CN111394144A - Mercury remover and preparation method thereof - Google Patents
Mercury remover and preparation method thereof Download PDFInfo
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- CN111394144A CN111394144A CN202010177449.0A CN202010177449A CN111394144A CN 111394144 A CN111394144 A CN 111394144A CN 202010177449 A CN202010177449 A CN 202010177449A CN 111394144 A CN111394144 A CN 111394144A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10L—FUELS NOT OTHERWISE PROVIDED FOR; NATURAL GAS; SYNTHETIC NATURAL GAS OBTAINED BY PROCESSES NOT COVERED BY SUBCLASSES C10G, C10K; LIQUEFIED PETROLEUM GAS; ADDING MATERIALS TO FUELS OR FIRES TO REDUCE SMOKE OR UNDESIRABLE DEPOSITS OR TO FACILITATE SOOT REMOVAL; FIRELIGHTERS
- C10L3/00—Gaseous fuels; Natural gas; Synthetic natural gas obtained by processes not covered by subclass C10G, C10K; Liquefied petroleum gas
- C10L3/06—Natural gas; Synthetic natural gas obtained by processes not covered by C10G, C10K3/02 or C10K3/04
- C10L3/10—Working-up natural gas or synthetic natural gas
- C10L3/101—Removal of contaminants
-
- 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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/64—Heavy metals or compounds thereof, e.g. mercury
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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
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/81—Solid phase processes
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- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a mercury removing agent, which takes an aluminum oxide tooth sphere or an aluminum oxide sphere as a carrier material, wherein the carrier material is loaded with 12-14% of an active substance CuS, or the carrier material is also loaded with 1.5-6% of an active substance ZnS. The demercuration effect of the demercuration agent is as follows: the mercury content can be reduced to 28 mu g/m after penetrating 20cm of the thickness of the mercury removing agent3Hereinafter, the duration was 28 days. The mercury content can be reduced to 0.01 mu g/m after penetrating 30cm of the thickness of the mercury removing agent3The duration is 34 days. The mercury capacity can reach 6.5 percent.
Description
Technical Field
The invention relates to the technical field of demercuration, in particular to a copper-zinc demercuration agent applied to natural gas and a preparation method thereof.
Background
Most natural gas fields in the world contain elementary mercury and mercury compounds, and the mercury content in natural gas is generally 1 mu g/m3~200μg/m3. In low-temperature systems such as natural gas liquefaction, condensate recovery and the like, mercury not only corrodes an aluminum plate-fin heat exchanger, but also poisons a noble metal catalyst in the natural gas chemical industry. Mercury and its compounds have high toxicity, mainly can cause diseases of nervous system, and mercury discharge can be circulated in biosphere, and with the development of petroleum industry, the harm of mercury to human body and environment is more and more obvious. The mercury content in the natural gas of the pipe-transported commodity of China specified by the middle petroleum is less than 28 mu g/m3The mercury in the foreign commodity natural gas is controlled to be 0.01 mu g/m3~10μg/m3Even so, the existing domestic mercury removal technology can not meet the control requirement of the mercury content in the natural gas of the pipeline transportation commodity in China.
At present, the natural gas demercuration technology mainly comprises chemical adsorption, solution absorption, low-temperature separation, anion resin and membrane separation and the like. The chemical adsorption demercuration process is widely applied to natural gas demercuration devices at home and abroad. At present, more mercury removing agents are used, such as sulfur-carrying activated carbon, metal sulfides, metal oxides and silver-carrying molecular sieves. The technical scheme is based on the theory that copper-zinc oxide has good removal effect on various industrial tail gases and toxic agents as a combined oxidation catalyst in the production process of other catalysts, and the oxides of the copper-zinc oxide are reserved according to a proportion to prepare the metal oxides and sulfides and enable the mercury removing agent to carry out oxidation adsorption on mercury.
Disclosure of Invention
The invention aims to provide a novel mercury removing agent, which ensures the accurate control of product components by selecting a proper carrier and aiming at the replacement improvement of chemical components and process technology, loads metal sulfide and a small amount of metal oxide on the carrier and ensures the stable existence of mercury removing active substances in a normal state and a specific environment.
