KR20150146479A - HCl removal agent and methods for preparation thereof - Google Patents

HCl removal agent and methods for preparation thereof Download PDF

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KR20150146479A
KR20150146479A KR1020150176312A KR20150176312A KR20150146479A KR 20150146479 A KR20150146479 A KR 20150146479A KR 1020150176312 A KR1020150176312 A KR 1020150176312A KR 20150176312 A KR20150176312 A KR 20150176312A KR 20150146479 A KR20150146479 A KR 20150146479A
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limestone
hcl
particle size
less
sodium carbonate
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KR1020150176312A
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KR101851437B1 (en
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빈성 후
춘옌 송
용리앙 귀
롱환 친
카이 루
쉐우 후
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허베이 유나이티드 유니버시티
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Treating Waste Gases (AREA)

Abstract

A method of producing a kind of HCl remover is to optimize rational process parameters with low cost industrial limestone, commercial sodium carbonate and potassium hydroxide as main raw materials, and to confirm the corresponding production method, and to control the calcination time of the industrial limestone, The pelletizing was carried out in the range of the desired finished product particle diameter to obtain a method of producing a HCl removing agent which is simple and easy to operate.

Description

HCl removal agents and methods for preparation thereof < RTI ID = 0.0 >

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a technical field of cleaning a combustion gas or coal gas with a complicated component and a high temperature, and more particularly, to a method of producing a kind of HCl remover.

As the amount of generated garbage in urban areas has increased, it has become necessary to provide a treatment method with a high processing capacity, detoxification and resource saving. As a result, the incineration power generation method has gradually replaced the conventional incineration method. Since chlorine-containing materials exist in urban household waste, HCl gas is contained in a certain concentration of combustion gas. Not only can this cause corrosive effects on flue ducts and metal parts of the incinerator, but it can also pollute the environment and harm the human body. In many HCI emission reduction control processes, tail gas purification treatment of waste incinerators can be relatively satisfied with emission standards. Therefore, the development of a new type of chlorine scavenger and its production method applied to the combustion gas characteristics has become a common concern to people.

As Korea's steel industry developed, especially the cost of production increased, many inexpensive iron ores began to be used with increasing attention. The amount of trace element, especially harmful element, is relatively high in cheap iron ore. If the content of chlorine element introduced into the blast furnace increases, the HCl content in the furnace coal gas also increases. There is no room. In recent years, metal members such as furnace coal gas pipes and TRT blades in each steel company have suffered from corrosion by HCl to different degrees. Therefore, a chlorine scavenger and its associated processes and techniques for removing HCl in blast furnace gases under dry dampening conditions have already become one of the hot issue issues that must be urgently addressed in the metallurgical field.

Although there has been a great deal of research on HCl removal in the fields of coal gasification combined cycle (IGCC), coal gasification fuel cell (MCFC), petrochemicals and refuse incineration, for example, when using fixed bed technology, Most alkaline HCl remover is mainly divided into limestone (limestone, asbestos and quicklime) and sodium groups (soda powder, sodium hydrogencarbonate). However, due to differences in combustion gas concentrations, flow rates and pressures generated in different industrial processes, these chlorine scavengers can not be fully applied to combustion gas and tail gas treatments such as waste incineration and furnace coal gas.

The present application focuses on the characteristics of high-temperature combustion gas and coal gas, which are complex in composition, based on the research of others in connection with the above background, and is used as a raw material of a low price, Invented a method for producing HCl remover which is fully applicable to coal gas.

It is an object of the present invention to provide a method for producing an HCl removing agent having a good HCl gas removing effect by using a raw material that is inexpensive.

