CN105536701A - A preparing method of an agent for removing room-temperature gaseous organic sulfur - Google Patents
A preparing method of an agent for removing room-temperature gaseous organic sulfur Download PDFInfo
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- CN105536701A CN105536701A CN201510977954.2A CN201510977954A CN105536701A CN 105536701 A CN105536701 A CN 105536701A CN 201510977954 A CN201510977954 A CN 201510977954A CN 105536701 A CN105536701 A CN 105536701A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
- B01D2253/10—Inorganic adsorbents
- B01D2253/102—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/30—Sulfur compounds
- B01D2257/306—Organic sulfur compounds, e.g. mercaptans
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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Abstract
The invention relates to a preparing method of an agent for removing room-temperature gaseous organic sulfur. The method adopts crop straw, rice hulls and rice straw type agricultural waste biomass as raw materials, and includes steps of (1) carbonizing, (2) preparing a C-silica sol solution and (3) modifying with a metal oxide. The method utilizes carbon sources and silicon sources in agricultural waste, thus reducing the cost. A metal element is adopted for modification so that a prepared product is high in performance for removing the room-temperature gaseous organic sulfur and the removing rate and breakthrough sulfur capacity are greatly increased.
Description
Technical field
The present invention relates to desulfurizing agent, particularly relate to a kind of preparation method for the agent of normal temperature gas phase organic sulfur removal.
Background technology
Organic sulfur is extensively present in the gas secondary industrys such as oil plant, Gas Purification Factory, gas purification factory as cos, carbon disulfide, low-carbon (LC) mercaptan etc.In many production environments as in the industrial circles such as metallurgy, agricultural chemicals, rubber and viscose rayon, all use organic sulfur, in environment, also have the organic sulfur of trace.These organic sulfurs cause very large harm to human body and environment.In chemical process, organic sulfur meeting etching apparatus, causes catalyst poisoning, and then improves industrial cost.Its removal methods has dry removal and wet method to remove two large classes, and dry method is widely used in removing of low concentration sulfide in gas, wherein active carbon due to specific area large, wide material sources come into one's own.Because organic sulfur is in neutral or extremely weak acidity, chemical property is relatively stable, and thus active carbon carrys out organic sulfide removal as just physical absorbent, and there is the phenomenon of limit absorption limit desorb, removal efficiency is low, the problem that Sulfur capacity is low.
In order to improve removal efficiency and the Sulfur capacity of active carbon, the method for active carbon being carried out to modification is divided into two classes, and a kind of is the modification of surface physics architectural characteristic, as adopted microwave treatment.Another kind is the modification of surface chemical property, as adopted alkali or the method such as carried metal and compound thereof, changes the Acidity of Aikalinity on its surface.CN101318130A provides the active carbon of a kind of organic base, inorganic base and metal salt for removing cos, and the conversion ratio of cos reaches 90%.CN101972658 provides a kind of inorganic base and metal salt active carbon, and for removing cos, clearance reaches more than 90%.Said method is all to increase the alkalescence of activated carbon surface for target, and in the environment that sour gas and organic sulfur coexist, result of use is not good.
Therefore, be necessary to find more suitable can the modified activated carbon of effective organic sulfide removal to meet market demand.
Summary of the invention
The technical problem to be solved in the present invention is higher for current existing desulfurizing agent cost preparation, the problems such as bad desulfurization effects, thering is provided a kind of is raw material with agricultural wastes, through metal-modified, with low cost, method is simple, and clearance and Sulfur capacity improve greatly, are applied to the preparation method of normal temperature gas phase organic sulfur removal agent.
