阅读说明：本技术 一种用于低浓度羰基硫净化的脱硫剂的制备方法 (Preparation method of desulfurizer for purifying low-concentration carbonyl sulfide ) 是由 周鹏翔 李彬 宁平 李建军 齐佳敏 杨迪 于 2021-09-17 设计创作，主要内容包括：本发明公开了一种用于低浓度羰基硫净化的脱硫剂的制备方法,该方法包括：(1)选取赤泥、改性助剂作为原料；(2)将用水溶解的改性助剂倒入预处理后的赤泥中并在搅拌均匀；将容器放入水浴锅内进行磁力搅拌蒸发；(3)将赤泥和改性助剂混合物置于60℃的真空干燥箱中干燥2h；(4)将干燥后的混合物研磨后置于管式炉中,在氮气氛围下以每分钟5℃的升温速率升温至400-500℃并恒温8-16小时,焙烧完成后在炉内冷却至室温；(5)将焙烧后的混合物用压片机压片,破碎后过40-60目筛,得到脱硫剂成品。本发明既可以减少赤泥对环境的污染,又可以对含低浓度的羰基硫体进行脱硫处理,以废治废,达到降低废气净化成本的目的,实现了大宗固废物的资源化循环利用。(The invention discloses a preparation method of a desulfurizer for purifying low-concentration carbonyl sulfide, which comprises the following steps: (1) selecting red mud and a modification auxiliary agent as raw materials; (2) pouring the modified auxiliary dissolved by water into the pretreated red mud and uniformly stirring; putting the container into a water bath kettle for magnetic stirring and evaporation; (3) placing the mixture of the red mud and the modification auxiliary agent in a vacuum drying oven at 60 ℃ for drying for 2 h; (4) grinding the dried mixture, placing the ground mixture in a tube furnace, heating the mixture to 400-500 ℃ at a heating rate of 5 ℃ per minute in a nitrogen atmosphere, keeping the temperature for 8-16 hours, and cooling the mixture to room temperature in the furnace after roasting is finished; (5) and tabletting the roasted mixture by using a tabletting machine, crushing, and sieving by using a 40-60-mesh sieve to obtain a finished product of the desulfurizer. The invention can reduce the pollution of the red mud to the environment, and can also carry out desulfurization treatment on carbonyl sulfide with low concentration, so as to treat waste with waste, achieve the purpose of reducing the purification cost of waste gas, and realize the recycling of a large amount of solid waste.)

1. A preparation method of a desulfurizing agent for purifying low-concentration carbonyl sulfide is characterized by comprising the following steps:

(1) preparing materials: selecting red mud and a modifying auxiliary agent as raw materials, wherein the modifying auxiliary agent accounts for 0-5% of the weight of the red mud;

(2) excess impregnation: pretreating red mud, adding a modification auxiliary agent into water for dissolving, pouring the pretreated red mud after the modification auxiliary agent is dissolved, and uniformly stirring in a container; putting the container into a water bath kettle, magnetically stirring and evaporating until the mixture of the red mud and the modification auxiliary agent is in a block shape;

(3) and (3) drying: placing the mixture of the red mud and the modification auxiliary agent in a vacuum drying oven at 60 ℃ for drying for 2h, and removing water;

(4) roasting: grinding the dried mixture, placing the ground mixture in a tube furnace, heating the mixture to 400-500 ℃ at a heating rate of 5 ℃ per minute in a nitrogen atmosphere, keeping the temperature for 8-16 hours, and cooling the mixture to room temperature in the furnace after roasting is finished;

(5) tabletting: and tabletting the roasted mixture by using a tabletting machine, crushing, and sieving by using a 40-60-mesh sieve to obtain a finished product of the desulfurizer.

2. The preparation method of the desulfurizing agent for purifying low-concentration carbonyl sulfide according to claim 1, wherein the modifying assistant in step (1) is polyethylene glycol.

3. The method for preparing a desulfurizing agent for purifying low-concentration carbonyl sulfide according to claim 1, wherein the step (2) of performing magnetic stirring evaporation in a water bath comprises the following steps: and magnetically stirring at 25 ℃ for 8-16h, adjusting the temperature to 40 ℃, and magnetically stirring and evaporating until the mixture of the red mud and the modification auxiliary agent is in a block shape.