In order to achieve the above object, the technology adopted by the present invention is as follows:

1) industrial limestone having a particle size of 5 mm or less, commercial sodium carbonate with a particle size of 3 mm or less and potassium hydroxide are used as raw materials for the production of HCl remover;

2) First, the industrial limestone sample is immersed in a potassium hydroxide solution at a concentration of 10% -15% for 1 hour, and then the limestone after the immersion is calcined at a high temperature of 700 ° C for 1-2 hours;

3) The calcined limestone and sodium carbonate obtained after calcination of limestone are pulverized to a particle size of 20 μm or less by using a ball milling process or other milling process, and light limestone: sodium carbonate = 30-70: 70-30 The mixture is preliminarily mixed for 10-15 minutes, and then the mixed powder is continuously polished by a milling process until the particle size of the powder reaches 80 탆 or less;

4) 3% of bentonite was added to the mixed powder, and the mixture was uniformly dry mixed. Pelletizing was carried out by adding water to the mixture using a disk-type granulator and then 3-10 mm of fine particles were selected for naturally drying Or by low-temperature drying under the condition of 100 DEG C to obtain an article of HCl remover.

Penetration time and once chlorine permeation capacity were measured for products made using the above method and selection of preferred process parameters has excellent performance by having a relatively long penetration time and a relatively high once chlorine permeation capacity in the product .

An advantage of the present invention is that the process is simple and easy to operate in that it provides a production method capable of producing a HCl remover excellent in performance using a raw material at a low price.

Hereinafter, the present invention will be described in detail with reference to specific experimental examples.

Experiment Example  One

1) industrial limestone having a particle size of less than 5 mm, commercial sodium carbonate having a particle size of less than 3 mm and potassium hydroxide as raw materials and used for the production of HCl remover;

2) A sample of limestone for industrial use was immersed in a potassium hydroxide solution of 10% concentration for 1 hour, and the limestone after dipping was calcined at a high temperature of 700 ° C for 1 hour;

3) The calcined limestone and sodium carbonate obtained after calcination of limestone are pulverized to 20 μm or less by using a ball milling process or other milling process, and mixed with light limestone: sodium carbonate = 30: 70 (weight percentage) Then, after premixing for 10 minutes, the mixed powder is continuously polished using a milling process until the particle size of the powder reaches 80 탆 or less;

4) 3% of bentonite was added to the prepared mixed powder, and the mixture was uniformly dry mixed. Pelletizing was performed by adding water to the mixture by using a disk-type granulating machine, and 3-10 mm fine particles were selected, Under conditions to obtain a finished article of HCl remover.

Experiment Example  2

1) industrial limestone having a particle size of less than 5 mm, commercial sodium carbonate having a particle size of less than 3 mm and potassium hydroxide as raw materials and used for the production of HCl remover;

2) The industrial limestone raw sample was immersed in a potassium hydroxide solution of 15% concentration for 1 hour, and then the limestone after the immersion was calcined at a high temperature condition of 700 ° C for 1 hour;

3) The calcined limestone and sodium carbonate obtained after calcination of limestone are pulverized to 20 μm or less by using a ball milling process or other milling process, and mixed with light limestone: sodium carbonate = 30: 70 (weight percentage) Then, after premixing for 10 minutes, the mixed powder is continuously polished using a milling process until the particle size of the powder reaches 80 탆 or less;

4) 3% of bentonite was added to the prepared mixed powder, and the mixture was uniformly dry mixed. Pelletizing was performed by adding water to the mixture by using a disk-type granulating machine, and 3-10 mm fine particles were selected, Under conditions to obtain a finished article of HCl remover.

Experiment Example  3

1) industrial limestone having a particle size of less than 5 mm, commercial sodium carbonate having a particle size of less than 3 mm and potassium hydroxide as raw materials and used for the production of HCl remover;

2) The industrial limestone source sample was immersed in a potassium hydroxide solution of 15% concentration for 1 hour, and the limestone after immersion was calcined at a high temperature of 700 ° C for 2 hours;

3) The calcined limestone and sodium carbonate obtained after calcination of limestone are pulverized to 20 μm or less by using a ball milling process or other milling process, and mixed with light limestone: sodium carbonate = 30: 70 (weight percentage) Then, after premixing for 10 minutes, the mixed powder is continuously polished using a milling process until the particle size of the powder reaches 80 탆 or less;

4) 3% of bentonite was added to the prepared mixed powder, and the mixture was uniformly dry mixed. Pelletizing was performed by adding water to the mixture by using a disk-type granulating machine, and 3-10 mm fine particles were selected, Under conditions to obtain a finished article of HCl remover.

