CN115318076A - Preparation method of high-precision high-sulfur-capacity desulfurizer at normal temperature - Google Patents
Preparation method of high-precision high-sulfur-capacity desulfurizer at normal temperature Download PDFInfo
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- CN115318076A CN115318076A CN202211260298.0A CN202211260298A CN115318076A CN 115318076 A CN115318076 A CN 115318076A CN 202211260298 A CN202211260298 A CN 202211260298A CN 115318076 A CN115318076 A CN 115318076A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/48—Sulfur compounds
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Abstract
The invention belongs to the field of a preparation method of a desulfurizer, and particularly relates to a preparation method of a desulfurizer with high precision and high sulfur capacity at normal temperature, which comprises the following steps: carrying out oxidation pretreatment on the iron oxide yellow coarse powder in an alkaline solution, and washing the pretreated iron oxide yellow, carrying out filter pressing by a filter press and drying to obtain a desulfurization dry base; then fully mixing the activated carbon powder and the binder to obtain a mixture; then putting the desulfurization dry basis into a mixer for full kneading; when the materials are fully kneaded, uniform and easy to form, the materials are made into required specifications through a strip extruding machine; the pre-treated iron oxide yellow desulfurization dry powder has fluffy materials and the specific surface area of the iron oxide yellow desulfurization dry powder is more than or equal to 350m 2 Per gram, further increase the effective contact surface between hydrogen sulfide molecules and the desulfurizerAnd the unit binding efficiency of the desulfurizer is improved.
Description
Technical Field
The invention belongs to the field of a preparation method of a desulfurizer, and particularly relates to a preparation method of a desulfurizer with high precision and high sulfur capacity at normal temperature.
Background
Along with the gradual increase of the demand of industrial and civil natural gas in recent years, a large amount of oil and gas fields at home and abroad are exploited, the demand of a desulfurizer is increased, the dry-process desulfurizer appearing in the market has various varieties, the desulfurization range and the desulfurization precision are greatly differentiated, the content of effective desulfurization components is insufficient, the total desulfurization amount is lower, customers are frequently replaced in industrial practical application, the hardening is serious, the agent is difficult to discharge, and certain economic loss is caused to enterprises, so that the development of the desulfurizer with high precision and high sulfur capacity at normal temperature is urgent.
At present, most of the dry-method normal-temperature desulfurizer in the market takes one or more raw materials of ferric oxide, zinc oxide, manganese oxide and ferro-calcium powder as main components to prepare various types of desulfurizer. Under normal temperature, the iron oxide desulfurizer is mainly used for the reasons of economy, easy synthesis of raw materials and the like, but under most conditions, the iron oxide desulfurizer is generally applied to the working conditions of low space velocity, low precision of an outlet desulfurizer and the like in industry, and the sulfur capacity and the desulfurization precision of the practical industrial application are seriously reduced for the working conditions of high space velocity, high hydrogen sulfide content and the like.
Among a plurality of desulfurizing agents in China, particularly the iron-based desulfurizing agent prepared by taking iron oxide as a raw material has lower desulfurizing effect than the processed raw material desulfurizing agent under the conditions of large space velocity and high content of hydrogen sulfide because of lower impurities and specific surface area of the iron-based raw material, and the desulfurizing amount and the desulfurizing precision are seriously reduced. The zinc-based desulfurizer prepared by using zinc oxide as a raw material has low penetrating sulfur capacity and frequent replacement at normal temperature, and is less applied to a rough-removing process in oil and gas fields, coal chemical industry and the like because of higher zinc oxide price and the like, so that the further application of the zinc-based desulfurizer is limited. For example, chinese patent document CN 102794088B discloses a method for preparing a spherical high sulfur capacity desulfurizer and a product thereof, the patent technology is to mix iron oxyhydroxide, a ball nut and a binder, gradually form a ball, prepare a high sulfur capacity desulfurizer with good diffusivity, qualitatively detect the outlet gas after desulfurization in 1% silver nitrate solution, and the penetration sulfur capacity can reach about 40%. However, after being placed for a period of time, the surface of the ball is smooth and dense, so that in the actual industrial application process, the gas bias flow is serious, the precision is poor, the same problem exists in laboratory evaluation, and the iron-based spherical desulfurizing agent is rarely used in industry at present. For example, chinese patent CN106268219A discloses an iron oxide fine desulfurizing agent and a preparation and application method thereof, which is prepared by mixing ferrous sulfate heptahydrate, calcium hydroxide, anhydrous copper sulfate, sodium hydroxide, bentonite and sodium carboxymethylcellulose, extruding into strips and drying. However, the technology of the patent shows that the iron oxide fine desulfurizer in the scheme has lower obvious effective components and limits the characteristic of high sulfur capacity of the iron oxide fine desulfurizer.