4. The preparation method of the desulfurizing agent for purifying low-concentration carbonyl sulfide according to claim 1, wherein the red mud in the step (2) is pretreated; the red mud is dried, and then the dried red mud is ground and sieved by a 200-mesh sieve.

5. The method as claimed in claim 2, wherein the molecular weight of the polyethylene glycol is 2000-6000.

6. The preparation method of the desulfurizing agent for purifying low-concentration carbonyl sulfide according to claim 1, wherein the solid-to-liquid ratio of the modifying assistant to water in the step (2) is 1: 5-8.

Technical Field

The invention relates to a preparation method of a desulfurizer for purifying low-concentration carbonyl sulfur, belonging to the technical field of adsorbents.

Background

Carbonyl sulfide (COS) is a colorless, odorless, toxic gas having a molecular structure similar to that of carbon dioxide, a linear structure, and is slightly soluble in water but easily soluble in an organic solvent. COS molecules have weak acidity and relatively stable chemical properties, but also have certain reaction activity under certain conditions, and can perform chemical reactions such as oxidation, hydrolysis, hydrogenation reduction and the like.

The technology of COS desulfurization is mainly divided into a dry method and a wet method. The dry method is convenient to operate, high in desulfurization precision, low in investment consumption, low in resistance when the equipment runs, and low in secondary pollution. Therefore, dry desulfurization techniques will be appreciated for low concentration COS purification. In the application of the practical COS desulfurizing agent, an adsorption method, an oxidation method, a catalytic hydrolysis method and a hydrogenation reduction method are four main dry method COS removing methods. The adsorption desulfurization method has the characteristics of simple operation, high desulfurization rate and less side reaction, but the adsorption quantity of the unmodified porous material to the COS is limited, and the raw material is modified to possibly meet the requirement on industrial application; the basic principle of removing COS by the oxidation method is to oxidize COS into SO₂Then SO is added₂The removal is carried out, the desulfurization rate is higher, but the treatment effect on low-concentration COS is not good enough; the principle of removing COS by catalytic hydrolysis method is that COS is first converted into H₂S, H is removed by a general method₂S, the aim of removing COS is fulfilled, the reaction temperature of the catalytic hydrolysis method is low, raw material gas is not consumed, side reactions are fewer, and the method is widely concerned by scientific researchers; the hydrogenation reduction method is to use a reducing agent (such as H)₂Etc.) conversion of COS to H₂S, similar to the catalytic hydrolysis method, belongs to a method for indirectly removing COS.

In view of the above, it is necessary to research a method for preparing a desulfurizing agent for purification of low-concentration carbonyl sulfide to solve the above technical problems.

Disclosure of Invention

The invention aims to overcome the problems in the prior art and provide a preparation method of a desulfurizer for purifying low-concentration carbonyl sulfur, wherein the prepared desulfurizer can reduce the pollution of red mud to the environment, and can also perform desulfurization treatment on gas containing low-concentration COS to treat wastes with processes of wastes against one another, thereby achieving the purposes of reducing the purification cost of waste gas and recycling the wastes.

In order to achieve the purpose, the invention adopts the technical scheme that:

according to one aspect of the invention, the invention provides a preparation method of a desulfurizing agent for purifying low-concentration carbonyl sulfur, which is characterized by comprising the following steps:

(1) preparing materials: selecting red mud and a modifying auxiliary agent as raw materials, wherein the modifying auxiliary agent accounts for 0-5% of the weight of the red mud;

(2) excess impregnation: pretreating red mud, adding a modification auxiliary agent into water for dissolving, pouring the pretreated red mud after the modification auxiliary agent is dissolved, and uniformly stirring in a container; putting the container into a water bath kettle, magnetically stirring and evaporating until the mixture of the red mud and the modification auxiliary agent is in a block shape;

(3) and (3) drying: placing the mixture of the red mud and the modification auxiliary agent in a vacuum drying oven at 60 ℃ for drying for 2h, and removing water;

(4) roasting: grinding the dried mixture, placing the ground mixture in a tube furnace, heating the mixture to 400-500 ℃ at a heating rate of 5 ℃ per minute in a nitrogen atmosphere, keeping the temperature for 8-16 hours, and cooling the mixture to room temperature in the furnace after roasting is finished;

(5) tabletting: and tabletting the roasted mixture by using a tabletting machine, crushing, and sieving by using a 40-60-mesh sieve to obtain a finished product of the desulfurizer.