Experiment Example  4

1) industrial limestone having a particle size of less than 5 mm, commercial sodium carbonate having a particle size of less than 3 mm and potassium hydroxide as raw materials and used for the production of HCl remover;

2) The industrial limestone source sample was immersed in a potassium hydroxide solution of 15% concentration for 1 hour, and the limestone after immersion was calcined at a high temperature of 700 ° C for 2 hours;

3) The calcined limestone and sodium carbonate obtained after calcination of limestone are pulverized to a particle size of 20 μm or less using a ball milling process or other milling process, and mixed with light limestone: sodium carbonate = 50: 50 (weight percentage) Then, after premixing for 15 minutes, the mixed powder is continuously polished by a milling process until the particle size of the powder reaches 80 탆 or less;

4) 3% of bentonite was added to the prepared mixed powder, and the mixture was uniformly dry mixed. Pelletizing was performed by adding water to the mixture by using a disk-type granulating machine, and 3-10 mm fine particles were selected, Under conditions to obtain a finished article of HCl remover.

Experiment Example  5

1) industrial limestone having a particle size of less than 5 mm, commercial sodium carbonate having a particle size of less than 3 mm and potassium hydroxide as raw materials and used for the production of HCl remover;

2) The industrial limestone source sample was immersed in a potassium hydroxide solution of 15% concentration for 1 hour, and the limestone after immersion was calcined at a high temperature of 700 ° C for 2 hours;

3) The calcined limestone and sodium carbonate obtained after calcination of limestone are ground to a particle size of 20 μm or less by using a ball milling process or other milling process and mixed with light limestone: sodium carbonate = 60:40 (weight percentage) Then, after premixing for 10 minutes, the mixed powder is continuously polished using a milling process until the particle size of the powder reaches 80 탆 or less;

4) 3% of bentonite was added to the prepared mixed powder, and the mixture was uniformly dry mixed. Pelletizing was performed by adding water to the mixture by using a disk-type granulating machine, and 3-10 mm fine particles were selected, Under conditions to obtain a finished article of HCl remover.

Experiment Example  6

1) industrial limestone having a particle size of less than 5 mm, commercial sodium carbonate having a particle size of less than 3 mm and potassium hydroxide as raw materials and used for the production of HCl remover;

2) The industrial limestone raw sample was immersed in a potassium hydroxide solution of 15% concentration for 1 hour, and the limestone after immersion was calcined at a high temperature condition of 700 ° C for 1.5 hours;

3) The calcined limestone and sodium carbonate obtained after calcination of limestone are pulverized to a size of 20 μm or less by using a ball milling process or other milling process, and mixed with light limestone: sodium carbonate = 70: 30 (weight percentage) And then preliminarily mixed for 13 minutes, and then the mixed powder is continuously polished by a milling process until the particle size of the powder reaches 80 탆 or less;

4) 3% of bentonite was added to the prepared mixed powder, and the mixture was uniformly dry mixed. Pelletizing was performed by adding water to the mixture by using a disk-type granulating machine, and 3-10 mm fine particles were selected, Under conditions to obtain a finished article of HCl remover.

