-molecular alcohol, the alcohol-containing vapor is collected, and the alcohol-containing vapor is rectified to obtain rectification raffinate and low-molecular alcohol.

The treatment method of waste potassium carbonate solution in the process of producing hydrogen peroxide by anthraquinone method is to reuse the alcohol wash filtrate during alcohol analysis.

The treatment method of waste potassium carbonate solution in the process of producing hydrogen peroxide by anthraquinone method is to reuse low-molecular alcohol during alcohol washing.

The treatment method of waste potassium carbonate solution in the process of producing hydrogen peroxide by anthraquinone method uses a coal gas furnace to incinerate condensed water and rectification raffinate. In this way, the biodegradable organic matter can be decomposed into useful gas at high temperature in the gas generator, which completely solves the problem of environmental pollution caused by waste discharge.

In the present invention, through steps such as evaporation and alcohol analysis, the different components in the waste potassium carbonate solution containing a large amount of anthraquinone degradation products produced in the process of producing hydrogen peroxide by anthraquinone method are properly separated and treated, so that the main component potassium carbonate can be obtained. Re-entering the hydrogen peroxide manufacturing process, saving resources, protecting the environment, and improving social and economic benefits.

Said low-molecular alcohol mainly refers to methanol or ethanol.

Description of drawings

The present invention will be further described in detail below in conjunction with the accompanying drawings.

Accompanying drawing 1 of this specification sheet is the main process flow diagram of the processing method of waste potassium carbonate solution in a kind of embodiment anthraquinone method of the present invention produces hydrogen peroxide process;

Fig. 2 is the main process flow diagram of the second embodiment.

Detailed ways

Example 1

In the first embodiment shown in Figure 1, the waste potassium carbonate solution in the process of producing hydrogen peroxide by anthraquinone method is first treated with the waste potassium carbonate solution containing a large amount of anthraquinone degradation products after the hydrogen peroxide working solution, and its COD _Cr is 20087.2 mg/L, put into the concentration pot and heat to concentrate. When the concentration of potassium carbonate reaches 85%, stop the concentration; while heating, collect steam to obtain condensed water. Add methanol into the concentration pot and stir to make potassium carbonate undergo alcohol analysis to obtain alcohol analysis slurry; put the alcohol analysis slurry into a rotary device with functions of filtering, washing, vacuum drying and dissolving, and in the rotary device In the method, firstly, the alcohol washing slurry is filtered to obtain the alcohol analysis filter residue and the alcohol analysis filtrate; the alcohol analysis filter residue is carried out alcohol washing and filtering with methanol (ethanol can also be used), to obtain the alcohol washing filter cake and the alcohol washing filtrate; the alcohol washing filtrate Reuse directly during alcohol analysis. Then the alcohol-washed filter cake is vacuum-dried to remove methanol to obtain solid potassium carbonate with a potassium carbonate content of about 95.3%. Then the obtained solid potassium carbonate is dissolved and sent to the hydrogen peroxide process for reuse. Carry out rectification to the alcohol analysis filtrate obtained in the above process to obtain rectification raffinate and rectified methanol, and rectify methanol to be used for pickling. The rectification residue of condensed water and alcohol filtrate is incinerated in a coal gas generator, and the organic matter in it is decomposed at high temperature to generate useful gas. In the process of producing hydrogen peroxide by the anthraquinone method, the potassium carbonate recovery rate of the waste potassium carbonate solution treatment method is 85%, the COD _Cr removal rate is greater than 90%, and there is no waste liquid discharge in the whole treatment process.