The red mud contains rich calcium, iron and aluminum oxides, has strong alkalinity, and can generate good adsorption effect on low-concentration carbonyl sulfide.

Preferably, the modifying assistant in the step (1) is polyethylene glycol.

Preferably, the step (2) is carried out in a water bath kettle by magnetic stirring evaporation, wherein: and magnetically stirring at 25 ℃ for 8-16h, adjusting the temperature to 40 ℃, and magnetically stirring and evaporating until the mixture of the red mud and the modification auxiliary agent is in a block shape.

Preferably, the red mud pretreatment in the step (2) is; the red mud is dried, and then the dried red mud is ground and sieved by a 200-mesh sieve.

Preferably, the molecular weight of the polyethylene glycol is 2000-.

Preferably, the solid-to-liquid ratio of the modification aid to water in the step (2) is 1: 5-8. In conclusion, the beneficial effects of the invention are as follows:

1. the method takes the red mud solid waste of an alumina plant as a main raw material, the modifying auxiliary agent selects polyethylene glycol, a certain amount of polyethylene glycol is added after the dried red mud is ground and sieved, the mixture is fully stirred, water is added to pour the dissolved polyethylene glycol into the red mud, the mixture is uniformly stirred, the mixture is magnetically stirred and evaporated to dryness in a water bath kettle, the polyethylene glycol is loaded on the surface of the red mud by an excessive dipping method, and Lewis base in the red mud is uniformly distributed again; baking at high temperature, adjusting the crystalline phase of the red mud component, tabletting and sieving to prepare the COS solid desulfurizer. The invention can reduce the pollution of the red mud to the environment, and can also carry out desulfurization treatment on carbonyl sulfide with low concentration, so as to treat waste with waste, achieve the purpose of reducing the purification cost of waste gas, and realize the recycling of a large amount of solid waste.

2. The desulfurizer prepared by using the industrial waste red mud as the raw material has good adsorption effect on carbonyl sulfide with low concentration, has high environmental protection property and high economy, accords with the national policy guidance of solid waste recycling, and achieves the purposes of treating waste by waste and recycling waste.

Drawings

FIG. 1 is a flow chart of the manufacturing process of the present invention;

FIG. 2 is a graph showing the effect of different treatment modes of red mud on the desulfurization efficiency of a desulfurizing agent;

FIG. 3 is a diagram showing the influence of modification aids and their different qualities on desulfurization efficiency of a desulfurizing agent;

FIG. 4 is a graph showing the effect of different calcination temperatures on desulfurization efficiency of a desulfurizing agent;

FIG. 5 is a graph showing the effect of different calcination times on desulfurization efficiency of a desulfurizing agent.

Detailed Description

Reference will now be made in detail to embodiments of the present invention, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to the same or similar elements or elements having the same or similar function throughout. The embodiments described below with reference to the accompanying drawings are illustrative only for the purpose of explaining the present invention, and are not to be construed as limiting the present invention.

The following describes in detail a method for preparing a desulfurizing agent for low-concentration carbonyl sulfide purification according to the present invention with reference to the accompanying drawings.

The Red Mud (RM) can be divided into sintering process red mud, Bayer process red mud and combination process red mud according to different production modes. The red mud has the characteristics of strong alkalinity, large yield and fine granularity, and generally has rich contents of calcium, aluminum and iron oxide. At present, the subsequent disposal of the red mud is difficult, and an open-air stacking mode is usually adopted, which has great damage to the land and can cause pollution to the atmosphere, water sources and the like. The method comprehensively utilizes the red mud, turns harm into benefit, changes waste into valuable, and is a method which not only contains economic benefit, but also accords with environmental benefit. The preparation method of the following example uses red mud as one of the main raw materials.

Example 1

The preparation method of the desulfurizer for purifying low-concentration carbonyl sulfide comprises the following specific steps:

(1) drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 5g of red mud, putting the red mud into a stirring container, pouring 25ml of water into the red mud, and uniformly stirring to obtain a mixture of the red mud and the water, wherein the weight of the polyethylene glycol is 0 g.