Experiment Example  7

1) industrial limestone having a particle size of less than 5 mm, commercial sodium carbonate having a particle size of less than 3 mm and potassium hydroxide as raw materials and used for the production of HCl remover;

2) The industrial limestone raw sample was immersed in a potassium hydroxide solution of 15% concentration for 1 hour, and the limestone after immersion was calcined at a high temperature condition of 700 ° C for 1.5 hours;

3) Light limestone and sodium carbonate obtained after calcination of limestone are pulverized to a particle size of 20 μm or less by using a ball milling process or other milling process and mixed with light limestone: sodium carbonate = 40: 60 (weight percentage) And then preliminarily mixed for 105 min, and then the mixed powder is continuously polished by a milling process until the particle size of the powder reaches 80 탆 or less;

4) 3% of bentonite was added to the prepared mixed powder, and the mixture was uniformly dry mixed. Pelletizing was performed by adding water to the mixture by using a disk-type granulating machine, and 3-10 mm fine particles were selected, Under conditions to obtain a finished article of HCl remover.

Experiment Example  8

1) industrial limestone having a particle size of less than 5 mm, commercial sodium carbonate having a particle size of less than 3 mm and potassium hydroxide as raw materials and used for the production of HCl remover;

2) A sample of limestone for industrial use was immersed in a potassium hydroxide solution of 10% concentration for 1 hour, and then the limestone after dipping was calcined at a high temperature of 700 ° C for 2 hours;

3) The calcined limestone and sodium carbonate obtained after calcination of limestone are pulverized to a particle size of 20 μm or less using a ball milling process or other milling process, and mixed with light limestone: sodium carbonate = 50: 50 (weight percentage) And then preliminarily mixed for 12 minutes, and then the mixed powder is continuously polished by a milling process until the particle size of the powder reaches 80 탆 or less;

4) 3% of bentonite was added to the prepared mixed powder, and the mixture was uniformly dry mixed. Pelletizing was performed by adding water to the mixture by using a disk-type granulating machine, and 3-10 mm fine particles were selected, Under conditions to obtain a finished article of HCl remover.

Store the finished product granules produced in different process steps in a dry environment.

Performance evaluation index of HCl remover

HCl elimination Experimental procedure: HCl removal Put a certain amount of HCl remover product in the test apparatus and fix the HCl concentration in the combustion gas or coal gas. The experimental apparatus is filled with the test gas and the flow rate of the test gas is stably maintained so that the HCl remover product sufficiently reacts with the test gas in the experimental apparatus.

Breakthrough time: In the HCl removal test apparatus, if the HCl content in the tail gas exceeds 1 ppm after the flue gas or coal gas is purified through HCl, it is judged that the HCl remover has permeated and the HCl remover is infiltrated from the HCl injection The time to penetration of the HCl remover is up to.

Measuring method of permeation time: The HCl concentration at the exit of the fixed bed reactor was measured by controlling the flow rate of the test combustion gas or coal gas to 5 L / min and controlling the HCl concentration to 200 ppm, and the HCl concentration at the outlet portion reached 1 ppm Record the time you are doing.

Once the chlorine infiltration capacity, the chlorine infiltration capacity is defined as the amount of chlorine infiltration capacity of the solid HCl remover, which maintains the outlet HCl concentration of the reactor equal to the inlet HCl concentration for 10 minutes under a pressure of 0.1-0.3 Mpa, Chlorine absorption refers to the mass percentage. The HCl volume fraction at the inlet is 0.99%.

Measuring Method of Chlorine Infiltration Capacity: Experimental time was 30 min. 20 grains were randomly sampled and analyzed with a laser gas analyzer. The chlorine permeation capacity .

The penetration time of the different amounts of HCl remover is different and the longer the penetration time is, the better the actual reactivity of the HCl remover and the HCl in the combustion gas or the coal gas is, and if the thickness of the material layer is the same, It is more advantageous to remove HCl in the gas. The single chlorine permeation capacity of different amounts of HCl remover is different and the higher the single chlorine permeation capacity of the HCl remover is, the stronger the HCl removal ability of the HCl remover is in the combustion gas or coal gas.

Table 1 compares the measured results of the infiltration time and the chlorine infiltration capacity of one experiment in the eight experimental examples.