The technical solution adopted for the present invention to solve the technical problems is:
For a preparation method for normal temperature gas phase organic sulfur removal agent, the method comprises the following steps:
(1) carbonize
By dry, to pulverize and the agriculture waste biomass material sieved is placed in hydrothermal reaction kettle, add water, solid-liquid mass ratio is 1:500 ~ 1:3, stirs; Reactor is placed in 160 ~ 200 DEG C of baking ovens, heats 10 ~ 50 hours, be cooled to room temperature, by solids isolated by filtration, washing, dry carbide;
(2) C-silica sol liquid
Is added 1 ~ 20% sodium hydroxide solution in the carbide that step (1) is obtained, carbide and NaOH mass ratio are 1:0.1 ~ 1:2, and 75 ~ 95 DEG C add thermal agitation 6 ~ 8 hours, form C-silica sol liquid;
(3) metal oxide modified
Be under the stirring state of 45 ~ 65 DEG C in temperature, the metal salt solution of 0.5 ~ 2mol/L is slowly added dropwise in the C-silica sol liquid of step (2), metal salt solution and C-silica sol liquid mass ratio are 1:0.5 ~ 2, after dropwising, continue stirring 1 ~ 6 hour, then at 60 ~ 80 DEG C dry 8 ~ 48 hours, pulverize, spend deionized water to neutral, dry 2h at 100 DEG C, be transferred to 200 ~ 600 DEG C of calcinations in tube furnace and obtain modification biological activated carbon, namely this product is the agent of normal temperature gas phase organic sulfur removal.
As limitation of the invention, the agriculture waste biomass material described in step of the present invention (1) is stalk, rice husk or straw.
As limitation of the invention, slaine described in step of the present invention (3) is can form one or more of the nitrate of metallic elements of ferrum, cobalt, chromium, silver, copper, nickel, zinc or the platinum that π complexing is good for, sulfate, chlorate or acetate with element sulphur.
After adopting technique scheme, the beneficial effect that the present invention obtains is:
It is raw material that the present invention chooses agricultural crop straw, rice husk and straw class agriculture waste living beings, itself contain cellulose, hemicellulose, soluble saccharide, these are all prepare the suitable carbon raw material of active carbon, the stripping in the basic conditions of silicon in ash content is a kind of excellent adhesive and gel-type vehicle.And use waste biomass materials, can greatly reduce costs, method is simple, utilize the metallic element that can form π complexing strong with organic sulfur to carry out modification simultaneously, the physical absorption becoming active carbon is Characteristic Adsorption, greatly improve clearance and the Sulfur capacity of desulfurizing agent, be a kind of excellent be applied to normal temperature gas phase organic sulfur removal remove agent.
Detailed description of the invention
The present invention is further illustrated with the following Examples more below, but it is to be understood that these embodiments are only the use illustrated, and should not be interpreted as restriction of the invention process.
Embodiment 1
For a preparation method for normal temperature gas phase organic sulfur removal agent, realize by following steps:
(1) carbonize
Dry, to pulverize and the rice husk crossing 50 mesh sieves is placed in hydrothermal reaction kettle, wherein add water, solid-liquid mass ratio is 1:500, stirs; Reactor is placed in 200 DEG C of baking ovens, heats 50 hours, be cooled to room temperature, by solids isolated by filtration, washing, dry carbide;
(2) C-silica sol liquid is prepared
To add 20% sodium hydroxide solution in carbide, carbide and NaOH mass ratio are 1:0.1, and 75 DEG C add thermal agitation 6 hours, form C-silica sol liquid;
(3) metal oxide modified
Be under the stirring state of 45 DEG C in temperature, the cupric sulfate salt solution of 2mol/L is slowly added dropwise in C-silica sol liquid, copper-bath and C-silica sol liquid mass ratio are 1:0.5, after dropwising, continue stirring 1 hour, then at 80 DEG C dry 8 hours, pulverize, spend deionized water to neutral, drying 2 hours at 100 DEG C, to be transferred in tube furnace 300 DEG C of calcinations 2 hours, to obtain modification biological activated carbon.This desulfurizing agent is 25 DEG C in temperature, and air speed is 3000h
-1, be 267mg/m for content
3during carbonyl sulfide removal, 1mg/m can be removed to
3, working sulfur capacity is 78.41mg/g.