Example 2

In the second embodiment shown in Figure 2, the waste potassium carbonate solution in the process of producing hydrogen peroxide by anthraquinone method is firstly treated with the waste potassium carbonate solution containing a large amount of anthraquinone degradation products after the hydrogen peroxide working solution is added to the concentrated pot for heating Concentrate, when the concentration of potassium carbonate reaches 90%, stop concentrating; while heating, collect steam to obtain condensed water. Add methanol into the concentration pot and stir to make potassium carbonate undergo alcohol analysis to obtain alcohol analysis slurry; put the above alcohol analysis slurry into a device with functions of filtering, washing and dissolving. The alcohol analysis slurry is filtered to obtain alcohol analysis filter residue and alcohol analysis filtrate; the alcohol analysis filter residue is alcohol washed and filtered with methanol to obtain alcohol wash filter cake and alcohol wash filtrate; the alcohol wash filtrate is directly reused during alcohol analysis. Then add water to dissolve the methanol-containing alcohol-washed filter cake, evaporate the solution to separate methanol and collect alcohol-containing vapor to obtain potassium carbonate solution and alcohol-containing vapor. Then the obtained potassium carbonate solution is sent to the hydrogen peroxide process for reuse. The alcohol analysis filtrate and alcohol-containing vapor obtained in the above process are treated by rectification to obtain rectification raffinate and rectified methanol, and the rectified methanol is reused. The condensed water and rectification residue produced by concentrating the waste potassium carbonate solution are incinerated in a coal gas generator. In the process of producing hydrogen peroxide by the anthraquinone method, the potassium carbonate recovery rate of the waste potassium carbonate solution treatment method is 85%, the COD _Cr removal rate is greater than 90%, and there is no waste liquid discharge in the whole treatment process.

The present invention is not limited to the specific embodiments described above, and all equivalent changes made according to the features and principles of the present invention fall within the protection scope of the present invention.

Claims (10)

1, a kind of processing method of waste potassium carbonate solution in the production hydrogen peroxide process of anthraquinone method is characterized in that comprising the steps: (1) Material concentration: the waste potassium carbonate solution is heated, evaporated and concentrated, and the concentration is increased to 60-95%; (2) Alcohol analysis: add low-molecular alcohol and stir to obtain alcohol analysis slurry; (3) Filtration: filter the alcohol analysis slurry to obtain alcohol analysis filter residue and alcohol analysis filtrate; (4) Alcohol washing and filtering: Alcohol washing and filtering are carried out on the alcohol analysis filter residue to obtain an alcohol washing filter cake and an alcohol washing filtrate. 2. the processing method of waste potassium carbonate solution in the production hydrogen peroxide process of anthraquinone method as claimed in claim 1, it is characterized in that comprising vacuum drying step: alcohol washing filter cake is carried out vacuum drying, obtains solid potassium carbonate. 3. the processing method of waste potassium carbonate solution in the production hydrogen peroxide process of anthraquinone method as claimed in claim 2, it is characterized in that: described filtration, alcohol washing filtration and vacuum drying step are to have filtration, washing and vacuum drying function together completed in the rotary device. 4. the processing method of waste potassium carbonate solution in the production hydrogen peroxide process of anthraquinone method as claimed in claim 1, it is characterized in that: alcohol analysis filtrate is carried out rectifying, obtains rectifying raffinate and low-molecular alcohol. 5. the processing method of waste potassium carbonate solution in the production hydrogen peroxide process of anthraquinone method as described in any one in claim 1 to 4, it is characterized in that: in the material concentration step, waste potassium carbonate solution concentration is brought up to 85-95 %. 6. the processing method of waste potassium carbonate solution in the production hydrogen peroxide process of anthraquinone method as claimed in claim 1, it is characterized in that comprising the dissolving dealcoholization step: wash filter cake with described alcohol of dissolving with water, carry out evaporation separation low-molecular alcohol to solution , to obtain potassium carbonate solution. 7. the processing method of spent potassium carbonate solution in the production hydrogen peroxide process of anthraquinone method as claimed in claim 6, it is characterized in that: when solution is evaporated and separated low molecular alcohol, alcohol-containing vapor is collected, and alcohol-containing vapor is rectified , to obtain rectification raffinate and low molecular weight alcohol. 8. the processing method of waste potassium carbonate solution in the production hydrogen peroxide process of anthraquinone method as described in any one in claim 1 to 4, it is characterized in that: alcohol washing filtrate is reused when alcohol analysis. 9. the processing method of spent potassium carbonate solution in the production hydrogen peroxide process of anthraquinone method as claimed in claim 4 or 7, it is characterized in that: low molecular weight alcohol is reused when washing with alcohol. 10. The method for processing waste potassium carbonate solution in the process of producing hydrogen peroxide by anthraquinone method as claimed in claim 4 or 7, characterized in that: utilize coal gas generator to incinerate condensed water and rectification raffinate.

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