CN104707469A - Preparing method of novel HCl removal agent - Google Patents
Preparing method of novel HCl removal agent Download PDFInfo
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- CN104707469A CN104707469A CN201510118755.6A CN201510118755A CN104707469A CN 104707469 A CN104707469 A CN 104707469A CN 201510118755 A CN201510118755 A CN 201510118755A CN 104707469 A CN104707469 A CN 104707469A
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Abstract
The invention provides a preparing method of a novel HCl removal agent. Cheap industrial limestone, commercial sodium carbonate and potassium hydroxide are used as main raw materials, reasonable technical parameters are optimized, and a corresponding preparing method is made. The preparing method of the novel HCl removal agent is simple in steps and easy to operate, is obtained through controlling the forging time of the industrial limestone, pelletizing by a pan pelletizer and optimizing the diameter range of finished pellets.
Description
Technical field
The present invention relates to complicated ingredient and high-temperature flue gas or gas purification technical field, particularly a kind of novel HCl removes the preparation method of agent.
Background technology
The increase of Municipal Domestic Garbage Output, needs to find that a kind of disposal ability is large, innoxious, the processing method of resource.Take advantage of a situation and raw burning electricity generation method instead of traditional landfill method gradually.Due to the existence of chlorine-bearing compound in domestic waste, make in the flue gas of discharging containing certain density HCl gas.This not only can produce corrosiveness to the back-end ductwork of incinerator and hardware, but also contaminated environment and being detrimental to health.Reduce discharging in Controlling Technology at many HCl, garbage incinerator tail gas purified treatment can meet discharge standard preferably.So exploitation novel dechlorination sorbent being applicable to this smoke characteristic and preparation method thereof becomes the problem that people pay close attention to jointly.
Along with the development of China's steel and iron industry, the especially increase of production cost, many cheap iron ores receive to be paid close attention to and progressively brings into use.The content of the especially harmful element of the trace element in cheap iron ore is higher, and the content of Cl element particularly brought in blast furnace increases, and makes the HCl content in blast furnace gas also in rising trend, exacerbates the corrosion of pipeline and equipment undoubtedly.In recent years, the HCl that the hardware such as blast furnace gas pipeline, TRT blade of each iron and steel enterprise all receives in various degree corrodes.Therefore, study the antichlor removing HCl in blast furnace gas under dry method dust condition and related process and technology thereof and become one of field of metallurgy hot issue urgently to be resolved hurrily.
Although done in fields such as integrated coal gasification combined cycle (IGCC), coal gasified fuel battery (MCFC), petrochemical industry and waste incinerations the large quantity research removing HCl, such as utilize bed technology, HCl used removes agent and mostly is alkaline HCl and removes agent, is mainly divided into lime base (limestone, white lime and quick lime) and sodium base (soda ash, sodium bicarbonate).But the flue gas concentration, flow rate and the pressure that produce due to different industrial process are different, make these antichlors can not be applicable to such flue gas such as such as waste incineration and blast furnace gas etc. and vent gas treatment completely.
The application is for above-mentioned background and use for reference other people Research foundation, for the high-temperature flue gas of complicated component and the feature of coal gas, invent and a kind ofly utilize cheap raw material, HCl removal effect good and the novel HCl that can be applied to high-temperature flue gas or coal gas completely removes the preparation method of agent.
Summary of the invention
Namely object of the present invention is that providing a kind of utilizes cheap raw material, and the novel HCl that can reach good HCl gas removal effect removes the preparation method of agent.
