CN113069907A

CN113069907A - Preparation method of wet-process complex iron desulfurizer

Info

Publication number: CN113069907A
Application number: CN202110498463.5A
Authority: CN
Inventors: 齐建光; 沈媛媛; 孟凡庆; 李鑫; 王英龙
Original assignee: Qingdao University of Science and Technology
Current assignee: Qingdao University of Science and Technology
Priority date: 2021-05-08
Filing date: 2021-05-08
Publication date: 2021-07-06

Abstract

The invention discloses an improved technology for removing sulfide from a gas mixture by a complex iron method, and provides a desulfurization solution with a multi-component combination and a corresponding desulfurization process thereof. The complex iron desulfurizer solution synthesized by the process has the advantages of good desulfurization performance, safe equipment operation, good operation elasticity, simple preparation method and the like.

Description

Preparation method of wet-process complex iron desulfurizer

[ technical field ] A method for producing a semiconductor device

The invention discloses a preparation method of a complex iron desulfurizer by multi-component wet desulphurization, belonging to the field of acid gas purification. The complex iron desulfurizer solution synthesized by the invention has the advantages of good desulfurization performance, safe equipment operation, good operation elasticity, simple preparation method and the like.

[ background of the invention ]

Because of the enhancement of the environmental awareness of people and the relation to the national civilization, the desulfurization becomes an important working section in the chemical industry. Desulfurization analysis is an important component in desulfurization industrial production for monitoring key parameters such as gas components, desulfurization solution, catalyst concentration, suspended sulfur and the like in real time in order to ensure normal operation of a desulfurization process. The high-efficiency desulfurizer is not beneficial to large-scale industrial popularization due to high price, and a complex iron desulfurization system is researched and screened, has good stability under the condition of partial alkali and high sulfur capacity, and is beneficial to large-scale industrial application.

At present, many complex iron desulfurization systems are being researched, and China also conducts research on the research and development of complex iron desulfurizing agents. And adding a stabilizer of anhydrous glucose in the process, and adjusting the pH value of the desulfurization solution to 8-10 by using a buffer solution. The method improves the desulfurization efficiency of the complex iron desulfurizer; the corrosion of equipment is reduced; the generated sulfur particles and the desulfurization mother liquor are easy to separate; the regeneration needs short time and low energy consumption. But most of them stay at the laboratory level, and the purpose of this research is to carry out large-scale industrial popularization. The complex iron system studied by the process mainly comprises FeSO₄EDTA, ammonia water, organic phosphate, stabilizer, compared with the commercial desulfurizing agents such as 888, MSQ, ADA and the like, the desulfurizing agent is more economical and has more market competitiveness. The screened desulfurizer has high sulfur capacity and good regeneration performance.

The invention adopts ferric chloride as a raw material to synthesize the complex iron desulfurizer, and provides a novel preparation method of the wet complex iron desulfurizer.

[ summary of the invention ]

[ problem to be solved ]

Aiming at the defects in the prior art, the invention aims to complex an iron desulfurizer by a wet method, so that the newly synthesized desulfurizer can efficiently remove sulfides from a gas mixture, thereby reducing equipment corrosion and solving the problems of poor stability of a desulfurization solution, high desulfurization cost, low reaction rate and the like in a desulfurization process.

[ solution ]

The invention is realized by the following technical scheme.

An improved complex iron method for removing sulfide from a gas mixture comprises the following components in percentage by weight: 10-100 ppm of an antioxidant, 5-50 ppm of a surfactant, and the balance of a complex iron catalyst and water, wherein the complex iron catalyst is composed of a complexing agent, deionized water, ammonia water and ferric chloride, and the complex iron desulfurizer is prepared by the following method.

Adding a complexing agent, deionized water and ammonia water into a reactor with a stirring function and a heating function, starting stirring, and heating to 100-150 ℃. EDTA was added with stirring.

Then, ferric chloride is dissolved in the aqueous solution, and the solution releases heat and is continuously stirred until all the solvent is obtained.

And finally, slowly dropwise adding the dissolved ferric chloride solution into the EDTA ammonia water solution, stirring for about 1h, and stabilizing to obtain the EDTA ferric amine solution after the improved process.

[ advantageous effects ]

Compared with the prior art, the invention mainly has the following beneficial effects:

(1) the complex iron desulfurizer solution prepared by the method can obtain a high-performance desulfurization effect, and solves the problem that sulfides in the mixture are difficult to remove.

(2) The method has the advantages of simple process, less investment equipment and high iron content in the iron-synthesizing desulfurizer.

[ description of the drawings ]

FIG. 1 is a diagram of the operating equipment of the preparation method of wet complex iron desulfurizer.