In conclusion, how to further improve the content of effective components and the desulfurization precision of the desulfurizer, improve the sulfur penetration capacity and reduce the cost of enterprise operation cost, thereby obtaining the high-precision high-sulfur-capacity desulfurizer, which is a technical problem to be solved in the field at present.
Disclosure of Invention
In order to overcome the defects in the background, the invention provides a preparation method of a desulfurizer with high precision and high sulfur capacity at normal temperature. The technical problems to be solved are to overcome the problems of low content of effective components, low sulfur penetration capacity and low precision of the normal-temperature desulfurizer in the prior art.
In order to achieve the purpose, the technical solution of the invention is as follows:
the invention provides a preparation method of a desulfurizer with high precision and high sulfur capacity at normal temperature, which comprises the following raw materials of iron oxide yellow coarse powder, activated carbon powder, a binder, alkali liquor and a dispersant, wherein the weight ratio of the activated carbon powder, the binder and the iron oxide yellow coarse powder in a preparation mixture of the desulfurizer with high precision and high sulfur capacity at normal temperature is (5-30). The preparation method comprises the following steps:
a. carrying out oxidation pretreatment on the iron oxide yellow coarse powder and a dispersing agent in an alkaline solution, and washing, filter-pressing and drying the pretreated iron oxide yellow to obtain a desulfurization dry basis;
b. fully mixing the activated carbon powder and the binder to obtain a mixture;
c. b, putting the desulfurization dry basis obtained in the step a into a mixture for kneading;
d. fully kneading the mixture evenly and easily molding the mixture to prepare a molding product with the required specification;
e. and drying and screening the formed product to obtain a desulfurizer product.
Preferably, the alkaline solution is a solution prepared from one or more of sodium hydroxide, sodium carbonate and ammonium bicarbonate, and the dispersant is one or more of sodium sulfonate and disodium hydrogen phosphate.
Preferably, in step b, the activated carbon powder: the specific surface area is more than or equal to 800 square meters per gram.
Preferably, in step b, the binder is one or more of sesbania gum and cellulose powder.
Preferably, in the steps a and b, the weight ratio of the activated carbon powder to the binder to the iron oxide yellow coarse powder is (10-30): (2-10): 180-240).
Preferably, the gauge is one or more of a cylinder, a hemp strip, and an irregular shape.
Preferably, in the step e, the drying temperature is 60-90 ℃, and the drying time is 40-120 minutes.
Further, the conditions of the pretreatment in the step a are as follows: 1. The pH of the solution is controlled at 9-10 and the temperature is controlled at 40 ℃. 2. Controlling the oxidation ventilation rate at 0.5-2 m/h and controlling the pretreatment oxidation time at 2-5h.
Further, the water washing in the step a) adopts a pH =6-8, and the temperature: and (4) normal temperature to 40 ℃.
Specifically, the iron oxide yellow coarse powder and alkali are prepared into slurry or solution with a certain concentration, meanwhile, a dispersing agent is added into the slurry, the iron oxide yellow is subjected to oxidation pretreatment in the alkaline solution, and the pretreated iron oxide yellow is subjected to multi-stage water washing, filter pressing and drying to obtain pure iron oxide yellow desulfurization dry powder. And carrying out full dry mixing and wet mixing on the desulfurized dry powder, the activated carbon powder and the sodium cellulose, and extruding and molding the obtained mixture through a strip extruder to obtain the desulfurizing agents with different shapes and particle sizes.