For achieving the above object, the technical solution used in the present invention is:
One), select industrial lime stone, commercial sodium carbonate and potassium hydroxide to remove agent as raw material for the preparation of HCl, wherein the granularity of lime stone will at below 5mm, and the granularity of sodium carbonate and potassium hydroxide will at below 3mm;
Two), first industrial lime stone former state is soaked 1h through potassium hydroxide solution, wherein the concentration of potassium hydroxide solution is at 10%-15%, and then the lime stone after immersion is placed in the hot conditions calcining 1-2h of 700 DEG C;
Three), by calcining after lime stone (hereinafter referred to as soft burnt lime stone) and sodium carbonate conventional ball milling techniques or other flouring technologies levigate to less than 20 μm, again according to soft burnt lime stone: sodium carbonate=30-70: 70-30 (percentage by weight) prepares burden, then premix is carried out, incorporation time is 10-15min, flouring technology is utilized by the powder mixed to proceed grinding, until the granularity of all powder is all below 80 μm;
Four), with the mixed-powder made, with addition of the bentonite of 3%, mixing is dry mixed.Utilize disc balling machine, vaporific adding water carries out pelletizing, and the finished product bead of screening 3-10mm, dries naturally or low temperature drying obtains the finished product that HCl removes agent under 100 DEG C of conditions.
The product prepared utilizing said method carries out the mensuration of time of break-through and a breakthrough chlorine content, and the technological parameter optimized makes product have longer time of break-through and higher breakthrough chlorine content, excellent performance.
Advantage of the present invention have employed cheap raw material, proposes the preparation method that the novel HCl that can prepare excellent performance removes agent, and the method step is simple, be easy to operation.
Detailed description of the invention
Below, by concrete experiment embodiment, the present invention is described in detail.
Experiment embodiment 1
One), select industrial lime stone, commercial sodium carbonate and potassium hydroxide to prepare HCl as raw material to remove agent, wherein the granularity of lime stone is less than 5mm, and the granularity of sodium carbonate and potassium hydroxide is less than 3mm;
Two), by industrial lime stone former state soak 1h through potassium hydroxide solution, wherein the concentration of potassium hydroxide solution is 10%, and then the lime stone after immersion is placed in the hot conditions calcining 1h of 700 DEG C;
Three), by calcining after lime stone (hereinafter referred to as soft burnt lime stone) and sodium carbonate conventional ball milling techniques or other flouring technologies levigate to less than 20 μm, again according to soft burnt lime stone: sodium carbonate=30: 70 (percentage by weights) are prepared burden, then premix is carried out, incorporation time is 10min, flouring technology is utilized by the powder mixed to proceed grinding, until the granularity of all powder is all below 80 μm;
Four), with the mixed-powder made, with addition of the bentonite of 3%, mixing is dry mixed.Utilize disc balling machine, vaporific adding water carries out pelletizing, and the finished product bead of screening 3-10mm, under 100 DEG C of conditions, low temperature drying obtains HCl and removes agent product.
Experiment embodiment 2
One), select industrial lime stone, commercial sodium carbonate and potassium hydroxide to prepare HCl as raw material to remove agent, wherein the granularity of lime stone is less than 5mm, and the granularity of sodium carbonate and potassium hydroxide is less than 3mm;
Two), by industrial lime stone former state soak 1h through potassium hydroxide solution, wherein the concentration of potassium hydroxide solution is 15%, and then the lime stone after immersion is placed in the hot conditions calcining 1h of 700 DEG C;
Three), by calcining after lime stone (hereinafter referred to as soft burnt lime stone) and sodium carbonate conventional ball milling techniques or other flouring technologies levigate to less than 20 μm, again according to soft burnt lime stone: sodium carbonate=30: 70 (percentage by weights) are prepared burden, then premix is carried out, incorporation time is 10min, flouring technology is utilized by the powder mixed to proceed grinding, until the granularity of all powder is all below 80 μm;
Four), with the mixed-powder made, with addition of the bentonite of 3%, mixing is dry mixed.Utilize disc balling machine, vaporific adding water carries out pelletizing, and the finished product bead of screening 3-10mm, under 100 DEG C of conditions, low temperature drying obtains HCl and removes agent product.