Embodiment 2
For a preparation method for normal temperature gas phase organic sulfur removal agent, realize by following steps:
(1) carbonize
Dry, to pulverize and the stalk crossing 50 mesh sieves is placed in hydrothermal reaction kettle, wherein add water, solid-liquid mass ratio is 1:500, stirs; Reactor is placed in 160 DEG C of baking ovens, heats 10 hours, be cooled to room temperature, by solids isolated by filtration, washing, dry carbide;
(2) C-silica sol liquid is prepared
To add 20% sodium hydroxide solution in carbide, carbide and NaOH mass ratio are 1:2, and 95 DEG C add thermal agitation 6 hours, form C-silica sol liquid;
(3) metal oxide modified
Be under the stirring state of 65 DEG C in temperature, the liquor argenti nitratis ophthalmicus of 0.5mol/L is slowly added dropwise in C-silica sol liquid, liquor argenti nitratis ophthalmicus and C-silica sol liquid mass ratio are 1:2, after dropwising, continue stirring 1 hour, then at 60 DEG C dry 48 hours, pulverize, spend deionized water to neutral, drying 2 hours at 100 DEG C, to be transferred in tube furnace 300 DEG C of calcinations 2 hours, to obtain modification biological activated carbon.This desulfurizing agent is 25 DEG C in temperature, and air speed is 3000h
-1, be 340mg/m for content
3during removal of carbon disulfide, 1mg/m can be removed to
3, working sulfur capacity is 34.8mg/g.
Embodiment 3
For a preparation method for normal temperature gas phase organic sulfur removal agent, realize by following steps:
(1) carbonize
Drying, pulverizing cross the maize straw of 50 mesh sieves and be placed in hydrothermal reaction kettle, wherein add water, solid-liquid mass ratio is 1:3, stirs; Reactor is placed in 200 DEG C of baking ovens, heats 10 hours, be cooled to room temperature, by solids isolated by filtration, washing, dry carbide;
(2) C-silica sol liquid is prepared
To add 1% sodium hydroxide solution in carbide, carbide and NaOH mass ratio are 1:0.1, and 75 DEG C add thermal agitation 6 hours, form C-silica sol liquid;
(3) metal oxide modified
Be under the stirring state of 65 DEG C in temperature, the nickel acetate solution of 2mol/L is slowly added dropwise in C-silica sol liquid, nickel acetate solution and C-silica sol liquid mass ratio are 1:2, after dropwising, continue stirring 6 hours, then at 60 DEG C dry 8 hours, pulverize, spend deionized water to neutral, drying 2 hours at 100 DEG C, to be transferred in tube furnace 600 DEG C of calcinations 2 hours, to obtain modification biological activated carbon.This desulfurizing agent is 25 DEG C in temperature, and air speed is 3000h
-1, be 100mg/m for content
3during carbonyl sulfide removal, 1mg/m can be removed to
3, working sulfur capacity is 88.9mg/g.
Embodiment 4
For a preparation method for normal temperature gas phase organic sulfur removal agent, realize by following steps:
(1) carbonize
Dry, to pulverize and the straw crossing 50 mesh sieves is placed in hydrothermal reaction kettle, wherein add water, solid-liquid mass ratio is 1:200, stirs; Reactor is placed in 180 DEG C of baking ovens, heats 40 hours, be cooled to room temperature, by solids isolated by filtration, washing, dry carbide;
(2) C-silica sol liquid
Is added 15% sodium hydroxide solution in the carbide that step (1) is obtained, carbide and NaOH mass ratio are 1:1, and 80 DEG C add thermal agitation 8 hours, form C-silica sol liquid;
(3) metal oxide modified
Be under the stirring state of 45 DEG C in temperature, be that the silver nitrate of 0.6mol/L and platinum nitrate solution (mol ratio of silver and platinum is 24:1) are slowly added dropwise in the C-silica sol liquid of step (2) by total concentration, metal salt solution and C-silica sol liquid mass ratio are 1:2, after dropwising, continue stirring 2 hours, then at 60 DEG C dry 8 hours, pulverize, spend deionized water to neutral, dry at 100 DEG C, be transferred to 600 DEG C of calcinations in tube furnace and obtain modification biological activated carbon.This desulfurizing agent is 25 DEG C in temperature, and air speed is 2000h
-1, be 400mg/m for content
3during removal of carbon disulfide, 1mg/m can be removed to
3, working sulfur capacity is 40.2mg/g.