(3) Placing the magnetic rotor into a container containing the mixture, placing the container into a water bath, magnetically stirring for 12h at 25 deg.C in the water bath, adjusting the temperature of the water bath to 40 deg.C, and magnetically stirring to evaporate the mixture into blocks.

(4) Putting the blocky red mud into a vacuum drying oven at 60 ℃ for drying for 2h, grinding, putting into a tubular furnace, roasting at 400 ℃ for 8h under the nitrogen atmosphere, and cooling to room temperature in the tubular furnace.

(5) Tabletting the roasted red mud by a tabletting machine, and sieving by a 40-60 mesh sieve to prepare the red mud-based desulfurizer.

Taking 0.45g of prepared red mud-based desulfurizer, and filling the red mud-based desulfurizer into a fixed bed reactor, wherein the inner diameter of the fixed bed reactor is 6mm, and the volume space velocity of the fixed bed reactor is 10000h^-1Under the conditions of normal pressure, 80 ℃ of reaction temperature, 3.60 percent of reaction relative humidity and 100ppm of COS content, the removal rate of the COS is more than 90 percent.

Control group 1

(1) Drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 0.45g of red mud, tabletting by using a tabletting machine, and sieving by using a 40-60 mesh sieve to prepare the red mud-based desulfurizer.

Control group 2

(1) Drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 5g of red mud, putting the red mud into a vacuum drying oven at 60 ℃ for drying for 2h, putting the red mud into a tube furnace, roasting the red mud for 8h at 400 ℃ in a nitrogen atmosphere, and cooling the red mud to room temperature in the tube furnace.

(3) Tabletting the roasted desulfurizer by a tablet machine, and sieving by a 40-60 mesh sieve to prepare the red mud-based desulfurizer.

(4) As shown in fig. 2, the inventors found that the desulfurization efficiency of the desulfurizer prepared by the preparation method of the embodiment 1 is much higher than that of the control group 1 and the control group 2, as compared with the case where the red mud in the control group 1 is not roasted and stirred to prepare the red mud-based desulfurizer, and the case where the red mud in the control group 2 is roasted at 400 ℃ for 8 hours in a nitrogen atmosphere but is not stirred to prepare the red mud-based desulfurizer. The inventor finds that whether red mud impregnation is carried out or not can directly influence the desulfurization efficiency through a large number of experiments.

Example 2

The preparation method of the desulfurizing agent for purifying low-concentration carbonyl sulfide, described in this embodiment, includes the following specific steps:

(1) drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 5g of red mud and 0.05g of polyethylene glycol, dissolving the polyethylene glycol in 25ml of water, pouring the red mud into the water, and uniformly stirring the mixture to obtain a mixture.

(3) Placing the magnetic rotor into a container containing the mixture, placing the container into a water bath, magnetically stirring for 12h at 25 ℃ in a water bath, adjusting the temperature of the water bath to 40 ℃, and magnetically stirring until the mixture is evaporated to dryness to form blocks.

(4) And (3) putting the blocky mixture into a vacuum drying oven at 60 ℃ for drying for 2h, grinding, putting into a tube furnace, roasting at 400 ℃ for 8h in a nitrogen atmosphere, and cooling to room temperature in the tube furnace.

(5) Tabletting the roasted mixture by a tabletting machine, and sieving by a 40-60 mesh sieve to prepare the desulfurizer.

Taking 0.45g of prepared desulfurizer, and filling the desulfurizer into a fixed bed reactor, wherein the inner diameter is 6mm, and the volume space velocity is 10000h^-1Under the conditions that the reaction pressure is normal pressure, the reaction temperature is 80 ℃, the reaction relative humidity is 3.60 percent and the content of COS is 100ppm, the removal rate of carbonyl sulfide (COS) is more than 90 percent.

Control group 1

(1) Drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 5g of red mud and 0.25g of polyethylene glycol, dissolving the polyethylene glycol in 25ml of water, pouring the red mud into the water, and uniformly stirring the mixture to obtain a mixture.

(3) Placing the magnetic rotor into a container, placing the container into a water bath, magnetically stirring for 12h at 25 ℃ of the water bath, adjusting the temperature of the water bath to 40 ℃, and magnetically stirring until the mixture is in a block shape.