Experiment embodiment 3
One), select industrial lime stone, commercial sodium carbonate and potassium hydroxide to prepare HCl as raw material to remove agent, wherein the granularity of lime stone is less than 5mm, and the granularity of sodium carbonate and potassium hydroxide is less than 3mm;
Two), by industrial lime stone former state soak 1h through potassium hydroxide solution, wherein the concentration of potassium hydroxide solution is 15%, and then the lime stone after immersion is placed in the hot conditions calcining 2h of 700 DEG C;
Three), by calcining after lime stone (hereinafter referred to as soft burnt lime stone) and sodium carbonate conventional ball milling techniques or other flouring technologies levigate to less than 20 μm, again according to soft burnt lime stone: sodium carbonate=30: 70 (percentage by weights) are prepared burden, then premix is carried out, incorporation time is 10min, flouring technology is utilized by the powder mixed to proceed grinding, until the granularity of all powder is all below 80 μm;
Four), with the mixed-powder made, with addition of the bentonite of 3%, mixing is dry mixed.Utilize disc balling machine, vaporific adding water carries out pelletizing, and the finished product bead of screening 3-10mm, under 100 DEG C of conditions, low temperature drying obtains HCl and removes agent product.
Experiment embodiment 4
One), select industrial lime stone, commercial sodium carbonate and potassium hydroxide to prepare HCl as raw material to remove agent, wherein the granularity of lime stone is less than 5mm, and the granularity of sodium carbonate and potassium hydroxide is less than 3mm;
Two), by industrial lime stone former state soak 1h through potassium hydroxide solution, wherein the concentration of potassium hydroxide solution is 15%, and then the lime stone after immersion is placed in the hot conditions calcining 2h of 700 DEG C;
Three), by calcining after lime stone (hereinafter referred to as soft burnt lime stone) and sodium carbonate conventional ball milling techniques or other flouring technologies levigate to less than 20 μm, again according to soft burnt lime stone: sodium carbonate=50: 50 (percentage by weights) are prepared burden, then premix is carried out, incorporation time is 15min, flouring technology is utilized by the powder mixed to proceed grinding, until the granularity of all powder is all below 80 μm;
Four), with the mixed-powder made, with addition of the bentonite of 3%, mixing is dry mixed.Utilize disc balling machine, vaporific adding water carries out pelletizing, and the finished product bead of screening 3-10mm, under 100 DEG C of conditions, low temperature drying obtains HCl and removes agent product.
Experiment embodiment 5
One), select industrial lime stone, commercial sodium carbonate and potassium hydroxide to prepare HCl as raw material to remove agent, wherein the granularity of lime stone is less than 5mm, and the granularity of sodium carbonate and potassium hydroxide is less than 3mm;
Two), by industrial lime stone former state soak 1h through potassium hydroxide solution, wherein the concentration of potassium hydroxide solution is 15%, and then the lime stone after immersion is placed in the hot conditions calcining 2h of 700 DEG C;
Three), by calcining after lime stone (hereinafter referred to as soft burnt lime stone) and sodium carbonate conventional ball milling techniques or other flouring technologies levigate to less than 20 μm, again according to soft burnt lime stone: sodium carbonate=60: 40 (percentage by weights) are prepared burden, then premix is carried out, incorporation time is 10min, flouring technology is utilized by the powder mixed to proceed grinding, until the granularity of all powder is all below 80 μm;
Four), with the mixed-powder made, with addition of the bentonite of 3%, mixing is dry mixed.Utilize disc balling machine, vaporific adding water carries out pelletizing, and the finished product bead of screening 3-10mm, under 100 DEG C of conditions, low temperature drying obtains HCl and removes agent product.
Experiment embodiment 6
One), select industrial lime stone, commercial sodium carbonate and potassium hydroxide to prepare HCl as raw material to remove agent, wherein the granularity of lime stone is less than 5mm, and the granularity of sodium carbonate and potassium hydroxide is less than 3mm;
Two), by industrial lime stone former state soak 1h through potassium hydroxide solution, wherein the concentration of potassium hydroxide solution is 15%, and then the lime stone after immersion is placed in the hot conditions calcining 1.5h of 700 DEG C;
Three), by calcining after lime stone (hereinafter referred to as soft burnt lime stone) and sodium carbonate conventional ball milling techniques or other flouring technologies levigate to less than 20 μm, again according to soft burnt lime stone: sodium carbonate=70: 30 (percentage by weights) are prepared burden, then premix is carried out, incorporation time is 13min, flouring technology is utilized by the powder mixed to proceed grinding, until the granularity of all powder is all below 80 μm;
Four), with the mixed-powder made, with addition of the bentonite of 3%, mixing is dry mixed.Utilize disc balling machine, vaporific adding water carries out pelletizing, and the finished product bead of screening 3-10mm, under 100 DEG C of conditions, low temperature drying obtains HCl and removes agent product.