Because the sulfur capacity of the iron oxide yellow coarse powder is low, the impurities are more, and the sulfur capacity is low when the iron oxide yellow coarse powder is used for desulfurization, the iron oxide yellow coarse powder is subjected to further oxidation pretreatment in an alkaline solution. Purpose of adding small amount of dispersant during the oxidative pretreatment: the crude iron oxide yellow is more uniformly distributed in the liquid solution, the rapid oxidation is promoted, the agglomeration is not easy to occur, and meanwhile, the specific surface area of the treated desulfurization dry powder is larger, and the hydrogen sulfide is easier to absorb and remove.
Further, the drying temperature is controlled to be 60-90 ℃, and the time is controlled to be 40-120min.
The application of the high-precision high-sulfur capacity desulfurizer is characterized in that the desulfurizer is applied to removal of hydrogen sulfide in synthesis ammonia raw gas, carbon dioxide raw gas and oil-gas field raw gas and can adsorb a certain amount of carbonyl sulfide.
Has the advantages that:
A. the iron oxide yellow desulfurization dry powder pretreated by the method is fluffy, the specific surface area is more than or equal to 350m < 2 >/g, the effective contact area of hydrogen sulfide molecules and a desulfurizer is further increased, and the unit combination efficiency of the desulfurizer is improved.
B. Most desulfurizing agents are cylindrical in specification and shape, smooth in surface, and neutral or alkaline. The most preferable specification and shape of the desulfurizer is strip-shaped, the treated iron oxide yellow desulfurization dry powder has stronger alkalinity (PH = 8-9), and the smooth dissociation of the hydrogen sulfide needs to be carried out in an alkaline environment, so that the dissociation of the hydrogen sulfide is promoted, and the hydrogen sulfide is more easily captured to react with the desulfurizer. And part of the activated carbon powder is added, so that the activated carbon powder has higher porosity, higher total desulfurization amount and better precision.
C. The desulfurizer of the invention realizes the characteristics of high sulfur capacity and high precision in practical industrial application, is convenient to fill and unload, is more convenient for long-term use of users, reduces frequent agent replacement, and has higher economic benefit.
Detailed Description
Firstly, iron oxide yellow coarse powder is pretreated, the purpose of the pretreatment is to ensure that the effective iron content of the iron oxide yellow coarse powder is higher, the iron oxide yellow coarse powder has larger specific surface area and better desulfurization and adsorption effects, and the method comprises the following specific steps:
scheme I for pretreating coarse iron oxide yellow powder raw material
1) Firstly, accurately weighing a certain amount of crude iron oxide yellow and soda ash, preparing the crude iron oxide yellow into slurry of about 20%, preparing the soda ash into the concentration of about 5%, adding a small amount of dispersant into an iron oxide yellow preparation tank (the adding amount of the dispersant accounts for 0.005% of the proportion of the iron oxide yellow), respectively conveying the mixture into an oxidation kettle through a conveying pump, and performing further oxidation pretreatment in an alkaline solution (purpose: the active iron content of the desulfurized dry powder is higher, the specific surface area of the treated desulfurized dry powder is larger, and hydrogen sulfide is easier to absorb and remove), and the pretreated iron oxide yellow is subjected to multi-stage water washing, filter pressing and drying to obtain pure desulfurized dry powder.
) After washing, the salt content in the desulfurization dry powder is controlled to be less than or equal to 1 percent, the desulfurization effect is better, and the precision is better.
) This product was used as feed 1.