(4) And (3) putting the blocky mixture into a vacuum drying oven at 60 ℃ for drying for 2h, grinding, putting into a tube furnace, roasting at 400 ℃ for 8h in a nitrogen atmosphere, and cooling to room temperature in the tube furnace.

(5) Tabletting the roasted mixture by a tabletting machine, and sieving by a 40-60 mesh sieve to prepare the red mud-based desulfurizer.

Control group 2

(1) Drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 5g of red mud and 0.15g of polyethylene glycol, dissolving the polyethylene glycol in 25ml of water, pouring the red mud into the water, and stirring the mixture to obtain a mixture.

(3) Placing the magnetic rotor into a container, placing the container into a water bath, magnetically stirring for 12h at 25 ℃ of the water bath, adjusting the temperature of the water bath to 40 ℃, and magnetically stirring until the mixture is evaporated to dryness to be in a block shape.

(4) And (3) putting the blocky mixture into a vacuum drying oven at 60 ℃ for drying for 2h, grinding, putting into a tube furnace, roasting at 400 ℃ for 8h in a nitrogen atmosphere, and cooling to room temperature in the tube furnace.

(5) Tabletting the roasted mixture by a tabletting machine, and sieving by a 40-60 mesh sieve to prepare the desulfurizer.

Control group 3

(1) Drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 5g of red mud and 0.025g of polyethylene glycol, dissolving the polyethylene glycol in 25ml of water, pouring the red mud into the water, and uniformly stirring the mixture to obtain a mixture.

(3) Placing the magnetic rotor into a container, placing the container into a water bath, magnetically stirring for 12h at 25 ℃ of the water bath, adjusting the temperature of the water bath to 40 ℃, and magnetically stirring until the mixture is evaporated to dryness to be in a block shape.

(4) And (3) putting the blocky mixture into a vacuum drying oven at 60 ℃ for drying for 2h, grinding, putting into a tube furnace, roasting at 400 ℃ for 8h in a nitrogen atmosphere, and cooling to room temperature in the tube furnace.

(5) Tabletting the roasted mixture by a tabletting machine, and sieving by a 40-60 mesh sieve to prepare the red mud-based desulfurizer.

Control group 4

(1) Drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 5g of red mud and 0g of polyethylene glycol, pouring 25ml of water into the red mud, and uniformly stirring to obtain a mixture.

(3) Placing the magnetic rotor into a container, placing the container into a water bath, magnetically stirring for 12h at 25 ℃ of the water bath, adjusting the temperature of the water bath to 40 ℃, and magnetically stirring until the mixture is evaporated to dryness to be in a block shape.

(4) And (3) putting the blocky mixture into a vacuum drying oven at 60 ℃ for drying for 2h, grinding, putting into a tube furnace, roasting at 400 ℃ for 8h in a nitrogen atmosphere, and cooling to room temperature in the tube furnace.

(5) Tabletting the roasted mixture by a tabletting machine, and sieving by a 40-60 mesh sieve to prepare the desulfurizer.

As shown in FIG. 3, the inventors found that the desulfurization efficiency of the desulfurizing agent is more or less affected by the amount of polyethylene glycol (PEG).

Example 3

The preparation method of the desulfurizing agent for purifying low-concentration carbonyl sulfide, described in this embodiment, includes the following specific steps:

(1) drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 5g of red mud and 0.05g of polyethylene glycol, dissolving the polyethylene glycol in 25ml of water, pouring the red mud into the water, and uniformly stirring the mixture to obtain a mixture.

(3) Placing the magnetic rotor into a container containing the mixture, placing the container into a water bath, magnetically stirring for 12h at 25 ℃ in the water bath, adjusting the temperature of the water bath to 40 ℃, and magnetically stirring until the mixture is evaporated to dryness to form blocks.

(4) And (3) putting the blocky mixture into a vacuum drying oven at 60 ℃ for drying for 2h, grinding, putting into a tube furnace, roasting at 500 ℃ for 8h under the nitrogen atmosphere, and cooling to room temperature in the tube furnace.

(5) Tabletting the roasted mixture by a tabletting machine, and sieving by a 40-60 mesh sieve to prepare the desulfurizer.