Experiment embodiment 7
One), select industrial lime stone, commercial sodium carbonate and potassium hydroxide to prepare HCl as raw material to remove agent, wherein the granularity of lime stone is less than 5mm, and the granularity of sodium carbonate and potassium hydroxide is less than 3mm;
Two), by industrial lime stone former state soak 1h through potassium hydroxide solution, wherein the concentration of potassium hydroxide solution is 15%, and then the lime stone after immersion is placed in the hot conditions calcining 1.5h of 700 DEG C;
Three), by calcining after lime stone (hereinafter referred to as soft burnt lime stone) and sodium carbonate conventional ball milling techniques or other flouring technologies levigate to less than 20 μm, again according to soft burnt lime stone: sodium carbonate=40: 60 (percentage by weights) are prepared burden, then premix is carried out, incorporation time is 15min, flouring technology is utilized by the powder mixed to proceed grinding, until the granularity of all powder is all below 80 μm;
Four), with the mixed-powder made, with addition of the bentonite of 3%, mixing is dry mixed.Utilize disc balling machine, vaporific adding water carries out pelletizing, and the finished product bead of screening 3-10mm, under 100 DEG C of conditions, low temperature drying obtains HCl and removes agent product.
Experiment embodiment 8
One), select industrial lime stone, commercial sodium carbonate and potassium hydroxide to prepare HCl as raw material to remove agent, wherein the granularity of lime stone is less than 5mm, and the granularity of sodium carbonate and potassium hydroxide is less than 3mm;
Two), by industrial lime stone former state soak 1h through potassium hydroxide solution, wherein the concentration of potassium hydroxide solution is 10%, and then the lime stone after immersion is placed in the hot conditions calcining 2h of 700 DEG C;
Three), by calcining after lime stone (hereinafter referred to as soft burnt lime stone) and sodium carbonate conventional ball milling techniques or other flouring technologies levigate to less than 20 μm, again according to soft burnt lime stone: sodium carbonate=50: 50 (percentage by weights) are prepared burden, then premix is carried out, incorporation time is 12min, flouring technology is utilized by the powder mixed to proceed grinding, until the granularity of all powder is all below 80 μm;
Four), with the mixed-powder made, with addition of the bentonite of 3%, mixing is dry mixed.Utilize disc balling machine, vaporific adding water carries out pelletizing, and the finished product bead of screening 3-10mm, under 100 DEG C of conditions, low temperature drying obtains HCl and removes agent product.
The finished product bead utilizing different process process to prepare is placed for subsequent use in dry environments.
HCl removes the Performance Evaluating Indexes of agent
HCl removes experimentation: remove in experimental provision at HCl and put into a certain amount of HCl and remove agent product, the HCl concentration in fixing thickness of feed layer and flue gas or coal gas.In experimental provision, be filled with experimental gas, keep the flow of experimental gas relatively stable, make HCl remove agent product and fully react with experimental gas in experimental provision.
Time of break-through: remove in experimental provision at HCl, flue gas or coal gas, when HCl removes that after agent purification, in tail gas, HCl content is more than 1ppm, think that HCl removes agent and penetrated, and from passing into HCl to HCl, to remove agent by the time penetrated be the time of break-through that HCl removes agent.
The assay method of time of break-through: experiment flue gas or gas flow control as 5L/min, HCl concentration controls, for 200ppm, to measure the HCl concentration in fixed bed reactors exit, and record exit HCl concentration reaches the time of 1ppm.
A breakthrough chlorine content: breakthrough chlorine content refers in 0-300 DEG C of temperature range, under the pressure condition of 0.1-0.3MPa, reactor outlet HCl concentration equals import HCl concentration and keeps 10min, and solid HCl removes the quality percentage that agent absorbs chlorine.Import HCl volume fraction is 0.99%.
The assay method of a breakthrough chlorine content: experiment flue gas or coal gas intake are 5L/min, HCl concentration is 1000ppm, and test period is 30min, random taking-up 20 beads adopt gas laser analysis-e/or determining breakthrough chlorine content.