Scheme II for pretreating coarse powder raw material of iron oxide yellow (II)
1) Firstly, accurately weighing a certain amount of crude iron oxide yellow and flake caustic soda, preparing the crude iron oxide yellow into slurry of about 20%, preparing the flake caustic soda into concentration of about 2.5%, adding a small amount of dispersant into an iron oxide yellow preparation tank (the adding amount of the dispersant accounts for 0.005% of the iron oxide yellow), respectively conveying the mixture into an oxidation kettle through a conveying pump, and performing further oxidation pretreatment in an alkaline solution (purpose: the active iron content of the desulfurized dry powder is higher, the specific surface area of the treated desulfurized dry powder is larger, and hydrogen sulfide is easier to absorb and remove), and the pretreated iron oxide yellow is subjected to multi-stage washing, pressure of a filter press and drying to obtain pure desulfurized dry powder.
2) After washing, the salt content in the desulfurization dry powder is controlled to be less than or equal to 1 percent, the desulfurization effect is better, and the precision is better.
3) This product was used as feed 2.
(III) iron oxide yellow coarse powder raw material pretreatment scheme III
1) Firstly, accurately weighing a certain amount of crude iron oxide yellow and ammonium bicarbonate, preparing the crude iron oxide yellow into slurry of about 20%, preparing calcined soda into concentration of about 5%, adding a small amount of dispersant into an iron oxide yellow preparation tank (the adding amount of the dispersant accounts for 0.005% of the iron oxide yellow), respectively conveying the mixture into an oxidation kettle through a conveying pump, and performing further oxidation pretreatment in an alkaline solution (purpose: the active iron content of the desulfurized dry powder is higher, the specific surface area of the treated desulfurized dry powder is larger, and hydrogen sulfide is easier to absorb and remove), and the pretreated iron oxide yellow is subjected to multistage washing, pressure of a filter press and drying to obtain pure desulfurized dry powder.
) After washing, the salt content in the desulfurization dry powder is controlled to be less than or equal to 1 percent, the desulfurization effect is better, and the precision is better.
3) This product was used as feed 3.
(IV) iron oxide yellow coarse powder raw material pretreatment scheme IV
1) Firstly, accurately weighing a certain amount of crude iron oxide yellow, sodium carbonate, sodium hydroxide and ammonium bicarbonate, preparing the crude iron oxide yellow into slurry of about 20 percent, preparing alkali into the concentration of about 5 percent, adding a small amount of dispersant into an iron oxide yellow preparation tank (the adding amount of the dispersant accounts for 0.005 percent of the proportion of the iron oxide yellow), respectively conveying the mixture into an oxidation kettle through a conveying pump, and carrying out further oxidation pretreatment in an alkaline solution (purpose: the active iron content of the desulfurized dry powder is higher, the specific surface area of the treated desulfurized dry powder is larger, and hydrogen sulfide is easier to absorb and remove), and the pretreated iron oxide yellow is subjected to multi-stage washing, pressure of a filter press and drying to obtain pure desulfurized dry powder.
) After washing, the salt content in the desulfurization dry powder is controlled to be less than or equal to 1 percent, the desulfurization effect is better, and the precision is better.
3) This product was used as feed 4.
Example 1:
(1) 20kg of fresh water is added into a kneader through a metering pump in advance, 200kg of the dried raw material 1 iron oxide yellow desulfurization dry powder is weighed through an electronic scale, and the kneader is started to knead for a plurality of minutes and then the operation is stopped. And then respectively weighing 10kg of active carbon powder and 6kg of sodium carboxymethylcellulose, respectively adding the active carbon powder and the sodium carboxymethylcellulose into a kneader to fully knead, and adding proper water according to the dryness and wetness degrees in the kneading process to facilitate molding.
(2) And (2) extruding the mixture obtained in the step (1) into strips through a strip extruding machine to form the strips, wherein the strips are hemp strips in the embodiment, and then drying the strips for 60min at the temperature of about 80 ℃ to obtain the high-precision high-sulfur capacity desulfurizer.