Embodiment 5
For a preparation method for normal temperature gas phase organic sulfur removal agent, realize by following steps:
(1) carbonize
By dry, to pulverize and the rice husk sieved is placed in hydrothermal reaction kettle, add water, solid-liquid mass ratio is 1:3, stirs; Reactor is placed in 200 DEG C of baking ovens, heats 20 hours, be cooled to room temperature, by solids isolated by filtration, washing, dry carbide;
(2) C-silica sol liquid
Is added 15% sodium hydroxide solution in the carbide that step (1) is obtained, carbide and NaOH mass ratio are 1:0.5, and 65 DEG C add thermal agitation 7 hours, form C-silica sol liquid;
(3) metal oxide modified
Be under the stirring state of 65 DEG C in temperature, be that zinc chloride and the ferric chloride solution (mol ratio of iron and zinc is 1:1) of 1mol/L is slowly added dropwise in the C-silica sol liquid of step (2) by total concentration, metal salt solution and C-silica sol liquid mass ratio are 1:0.5, after dropwising, continue stirring 4 hours, then at 60 DEG C dry 20 hours, pulverize, spend deionized water to neutral, dry at 100 DEG C, be transferred to 400 DEG C of calcinations in tube furnace and obtain modification biological activated carbon.This desulfurizing agent is 25 DEG C in temperature, and air speed is 1000h
-1, be 200mg/m for content
3during carbonyl sulfide removal, 1mg/m can be removed to
3, working sulfur capacity is 67.8mg/g.
Embodiment 6
(1) carbonize
By dry, to pulverize and the straw sieved is placed in hydrothermal reaction kettle, add water, solid-liquid mass ratio is 1:100, stirs; Reactor is placed in 190 DEG C of baking ovens, heats 300 hours, be cooled to room temperature, by solids isolated by filtration, washing, dry carbide;
(2) C-silica sol liquid
Is added 5% sodium hydroxide solution in the carbide that step (1) is obtained, carbide and NaOH mass ratio are 1:1, and 95 DEG C add thermal agitation 6 hours, form C-silica sol liquid;
(3) metal oxide modified
Be under the stirring state of 50 DEG C in temperature, the cobaltous sulfate of total concentration 2mol/L and chromium nitrate solution (mol ratio of cobalt and chromium is 1:1) are slowly added dropwise in the C-silica sol liquid of step (2), metal salt solution and C-silica sol liquid mass ratio are 1:1.5, after dropwising, continue stirring 6 hours, then at 60 DEG C dry 24 hours, pulverize, spend deionized water to neutral, dry at 100 DEG C, be transferred to 500 DEG C of calcinations in tube furnace and obtain modification biological activated carbon.This desulfurizing agent is 25 DEG C in temperature, and air speed is 1000h
-1, be 325mg/m for content
3during carbonyl sulfide removal, 1mg/m can be removed to
3, working sulfur capacity is 94.4mg/g.
As can be seen from the above embodiments, what the present invention obtained removes agent for normal temperature gas phase organic sulfur, and when deviating from organic sulfur, clearance and working sulfur capacity are all high than method in the past, better effects if.
With above-mentioned according to desirable embodiment of the present invention for enlightenment, by above-mentioned description, relevant staff in the scope not departing from this invention technological thought, can carry out various change and amendment completely.The technical scope of this invention is not limited to the content on description, must determine its technical scope according to right.
Claims (3)
1., for a preparation method for normal temperature gas phase organic sulfur removal agent, it is characterized in that the method comprises the following steps:
(1) carbonize
By dry, to pulverize and the agriculture waste biomass material sieved is placed in hydrothermal reaction kettle, add water, solid-liquid mass ratio is 1:500 ~ 1:3, stirs; Reactor is placed in 160 ~ 200 DEG C of baking ovens, heats 10 ~ 50 hours, be cooled to room temperature, by solids isolated by filtration, washing, dry carbide;
(2) C-silica sol liquid
Is added 1 ~ 20% sodium hydroxide solution in the carbide that step (1) is obtained, carbide and NaOH mass ratio are 1:0.1 ~ 1:2, and 75 ~ 95 DEG C add thermal agitation 6 ~ 8 hours, form C-silica sol liquid;
(3) metal oxide modified
Be under the stirring state of 45 ~ 65 DEG C in temperature, the metal salt solution of 0.5 ~ 2mol/L is slowly added dropwise in the C-silica sol liquid of step (2), metal salt solution and C-silica sol liquid mass ratio are 1:0.5 ~ 2, after dropwising, continue stirring 1 ~ 6 hour, then at 60 ~ 80 DEG C dry 8 ~ 48 hours, pulverize, spend deionized water to neutral, dry 2h at 100 DEG C, be transferred to 200 ~ 600 DEG C of calcinations in tube furnace, obtain modification biological activated carbon, namely this product is the agent of normal temperature gas phase organic sulfur removal.