The time of break-through that different HCl removes agent is different, and time of break-through is longer, illustrates that this HCl removes the real reaction of the HCl in agent and flue gas or coal gas better, under identical thickness of feed layer, is more conducive to removing the HCl in flue gas or coal gas; Different HCl remove a breakthrough chlorine content difference of agent, and the breakthrough chlorine content that HCl removes agent is higher, illustrate to remove agent by HCl to remove the ability of HCl in flue gas or coal gas stronger.
Table 1 be classified as the measured result contrast of the time of break-through of 8 experiment embodiments and a breakthrough chlorine content.
The measurement result of table 1 time of break-through and a breakthrough chlorine content
Result listed by table 1, the ratio that HCl removes soft burnt lime stone and sodium carbonate in agent has obvious impact to time of break-through and a breakthrough chlorine content, and the high-temperature calcination time of soft burnt lime stone also affects the effect that HCl removes simultaneously.
Compared with soft burnt lime stone, Na
2cO
3a certain amount of H can be generated when reacting with HCl
2o, so have a higher breakthrough chlorine content, therefore, HCl removes the proportioning of the two in agent affects HCl removal effect.
Although lime stone also has good HCl removal effect, research finds, because lime stone is after light-burned, part is decomposed, and voidage obviously increases, and improves the dynamic conditions reacted with HCl, HCl removal effect also makes moderate progress, and therefore the present invention has selected soft burnt lime stone.Limestone surfaces has some micropores, and micro-pore diameter is between 20 ~ 100 μm, and in unit square millimeter, number cells magnitude is in 0 ~ 10 × 103 range intervals; The micropore that soft burnt lime stone has number ratio more, micro-pore diameter is in 0.1 ~ 20 μm of range intervals, and in unit square millimeter, number cells magnitude is in 0 ~ 10 × 105 range intervals.Gas molecule absorption has selective (being called for short polarity absorption), and HCl removes the molecule that in the easy adsorption gas molecule of agent surface micropore, diameter is close with self micro-pore diameter.The molecular diameter of HCl is at about 10 μm, comparatively close with soft burnt lime stone surface micropore diameter range, according to polarity absorption principle, the HCl molecule in soft burnt lime stone absorption easier than lime stone blast furnace gas, and then lime stone HCl can be improved remove agent breakthrough chlorine content.High-temperature calcination time gesture will inevitably affect calcining effect, thus the HCl affecting lime stone removes ability.
KOH also has certain HCl removal effect, but owing to having strong basicity and corrosivity, easily absorbs moisture generation deliquescence around, forms the aqueous slkali that alkalescence is very strong, can cause heavy corrosion to flue gas or gas piping and other auxiliary devices.Therefore the present invention is not with addition of KOH, but design soaks lime stone with it, and then carries out light-burned, to bring appropriate KOH into, improves HCl removal effect.
By above-mentioned experiment and interpretation of result known, under be optimize the simple preparation technology of rear step and technical parameter based on the application, add that rational raw material is selected, the flue gas or the coal gas HCl that just obtain excellent performance remove agent, the industrial circle such as metallurgy industry and waste incineration secondary electricity generation can be applicable to well, effectively extension device service life and reduce production cost.
Claims (3)
1. novel HCl removes a preparation method for agent, and it prepares primarily of following steps:
One), select industrial lime stone, commercial sodium carbonate and potassium hydroxide as raw material for the preparation of antichlor, wherein the granularity of lime stone will at below 5mm, and the granularity of sodium carbonate and potassium hydroxide will at below 3mm;
Two), first industrial lime stone former state is soaked 1h through potassium hydroxide solution, wherein the concentration of potassium hydroxide solution is at 10%-15%, and then the lime stone after immersion is placed in the hot conditions calcining 1-2h of 700 DEG C;
Three), by calcining after lime stone (hereinafter referred to as soft burnt lime stone) and sodium carbonate conventional ball milling techniques or other flouring technologies levigate to less than 20 μm, again according to soft burnt lime stone: sodium carbonate=30-70: 70-30 (percentage by weight) prepares burden, then premix is carried out, incorporation time is 10-15min, flouring technology is utilized by the powder mixed to proceed grinding, until the granularity of all powder is all below 80 μm;
Four), with the mixed-powder made, with addition of the bentonite of 3%, mixing is dry mixed.Utilize disc balling machine, vaporific adding water carries out pelletizing, and the finished product bead of screening 3-10mm, dries or low temperature drying obtains antichlor under 100 DEG C of conditions finished product naturally.