The invention is realized by adopting the following technical scheme:
1. a copper mercury removing agent takes aluminum oxide tooth spheres or aluminum oxide spheres as a carrier material, and the carrier material is loaded with 12-14% of an active substance CuS (based on the mass of the product mercury removing agent).
The preparation method of the copper mercury removing agent comprises the following steps:
(1) solution preparation
Heating ammonia water serving as a solvent to 50-60 ℃, adding a cosolvent ammonium bicarbonate, adding basic copper carbonate after the dissolution is finished, dissolving to form a copper ammonia solution, and standing for more than 2 hours at 50-60 ℃ to form a solution A, wherein the proportion of the basic copper carbonate (kg), the ammonium bicarbonate (kg) and the ammonia water (L) = 20-25: 10-13: 100 is added;
(2) and dipping the mixture
Taking an aluminum oxide tooth sphere or an aluminum oxide sphere with the diameter of 3-5 mm as a carrier, taking the solution A as an impregnation liquid, soaking for 30min according to the proportion of the carrier to the solution =1 (kg): 1 (L), filtering out the impregnation material, and directly calcining;
(3) and calcining
The activation adopts a fluidized bed furnace: placing the impregnated material on a screen plate, passing air flow at 180 ℃ from the lower part through the screen plate to enable the material to be in a boiling state, adjusting the air flow speed to enable the material temperature to be raised to 130-150 ℃ within 30-40 minutes, maintaining the temperature for 25-50 min, and discharging;
(4) and vulcanizing
Under normal temperature, putting the material under pure hydrogen sulfide flow for vulcanization, so that most of copper oxide loaded in the calcined material is converted into copper sulfide; the vulcanization process is finished in 2.5-3 hours by taking the material weight gain of 5% as an end point.
2. A copper-zinc mercury removing agent takes aluminum oxide tooth spheres or aluminum oxide spheres as carrier materials, and the carrier materials are loaded with 12-14% of active substance CuS (calculated by the mass of the product mercury removing agent) and 1.5-6% of active substance ZnS (calculated by the mass of the product mercury removing agent).
The preparation method of the copper-zinc mercury removing agent comprises the following steps:
(1) solution preparation
Heating ammonia water serving as a solvent to 50-60 ℃, adding a cosolvent ammonium bicarbonate, adding basic copper carbonate after the dissolution is finished, dissolving to form a copper ammonia solution, wherein the adding proportion is that basic copper carbonate (kg), ammonium bicarbonate (kg), ammonia water (L) = 20-25: 10-13: 100, and standing for more than 2 hours at 50-60 ℃ to form a solution A;
heating ammonia water serving as a solvent to 50-60 ℃, adding a cosolvent ammonium bicarbonate, adding basic zinc carbonate after the ammonium bicarbonate is dissolved, and adding an alkali zinc solution after the basic zinc carbonate is dissolved, wherein the adding proportion is as follows: basic zinc carbonate (kg), ammonium bicarbonate (kg), ammonia =12:9:120 to form a solution B;
mixing the solution A and the solution B according to a volume ratio of 25:3, stirring completely, and standing for more than 2 hours at 50-60 ℃ to form a solution C;
(2) impregnation process
Taking an aluminum oxide tooth sphere or an aluminum oxide sphere with the diameter of 3-5 mm as a carrier, taking a C solution as an impregnation liquid, soaking for 30min according to the proportion of the carrier to the solution =1 (kg): 1 (L), filtering out the impregnation material, and directly calcining;
(3) and calcining
Adopting a fluidized bed furnace: placing the impregnated material on a screen plate, passing air flow at 180 ℃ from the lower part through the screen plate to enable the material to be in a boiling state, adjusting the air flow speed to enable the material temperature to be increased to 130-150 ℃ within 30-40 minutes and maintain for 25-50 min, then increasing the temperature to 160-165 ℃ and maintain for 25min, and discharging;
(4) and vulcanizing
The method comprises the steps of putting a material under a pure hydrogen sulfide flow at normal temperature for vulcanization, so that most of copper-zinc oxide loaded in the calcined material is converted into sulfide (copper sulfide and zinc sulfide), the vulcanization process is finished at the end point of 5.7% of weight gain of the material, and the vulcanization process is finished within 2.5-3 h.