[ detailed description ] embodiments

Example 1:

100mL of deionized water, 97g of ferric chloride and 2mL of sulfuric acid are taken. 97g of ferric chloride is slowly dissolved into 100mL of deionized water, and then the mixture is continuously stirred, the reaction releases heat, and the ferric chloride is slowly dissolved without continuous stirring. After complete dissolution, the mixture is left to stand to room temperature. Then weighing 100g of EDTA and 200mL of ammonia water, dissolving while stirring in a fume hood, after the EDTA is completely dissolved, the solution is clear, slowly adding the ferric chloride solution into the EDTA ammonia water solution, and continuously stirring in the dissolving process to prevent the formation of precipitates. And finally, adding polyaspartic acid, glycerol and a sorbitol stabilizer into the solution, and stirring to completely dissolve the polyaspartic acid, glycerol and sorbitol stabilizer to obtain a solution, namely the reddish brown complex iron desulfurizer solution which has strong desulfurization performance.

Example 2:

100mL of deionized water, 97g of ferric chloride and 2mL of sulfuric acid are taken. 97g of ferric chloride is slowly dissolved into 100mL of deionized water, and then the mixture is continuously stirred, the reaction releases heat, and the ferric chloride is slowly dissolved without continuous stirring. After complete dissolution, the mixture is left to stand to room temperature. Then weighing 100g of EDTA and 200mL of ammonia water, dissolving while stirring in a fume hood, after the EDTA is completely dissolved, the solution is clear, slowly adding the ferric chloride solution into the EDTA ammonia water solution, and continuously stirring in the dissolving process to prevent the formation of precipitates. Adding polyaspartic acid, glycerol and sorbitol stabilizer in batches during stirring, and stirring to completely dissolve to obtain a solution, namely the reddish brown complex iron desulfurizer solution, which has strong desulfurization performance.

Example 3:

100mL of deionized water, 97g of ferric chloride and 2mL of sulfuric acid are taken. 97g of ferric chloride is slowly dissolved into 100mL of deionized water, then stirring is carried out continuously, the reaction releases heat, the ferric chloride needs to be slowly dissolved and stirring is not carried out continuously, and in addition, a part of content of stabilizer is additionally added. After complete dissolution, the mixture is left to stand to room temperature. Then weighing 100g of EDTA and 200mL of ammonia water, dissolving while stirring in a fume hood, after the EDTA is completely dissolved, the solution is clear, adding another part of stabilizer, then slowly adding the ferric chloride solution into the EDTA ammonia water solution, and continuously stirring in the dissolving process to prevent the formation of precipitates. Adding polyaspartic acid, glycerol and sorbitol stabilizer in batches during stirring, and stirring to completely dissolve to obtain a solution, namely the reddish brown complex iron desulfurizer solution, which has strong desulfurization performance.

Claims

1. an improved complex iron method removes sulfide from gas mixture, comprising the composition of the following percentage by weight: antioxidant 10～100ppm, surfactant 5～50ppm, and the rest are complex iron catalyst and water, wherein, The complex iron catalyst is composed of a complexing agent, deionized water, ammonia water and ferric chloride, and the complex iron desulfurizing agent is prepared by the following method;

Add the complexing agent, deionized water and ammonia water into the reactor with stirring function and heating function, start stirring, heat up to 100-150 °C, and add EDTA while stirring;

Then, ferric chloride is dissolved in the aqueous solution, the dissolution is exothermic, and the stirring is continued until all the solvent is present;

Finally, the dissolved ferric chloride solution was slowly added dropwise to the EDTA ammonia solution, stirred for about 1 hour, and stabilized to obtain a complex iron desulfurizer solution with the improved process;

(1) Take 100mL of deionized water, 97g of ferric chloride, and 2mL of sulfuric acid, respectively, first slowly dissolve 97g of ferric chloride into 100mL of deionized water, and then keep stirring, the reaction is exothermic, and must be slowly dissolved and kept stirring;

(2) Take 100 g of EDTA and 200 mL of ammonia water and dissolve them in a fume hood while stirring. After the EDTA is completely dissolved, the solution is clear. At this time, the ferric chloride solution is slowly added to the EDTA ammonia solution. form;

(3) Add polyaspartic acid, glycerol, and sorbitol stabilizer to the solution, and after stirring to dissolve completely, the obtained solution is a reddish-brown complex iron desulfurizer solution, which has strong desulfurization performance.

2. the preparation method of a kind of wet method complex iron desulfurizer according to claim 1, is characterized in that: described preparation required complexing agent of complex iron catalyst, deionized water, ammoniacal liquor, ferric chloride etc. The raw materials are readily available, the experimental device is simple, and the maneuverability is large.

3. the preparation method of a kind of wet method complex iron desulfurizer according to claim 1, is characterized in that: the stability of described wet method complex iron desulfurizer is strong, adjust solution pH to 8～10 with ammoniacal liquor, Alkaline environment desulfurization effect is stronger.