(3) The method comprises the steps of grinding the dried desulfurizer by using a mortar, sieving the ground desulfurizer by using a 80-mesh sieve, weighing 1mL (about 0.8 g) of the desulfurizer as a sample, adding dropwise water to moisten the sample (the added water amount is 7% -10% of the sample amount), uniformly filling the sample into a glass reaction tube with the filling height of 3cm to 4cm, connecting one end of the glass reaction tube to a hydrogen sulfide gas steel cylinder for providing hydrogen sulfide standard gas (the hydrogen sulfide content is 4.0 +/-0.2%, and the balance is nitrogen) for the glass reaction tube, connecting the other end of the glass reaction tube to a reactor of 0.02mol/L silver nitrate solution, finally connecting the reactor to a wet gas flowmeter, recording the initial value of the wet gas flowmeter, then opening a valve of the hydrogen sulfide gas steel cylinder, controlling the flow rate to be 200 Nm/h-400 Nm/h, observing the condition of the glass reaction tube at any time in a test, observing the bubbling speed, closing the valve to stop the test when black precipitate just appears in the reactor filled with silver nitrate, recording the end value of the gas flowmeter, and recording the end value of the wet gas flowmeter, wherein the difference between the end value of the wet gas flowmeter and the initial value is measured as the penetration rate of the sulfur capacity of the desulfurizer, and the sulfur penetration of 48.5% of the wet desulfurizer in the embodiment.
Example 2:
(1) 20kg of fresh water is added into a kneader through a metering pump in advance, 200kg of the dried raw material 2 iron oxide yellow desulfurization dry powder is weighed through an electronic scale, and the kneader is started to knead for a plurality of minutes and then the operation is stopped. And respectively weighing 10kg of activated carbon powder and 6kg of sodium carboxymethylcellulose, respectively adding into a kneader for fully kneading, and adding proper water amount according to the dryness and wetness degree in the kneading process to facilitate molding.
(2) And (2) extruding the mixture obtained in the step (1) into strips through a strip extruding machine to form the strips, wherein the strips are hemp strips in the embodiment, and then drying the strips for 60min at the temperature of about 80 ℃ to obtain the high-precision high-sulfur capacity desulfurizer.
(3) The method comprises the steps of grinding the dried desulfurizer by using a mortar, sieving the ground desulfurizer by using an 80-mesh sieve, weighing 1mL (about 0.8 g) of the desulfurizer as a sample, adding dropwise water to moisten the sample (the added water amount is 7% -10% of the sample amount), uniformly filling the sample into a glass reaction tube with the filling height of 3cm to 4cm, connecting one end of the glass reaction tube to a hydrogen sulfide gas steel cylinder for providing hydrogen sulfide standard gas (the hydrogen sulfide content is 4.0 +/-0.2%, and the balance is nitrogen) for the glass reaction tube, connecting the other end of the glass reaction tube to a reactor of 0.02mol/L silver nitrate solution, finally connecting the reactor to a wet gas flowmeter, recording the initial value of the wet gas flowmeter, then opening a valve of the hydrogen sulfide gas steel cylinder, controlling the flow rate to be 200 Nm/h-400 Nm/h, observing the condition of the glass reaction tube at any time in a test, observing the bubbling speed, closing the valve to stop the test when black precipitate just appears in the reactor filled with silver nitrate, recording the end value of the gas flowmeter, and recording the end value of the wet gas flowmeter, wherein the difference between the end value of the wet gas flowmeter and the initial value is 43.43% of the sulfur penetration of the desulfurizer.
Example 3:
(1) 20kg of fresh water is added into a kneader through a metering pump in advance, 200kg of the dried raw material 3 iron oxide yellow desulfurization dry powder is weighed through an electronic scale, and the kneader is started to knead for a plurality of minutes and then the operation is stopped. And respectively weighing 10kg of activated carbon powder and 6kg of sodium carboxymethylcellulose, respectively adding into a kneader for fully kneading, and adding proper water amount according to the dryness and wetness degree in the kneading process to facilitate molding.
(2) And (2) extruding the mixture obtained in the step (1) into strips through a strip extruding machine to form the strips, wherein the strips are hemp strips in the embodiment, and then drying the strips for 60min at the temperature of about 80 ℃ to obtain the high-precision high-sulfur capacity desulfurizer.