Table 1 Measurement results of penetration time and chlorine penetration capacity

Example No. Breakthrough time, min Once chlorine infiltration capacity,% One 409 5.87 2 412 5.89 3 415 5.91 4 404 5.86 5 397 5.86 6 393 5.85 7 411 5.90 8 403 5.85

As can be seen from the results in Table 1, the ratio of light limestone to sodium carbonate in the HCl remover has a significant effect on both the penetration time and the once chlorine permeation capacity, while the high temperature calcination time of light limestone also affects the HCl removal effect .

Compared with light limestone, Na 2 CO 3 and HCl can produce a certain amount of H 2 O, which has a relatively high once chlorine permeation capacity. Therefore, It affects.

Although limestone also has a good HCl removal effect, studies have shown that porosity is significantly increased due to partial decomposition after limestone has gone through a light load, and that improving the kinetics of the reaction with HCl also improves the HCl removal effect Thus, the present invention selected light limestone. There are a certain number of fine pores on the surface of the limestone, the diameter of the fine pores is between 20 and 100 μm, and the fine pore volume level within the unit square millimeter is within the range of 0 to 10 × 105. The gas molecule adsorption is selective (abbreviated polarity adsorption) and the micropores on the surface of the HCl remover are easily adsorbed by molecules of gas molecules whose diameters are similar to their micropore diameters. The molecular diameter of HCl is about 10 탆, which is relatively close to the diameter of the light limestone surface. Depending on the polarity adsorption principle, light limestone is easier to adsorb HCl molecules in the coal gas of the furnace than limestone, and furthermore, The chlorine permeation capacity can be increased. The high-temperature firing time necessarily affects the calcination effect, thus affecting the HCl removal capacity of the limestone.

KOH also has a predetermined HCl removal effect, but since it has both strong alkali and corrosive properties, it readily absorbs the surrounding water, forming deliquescence and forming an alkaline solution having a very high alkalinity, May result in serious adverse effects on pipelines and other accessory equipment. Therefore, the present invention is designed so that an appropriate amount of KOH is introduced to improve the HCl removal effect by applying light after immersing limestone without adding KOH.

Through the above experiments and analysis of results, it can be seen that the post-optimization procedure of the present application is based on the simple manufacturing process and the technical parameters, and the selection of a reasonable raw material is added to obtain a HCl remover for combustion gas or coal gas with excellent performance have. This can be applied to the metal smelting industry and the industrial fields such as the second power generation of waste incineration, effectively extending the service life of the equipment and reducing the production cost.

Claims (2)

In the method for producing HCl remover,
1) industrial limestone having a particle size of 5 mm or less, commercial sodium carbonate having a particle size of 3 mm or less and potassium hydroxide as raw materials and used for the production of HCl remover;
2) First, the industrial limestone sample is immersed in a potassium hydroxide solution at a concentration of 10% -15% for 1 hour, and then the limestone after the immersion is calcined at a high temperature of 700 ° C for 1-2 hours;
3) The calcined limestone and sodium carbonate obtained after calcination of limestone are pulverized to a particle size of 20 μm or less by using a ball milling process or other milling process, and light limestone: sodium carbonate = 30-70: 70-30 The mixture is preliminarily mixed for 10-15 minutes, and then the mixed powder is continuously polished by a milling process until the particle size of the powder reaches 80 탆 or less;
4) 3% of bentonite was added to the mixed powder, and the mixture was uniformly dry mixed. Pelletizing was performed by adding water to the pellet using a disk-type granulating machine, and then fine particles of 3-10 mm were selected and dried naturally Lt; RTI ID = 0.0 > 100 C < / RTI > to obtain an article of HCl remover. The method according to claim 1,
And the high-temperature baking time at 700 占 폚 in step (2) is 1.5 hours.
KR1020150176312A 2015-03-18 2015-12-10 HCl removal agent and methods for preparation thereof KR101851437B1 (en)

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CN105289242B (en) * 2015-09-25 2019-03-08 重庆长风化学工业有限公司 Sustained release neutralization method for hydrogen chloride gas
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