Taking 0.45g of prepared red mud-based desulfurizer, and filling the red mud-based desulfurizer into a fixed bed reactor, wherein the inner diameter of the fixed bed reactor is 6mm, and the volume space velocity of the fixed bed reactor is 10000h^-1Under the conditions of normal pressure, 80 ℃ of reaction temperature, 3.60 percent of reaction relative humidity and 100ppm of COS content, the removal rate of the COS is more than 99 percent.

Control group 1

(1) Drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 5g of red mud and 0.05g of polyethylene glycol, dissolving the polyethylene glycol in 25ml of water, pouring the red mud into the water, and uniformly stirring the mixture to obtain a mixture.

(3) Placing the magnetic rotor into a container containing the mixture, placing the container into a water bath, magnetically stirring for 12h at 25 ℃ in the water bath, adjusting the temperature of the water bath to 40 ℃, and magnetically stirring until the mixture is evaporated to dryness to form blocks.

(4) And (3) putting the blocky mixture into a vacuum drying oven at 60 ℃ for drying for 2h, grinding, putting into a tube furnace, roasting at 350 ℃ for 8h under the nitrogen atmosphere, and cooling to room temperature in the tube furnace.

(5) Tabletting the roasted mixture by a tabletting machine, and sieving by a 40-60 mesh sieve to prepare the desulfurizer.

Control group 2

(1) Drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 5g of red mud and 0.05g of polyethylene glycol, dissolving the polyethylene glycol in 25ml of water, pouring the red mud into the water, and uniformly stirring the mixture to obtain a mixture.

(3) Placing the magnetic rotor into a container containing the mixture, placing the container into a water bath, magnetically stirring for 12h at 25 ℃ in the water bath, adjusting the temperature of the water bath to 40 ℃, and magnetically stirring until the mixture is evaporated to dryness to form blocks.

(4) And (3) putting the blocky mixture into a vacuum drying oven at 60 ℃ for drying for 2h, grinding, putting into a tube furnace, roasting at 400 ℃ for 8h in a nitrogen atmosphere, and cooling to room temperature in the tube furnace.

(5) Tabletting the roasted mixture by a tabletting machine, and sieving by a 40-60 mesh sieve to prepare the red mud-based desulfurizer.

Control group 3

(1) Drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 5g of red mud and 0.05g of polyethylene glycol, dissolving the polyethylene glycol in 25ml of water, pouring the red mud into the water, and uniformly stirring the mixture to obtain a mixture.

(3) Placing the magnetic rotor into a container containing the mixture, placing the container into a water bath, magnetically stirring for 12h at 25 ℃ in the water bath, adjusting the temperature of the water bath to 40 ℃, and magnetically stirring until the mixture is evaporated to dryness to form blocks.

(4) And (3) putting the blocky mixture into a vacuum drying oven at 60 ℃ for drying for 2h, grinding, putting into a tube furnace, roasting at 450 ℃ for 8h in a nitrogen atmosphere, and cooling to room temperature in the tube furnace.

(5) Tabletting the roasted mixture by a tabletting machine, and sieving by a 40-60 mesh sieve to prepare the desulfurizer.

Control group 4

(1) Drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 5g of red mud and 0.05g of polyethylene glycol, dissolving the polyethylene glycol in 25ml of water, pouring the red mud into the water, and uniformly stirring the mixture to obtain a mixture.

(3) Placing the magnetic rotor into a container containing the mixture, placing the container into a water bath, magnetically stirring for 12h at 25 ℃ in the water bath, adjusting the temperature of the water bath to 40 ℃, and magnetically stirring until the mixture is evaporated to dryness to form blocks.

(4) And (3) putting the blocky mixture into a vacuum drying oven at 60 ℃ for drying for 2h, grinding, putting into a tube furnace, roasting at 550 ℃ for 8h under the nitrogen atmosphere, and cooling to room temperature in the tube furnace.

(5) Tabletting the roasted mixture by a tabletting machine, and sieving by a 40-60 mesh sieve to prepare the desulfurizer.

As shown in FIG. 4, the inventors found that the desulfurization efficiency of the desulfurizing agent is directly affected by the high and low calcination temperature.