The mercury removing agent prepared by the invention has the following advantages:
1. the mercury removing agent has high reaction and adsorption effects on mercury and compounds.
2. The mercury remover has a stable and highly dispersed reaction phase.
3. The mercury is adsorbed in the carrier in a stable form and no mercurides are emitted into the atmosphere.
4. The mercury capacity of the adsorbent is high, and is obviously superior to similar products at home and abroad.
The invention has reasonable design and good practical application value.
Detailed Description
The following provides a detailed description of specific embodiments of the present invention.
1. The mercury removing principle of the mercury removing agent is as follows
Hg + MXSY→MSSY -1+ HgS (catalytic upgrading with copper zinc sulphide).
2. Process for the validation of support materials
1) Taking activated carbon as a carrier: the method mainly loads the coal columnar activated carbon, the crushed coal activated carbon and the coconut shell activated carbon with sulfides, and the sulfide molecules are large and loaded in the activated carbon to influence the adsorption effect on mercury, so that the evaluation adsorption rate is low.
2) And preparing the mercury removing agent by a direct balling process: the metal sulfide and the adhesive are mixed in a certain proportion for molding, the strength and the adsorption performance of a sample molded by mixing cannot reach preset indexes, the material waste is more, and the process is not suitable for preparing the mercury removing agent.
3) And selecting a carrier: the active alumina ball is a porous solid material with high dispersity and has a large specific surface area, and the microporous surface of the active alumina ball has the characteristics required by catalytic action. Finally, according to the application conditions of the mercury removing agent and the technical requirements of the mercury removing agent, the aluminum oxide sphere or the aluminum oxide tooth sphere is determined to be a carrier for preparing the natural gas mercury removing agent.
3. Establishment of active Material Loading Pattern
According to the demercuration principle, the active substance of the demercuration agent is determined to be metal sulfide, and direct impregnation cannot be realized because the metal sulfide is a solid insoluble substance. So that the copper and zinc are loaded on the carrier material by impregnation according to a preset proportion in the form of an ammoniated complex of copper and zinc, and then the metal sulfide is loaded on the surface of the carrier material by the processes of calcination and vulcanization.
4. Sample optimization
According to the determined process, the metal content of the load is continuously changed, the load capacity of the metal sulfide is optimized, the calcining temperature, the calcining time and the vulcanization degree are optimized, the process scheme that the proportioning is carried out in the range of 9: 1-2 of the ratio of copper to zinc is finally determined, the temperature is increased to 130-150 ℃ within 30-40 minutes and is maintained for a set time, then the temperature is increased to 150-170 ℃ and is maintained for a set time is finally determined, and the sample is trial-produced to obtain the mercury removing agent sample with better performance.
5. The product is prepared by the following steps
5.1, the component ratio of the product is as follows:
5.2, a manufacturing process:
the sample preparation process comprises the following steps: solution preparation, impregnation, calcination and vulcanization.
5.2.1, solution preparation process:
heating ammonia water serving as a solvent to 50-60 ℃, adding a cosolvent ammonium bicarbonate, adding basic copper carbonate after the dissolution is finished, and dissolving to form a copper ammonia solution (the adding proportion is basic copper carbonate (Kg): ammonium bicarbonate (Kg): ammonia water (L) = 20-25: 10-13: 100), and standing for more than 2 hours at 50-60 ℃ to form a solution A (for TG-1 and TG-3).
Heating ammonia water serving as a solvent to 50-60 ℃, adding a cosolvent ammonium bicarbonate, adding basic zinc carbonate after the dissolution is finished, and dissolving the alkali zinc carbonate to form a solution B (the ratio of the added basic zinc carbonate (Kg): ammonium bicarbonate (Kg): ammonia water =12:9: 120).