2. novel HCl according to claim 1 removes the preparation method of agent, it is characterized in that: 700 DEG C of high-temperature calcination times preferably two) in step are 1.5h.
3. novel HCl according to claim 1 removes the preparation method of agent, it is characterized in that: step 4) in have employed common disk pellet forming process, the finished product the small ball's diameter scope filtered out is 3-10mm, and naturally dries or low temperature drying under 100 DEG C of conditions.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510118755.6A CN104707469B (en) | 2015-03-18 | 2015-03-18 | A kind of preparation method of HCl scavenger |
| KR1020150176312A KR101851437B1 (en) | 2015-03-18 | 2015-12-10 | HCl removal agent and methods for preparation thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510118755.6A CN104707469B (en) | 2015-03-18 | 2015-03-18 | A kind of preparation method of HCl scavenger |
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| CN104707469A true CN104707469A (en) | 2015-06-17 |
| CN104707469B CN104707469B (en) | 2016-09-14 |
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| CN (1) | CN104707469B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105289242A (en) * | 2015-09-25 | 2016-02-03 | 重庆长风化学工业有限公司 | Sustained-release neutralizing method for hydrogen chloride gas |
| CN108602011A (en) * | 2015-12-30 | 2018-09-28 | 勒瓦研究开发股份有限公司 | Composition for purification flue gas |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1147977A (en) * | 1996-04-26 | 1997-04-23 | 湖北省化学研究所 | Refined antichlor and method for preparing same |
| JP2004255228A (en) * | 2003-02-24 | 2004-09-16 | Kishun Kin | Method for treating aqueous solution of halogen compound, acidic aqueous solution, or acidic gas, and its apparatus |
| US20080280750A1 (en) * | 2007-05-09 | 2008-11-13 | Pao-Chu Liu | Catalysts for treating acid and halogen gases and production methods thereof |
| CN101773768A (en) * | 2010-03-16 | 2010-07-14 | 长春惠工净化工业有限公司 | Dechlorinating agent used for removing HCl from gas by dry method and preparation method thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100344345C (en) | 2001-10-12 | 2007-10-24 | 旭硝子株式会社 | Method for removing halogen series gas |
-
2015
- 2015-03-18 CN CN201510118755.6A patent/CN104707469B/en not_active Expired - Fee Related
- 2015-12-10 KR KR1020150176312A patent/KR101851437B1/en active IP Right Grant
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1147977A (en) * | 1996-04-26 | 1997-04-23 | 湖北省化学研究所 | Refined antichlor and method for preparing same |
| JP2004255228A (en) * | 2003-02-24 | 2004-09-16 | Kishun Kin | Method for treating aqueous solution of halogen compound, acidic aqueous solution, or acidic gas, and its apparatus |
| US20080280750A1 (en) * | 2007-05-09 | 2008-11-13 | Pao-Chu Liu | Catalysts for treating acid and halogen gases and production methods thereof |
| CN101773768A (en) * | 2010-03-16 | 2010-07-14 | 长春惠工净化工业有限公司 | Dechlorinating agent used for removing HCl from gas by dry method and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105289242A (en) * | 2015-09-25 | 2016-02-03 | 重庆长风化学工业有限公司 | Sustained-release neutralizing method for hydrogen chloride gas |
| 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 |
| CN108602011A (en) * | 2015-12-30 | 2018-09-28 | 勒瓦研究开发股份有限公司 | Composition for purification flue gas |
Also Published As
| Publication number | Publication date |
|---|---|
| KR101851437B1 (en) | 2018-04-24 |
| CN104707469B (en) | 2016-09-14 |
| KR20150146479A (en) | 2015-12-31 |
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