Example 4

The preparation method of the desulfurizing agent for purifying low-concentration carbonyl sulfide, described in this embodiment, includes the following specific steps:

(1) drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 5g of red mud and 0.05g of polyethylene glycol, dissolving the polyethylene glycol in 25ml of water, pouring the red mud into the water, and uniformly stirring the mixture to obtain a mixture.

(3) Placing the magnetic rotor into a container containing the mixture, placing the container into a water bath, magnetically stirring for 12h at 25 ℃ in the water bath, adjusting the temperature of the water bath to 40 ℃, and magnetically stirring until the mixture is evaporated to dryness to form blocks.

(4) And (3) putting the blocky mixture into a vacuum drying oven at 60 ℃ for drying for 2h, grinding, putting into a tube furnace, roasting at 500 ℃ for 8h under the nitrogen atmosphere, and cooling to room temperature in the tube furnace.

(5) Tabletting the roasted mixture by a tabletting machine, and sieving by a 40-60 mesh sieve to prepare the desulfurizer.

Taking 0.45g of prepared red mud-based desulfurizer, and filling the red mud-based desulfurizer into a fixed bed reactor, wherein the inner diameter of the fixed bed reactor is 6mm, and the volume space velocity of the fixed bed reactor is 10000h^-1Under the conditions of normal pressure, 80 ℃ of reaction temperature, 3.60 percent of reaction relative humidity and 100ppm of COS content, the removal rate of the COS is more than 99 percent.

Control group 1

(1) Drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 5g of red mud and 0.05g of polyethylene glycol, dissolving the polyethylene glycol in 25ml of water, pouring the red mud into the water, and uniformly stirring the mixture to obtain a mixture.

(3) Placing the magnetic rotor into a container containing the mixture, placing the container into a water bath, magnetically stirring for 12h at 25 ℃ in the water bath, adjusting the temperature of the water bath to 40 ℃, and magnetically stirring until the mixture is evaporated to dryness to form blocks.

(4) And (3) putting the blocky mixture into a vacuum drying oven at 60 ℃ for drying for 2h, grinding, putting into a tube furnace, roasting for 4h at 500 ℃ in a nitrogen atmosphere, and cooling to room temperature in the tube furnace.

(5) Tabletting the roasted mixture by a tabletting machine, and sieving by a 40-60 mesh sieve to prepare the red mud-based desulfurizer.

Control group 2

(1) Drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 5g of red mud and 0.05g of polyethylene glycol, dissolving the polyethylene glycol in 25ml of water, pouring the red mud into the water, and uniformly stirring the mixture to obtain a mixture.

(3) Placing the magnetic rotor into a container containing the mixture, placing the container into a water bath, magnetically stirring for 12h at 25 ℃ in the water bath, adjusting the temperature of the water bath to 40 ℃, and magnetically stirring until the mixture is evaporated to dryness to form blocks.

(4) And (3) putting the blocky mixture into a vacuum drying oven at 60 ℃ for drying for 2h, grinding, putting into a tube furnace, roasting at 500 ℃ for 12h in a nitrogen atmosphere, and cooling to room temperature in the tube furnace.

(5) Tabletting the roasted mixture by a tabletting machine, and sieving by a 40-60 mesh sieve to prepare the red mud-based desulfurizer.

Control group 3

(1) Drying the red mud in a drying oven at 105 ℃, sieving with a 200-mesh sieve, and storing for later use.

(2) Weighing 5g of red mud and 0.05g of polyethylene glycol, dissolving the polyethylene glycol in 25ml of water, pouring the red mud into the water, and uniformly stirring the mixture to obtain a mixture.

(3) Placing the magnetic rotor into a container containing the mixture, placing the container into a water bath, magnetically stirring for 12h at 25 ℃ in the water bath, adjusting the temperature of the water bath to 40 ℃, and magnetically stirring until the mixture is evaporated to dryness to form blocks.

(4) And (3) putting the blocky mixture into a vacuum drying oven at 60 ℃ for drying for 2h, grinding, putting into a tube furnace, roasting at 500 ℃ for 16h under the nitrogen atmosphere, and cooling to room temperature in the tube furnace.

(5) Tabletting the roasted mixture by a tabletting machine, and sieving by a 40-60 mesh sieve to prepare the red mud-based desulfurizer.

As shown in fig. 5, the inventors found that the length of the calcination time directly affects the desulfurization efficiency of the desulfurizing agent.

Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.