Mixing the solution A and the solution B in a volume ratio of 25:3, stirring completely, and standing at 50-60 ℃ for more than 2h to form a solution C (for TG-4 and TG-5).
5.2.2 impregnation Process
TG-1, soaking the spherical alumina body with the diameter of 3-5 mm serving as a carrier material and the solution A serving as a soaking solution according to the proportion of the carrier solution =1 (kg): 1 (L) for 30min, filtering out the soaking material, directly calcining and not standing.
TG-3: the same TG-1 is adopted, but the carrier adopts an aluminum oxide tooth sphere with the diameter of 3-5 mm.
TG-4: the same TG-1 but the solution was C solution.
TG-5: the same as TG-4, but the carrier adopts an aluminum oxide tooth sphere with the diameter of 3-5 mm.
5.2.3 calcination procedure
Activating TG-1 and TG-3 samples by adopting a fluidized bed furnace: placing the impregnated material on a screen plate, passing air flow of 180 ℃ through the screen plate from the lower part to enable the material to be in a boiling state, adjusting the air flow speed to enable the material temperature to be raised to 130-150 ℃ within 30-40 minutes, maintaining the temperature for 25-50 min, and discharging.
Activating TG-4 and TG-5 samples by adopting a fluidized bed furnace: placing the impregnated material on a screen plate, passing 180 ℃ air flow through the screen plate from the lower part to enable the material to be in a boiling state, adjusting the air flow speed to enable the material temperature to be increased to 130-150 ℃ within 30-40 minutes and maintain for 25-50 min, then increasing the temperature to 160-165 ℃ and maintain for 25min, and discharging.
5.2.4 vulcanization Process
The four samples have the same vulcanizing process, and the materials are vulcanized by placing the materials under pure hydrogen sulfide flow at normal temperature, so that the copper-zinc oxide loaded in the calcined materials is converted into copper-zinc sulfide. The method is characterized in that the vulcanization process of the TG-1 and TG-3 materials takes the material weight gain of 5% as an end point, the vulcanization process of the TG-4 and TG-5 materials takes the material weight gain of 5.7% as an end point, the vulcanization process is an exothermic reaction, and the ventilation speed of hydrogen sulfide and the reaction temperature need to be strictly controlled, so that the vulcanization process is completed within 2.5-3 hours.
6. Performance detection
The performance detection of the demercuration agent comprises the steps of sequentially passing gas with a certain mercury content through 4 groups of detection tubes, wherein each group of detection tubes is connected with 7 adsorption tubes filled with the demercuration agent in series, the ambient temperature is 24-28 ℃, the gas flow rate is 1.0-2.0L/min, the tube diameter of each adsorption tube is 1.5cm, the length is 10 cm., the gas mercury content in front of and behind each adsorption tube is detected at regular intervals, so that the demercuration effect of the demercuration agent can be known, the demercuration performance detection process lasts for 34 days, data analysis is carried out at regular time every day, and data are displayed at regular intervals of every 10 days, as shown in table 1:
TABLE 1 parallel detection of four groups of mercury removing agent samples
The desulfurization effect TG-5 is more than TG-3 and more than TG-4 is more than TG-1 in the four samples through detection, and the comprehensive analysis shows that the TG-5 type mercury removing agent has excellent performance.
The specific demercuration effect of sample TG-5 is: the mercury content can be reduced to 28 mu g/m after penetrating 20cm of the thickness of the mercury removing agent3Hereinafter, the duration was 28 days. The mercury content can be reduced to 0.01 mu g/m after penetrating 30cm of the thickness of the mercury removing agent3The duration is 34 days. The mercury capacity can reach 6.5 percent.
Unless otherwise specified, the technical means used in the present invention are well known to those skilled in the art. In addition, the embodiments should be considered illustrative, and not restrictive, of the scope of the invention, which is defined solely by the claims. It will be apparent to those skilled in the art that various changes or modifications in the components and amounts of the materials used in these embodiments can be made without departing from the spirit and scope of the invention.