2. a kind of preparation method for the agent of normal temperature gas phase organic sulfur removal according to claim 1, is characterized in that the agriculture waste biomass material described in step (1) is stalk, rice husk or straw.
3. a kind of preparation method for the agent of normal temperature gas phase organic sulfur removal according to claim 1, slaine described in step (3) is can form one or more of the nitrate of metallic elements of ferrum, cobalt, chromium, silver, copper, nickel, zinc or the platinum that π complexing is good for, sulfate, chlorate or acetate with element sulphur.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105921111A (en) * | 2016-06-07 | 2016-09-07 | 马鞍山市顺达环保设备有限公司 | Efficient composite desulfurizer and preparation method thereof |
| CN109499530A (en) * | 2018-11-21 | 2019-03-22 | 常熟理工学院 | A kind of preparation method and applications of biomass active carbon nanometer composite material |
| CN110681363A (en) * | 2019-09-17 | 2020-01-14 | 太原工业学院 | Method for preparing corn straw adsorbent by microwave induced pyrolysis method |
| CN114192114A (en) * | 2021-12-28 | 2022-03-18 | 山东亮剑环保新材料有限公司 | Preparation method of metal ion modified activated carbon desulfurizer |
| CN114682211A (en) * | 2020-12-30 | 2022-07-01 | 丰益(上海)生物技术研发中心有限公司 | Modification method of activated carbon |
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| CN101318130A (en) * | 2008-07-10 | 2008-12-10 | 昆明理工大学 | Absorbent charcoal based catalyst for hydrolyzation and catalysis of carbonyl sulphur in low-temperature and preparation method thereof |
| CN102600850A (en) * | 2012-01-13 | 2012-07-25 | 昆明理工大学 | Method for preparing catalyst capable of being subjected to carbon oxysulfide removal and carbon disulfide removal simultaneously |
| CN102941066A (en) * | 2012-10-30 | 2013-02-27 | 陕西启源科技发展有限责任公司 | Preparation method of diesel oil desulphurization adsorbent by using rice husks |
| CN104307469A (en) * | 2014-09-29 | 2015-01-28 | 中国石油化工股份有限公司 | Desulfurization absorbent for deeply desulfurizing refined diesel oil and preparation method of desulfurization absorbent |
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2015
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Patent Citations (4)
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| CN101318130A (en) * | 2008-07-10 | 2008-12-10 | 昆明理工大学 | Absorbent charcoal based catalyst for hydrolyzation and catalysis of carbonyl sulphur in low-temperature and preparation method thereof |
| CN102600850A (en) * | 2012-01-13 | 2012-07-25 | 昆明理工大学 | Method for preparing catalyst capable of being subjected to carbon oxysulfide removal and carbon disulfide removal simultaneously |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105921111A (en) * | 2016-06-07 | 2016-09-07 | 马鞍山市顺达环保设备有限公司 | Efficient composite desulfurizer and preparation method thereof |
| CN109499530A (en) * | 2018-11-21 | 2019-03-22 | 常熟理工学院 | A kind of preparation method and applications of biomass active carbon nanometer composite material |
| CN110681363A (en) * | 2019-09-17 | 2020-01-14 | 太原工业学院 | Method for preparing corn straw adsorbent by microwave induced pyrolysis method |
| CN114682211A (en) * | 2020-12-30 | 2022-07-01 | 丰益(上海)生物技术研发中心有限公司 | Modification method of activated carbon |
| CN114192114A (en) * | 2021-12-28 | 2022-03-18 | 山东亮剑环保新材料有限公司 | Preparation method of metal ion modified activated carbon desulfurizer |
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| CN105536701B (en) | 2018-10-19 |
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