Claims (4)
1. A mercury removing agent, which is characterized in that: the method comprises the following steps of taking an aluminum oxide tooth sphere or an aluminum oxide sphere as a carrier material, and loading 12-14% of an active substance CuS on the carrier material.
2. A mercury remover as claimed in claim 1, wherein: the carrier material is also loaded with 1.5-6% of active material ZnS.
3. A method for preparing a mercury removing agent according to claim 1, which is characterized in that: the method comprises the following steps:
(1) solution preparation
Heating ammonia water serving as a solvent to 50-60 ℃, adding a cosolvent ammonium bicarbonate, adding basic copper carbonate to dissolve after the dissolution is finished to form a copper ammonia solution, and standing for more than 2 hours at 50-60 ℃ to form a solution A, wherein the proportion of the basic copper carbonate (kg), the ammonium bicarbonate (kg) and the ammonia water (L) = 20-25: 10-13: 100 is that;
(2) and dipping the mixture
Taking an aluminum oxide tooth sphere or an aluminum oxide sphere with the diameter of 3-5 mm as a carrier, taking the solution A as an impregnation liquid, soaking for 30min according to the proportion of the carrier to the solution =1 (kg): 1 (L), filtering out the impregnation material, and directly calcining;
(3) and calcining
The activation adopts a fluidized bed furnace: placing the impregnated material on a screen plate, passing air flow at 180 ℃ from the lower part through the screen plate to enable the material to be in a boiling state, adjusting the air flow speed to enable the material temperature to be raised to 130-150 ℃ within 30-40 minutes, maintaining the temperature for 25-50 min, and discharging;
(4) and vulcanizing
Under normal temperature, putting the material under pure hydrogen sulfide flow for vulcanization, so that copper oxide loaded in the calcined material is converted into copper sulfide; the material vulcanization process is finished at the end point of 5% of material weight increase, and the vulcanization process is finished within 2.5-3 h.
4. A method for preparing a mercury removing agent according to claim 2, characterized in that: the method comprises the following steps:
(1) solution preparation
Heating ammonia water serving as a solvent to 50-60 ℃, adding a cosolvent ammonium bicarbonate, adding basic copper carbonate after the dissolution is finished, dissolving to form a copper ammonia solution, wherein the adding proportion is that basic copper carbonate (kg), ammonium bicarbonate (kg), ammonia water (L) = 20-25: 10-13: 100, and standing for more than 2 hours at 50-60 ℃ to form a solution A;
heating ammonia water serving as a solvent to 50-60 ℃, adding a cosolvent ammonium bicarbonate, adding basic zinc carbonate after the ammonium bicarbonate is dissolved, and adding an alkali zinc solution after the basic zinc carbonate is dissolved, wherein the adding proportion is as follows: basic zinc carbonate (kg), ammonium bicarbonate (kg), ammonia =12:9:120 to form a solution B;
mixing the solution A and the solution B according to a volume ratio of 25:3, stirring completely, and standing for more than 2 hours at 50-60 ℃ to form a solution C;
(2) impregnation process
Taking an aluminum oxide tooth sphere or an aluminum oxide sphere with the diameter of 3-5 mm as a carrier, taking a C solution as an impregnation liquid, soaking for 30min according to the proportion of the carrier to the solution =1 (kg): 1 (L), filtering out the impregnation material, and directly calcining;
(3) and calcining
Adopting a fluidized bed furnace: placing the impregnated material on a screen plate, passing air flow at 180 ℃ from the lower part through the screen plate to enable the material to be in a boiling state, adjusting the air flow speed to enable the material temperature to be increased to 130-150 ℃ within 30-40 minutes and maintain for 25-50 min, then increasing the temperature to 160-165 ℃ and maintain for 25min, and discharging;
(4) and vulcanizing
The method comprises the steps of putting a material under a pure hydrogen sulfide flow at normal temperature for vulcanization, so that copper-zinc oxide loaded in the calcined material is converted into sulfide, the material vulcanization process takes 5.7% of weight gain of the material as an end point, and the vulcanization process is completed within 2.5-3 h.
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