(3) The method comprises the steps of grinding the dried desulfurizer by using a mortar, screening the ground desulfurizer by using an 80-mesh screen, weighing 1mL (about 0.8 g) of the ground desulfurizer as a sample, dripping water to moisten the sample (the water addition amount is 7% -10% of the sample amount), uniformly filling the sample into a glass reaction tube, wherein the filling height is 3cm to 4cm, one end of the glass reaction tube is connected with a hydrogen sulfide gas steel cylinder and used for supplying hydrogen sulfide standard gas (the hydrogen sulfide content is 4.0 +/-0.2%, and the balance is nitrogen) to the glass reaction tube, the other end of the glass reaction tube is connected with a reactor of 0.02mol/L of silver nitrate solution, the reactor is finally connected to a wet gas flowmeter, recording the initial value of the wet gas flowmeter, then opening a valve of the hydrogen sulfide gas steel cylinder, controlling the flow rate to be 200 Nm/h-400 Nm/h, observing the condition of the glass reaction tube at any time in the test, the bubbling speed, closing the valve to stop the test when black precipitate appears in the reactor filled with the silver nitrate, recording the end value of the gas flowmeter, and measuring the difference between the end value of the wet gas flowmeter and the initial value of the wet gas flowmeter, namely the sulfur capacity of the desulfurizer, wherein the penetration rate is just 50.4.4% of the wet desulfurizer in the embodiment.
Example 4:
(1) 20kg of fresh water is added into a kneader through a metering pump in advance, 200kg of the dried sample 4 iron oxide yellow desulfurized dry powder is weighed through an electronic scale, and the kneader is started to knead for a plurality of minutes and then the operation is stopped. And respectively weighing 10kg of activated carbon powder and 6kg of sodium carboxymethylcellulose, respectively adding into a kneader for fully kneading, and adding proper water amount according to the dryness and wetness degree in the kneading process to facilitate molding.
(2) And (2) extruding the mixture obtained in the step (1) into strips through a strip extruding machine for molding, and then drying the strips for 60min at about 80 ℃ to obtain the high-precision high-sulfur capacity desulfurizer.
(3) The method comprises the steps of grinding the dried desulfurizer by using a mortar, sieving the ground desulfurizer by using an 80-mesh sieve, weighing 1mL (about 0.8 g) of the desulfurizer as a sample, adding dropwise water to moisten the sample (the added water amount is 7% -10% of the sample amount), uniformly filling the sample into a glass reaction tube with the filling height of 3cm to 4cm, connecting one end of the glass reaction tube to a hydrogen sulfide gas steel cylinder for providing hydrogen sulfide standard gas (the hydrogen sulfide content is 4.0 +/-0.2%, and the balance is nitrogen) for the glass reaction tube, connecting the other end of the glass reaction tube to a reactor of 0.02mol/L silver nitrate solution, finally connecting the reactor to a wet gas flowmeter, recording the initial value of the wet gas flowmeter, then opening a valve of the hydrogen sulfide gas steel cylinder, controlling the flow rate to be 200 Nm/h-400 Nm/h, observing the condition of the glass reaction tube at any time in a test, observing the bubbling speed, closing the valve to stop the test when black precipitate just appears in the reactor filled with silver nitrate, and recording the end value of the gas flowmeter, wherein the difference between the end value of the wet gas flowmeter and the initial value is measured as the penetration rate of the sulfur capacity of the desulfurizer in this embodiment, and the sulfur capacity is 46.8% of the sulfur.
Example 5:
(1) Adding 20kg of fresh water into a kneader through a metering pump in advance, weighing 180kg of the dried sample 1 iron oxide yellow desulfurized dry powder through an electronic scale, starting the kneader and kneading for a plurality of minutes, and stopping. And then respectively weighing 5kg of active carbon powder and 5kg of sodium carboxymethylcellulose, respectively adding the active carbon powder and the sodium carboxymethylcellulose into a kneader to fully knead, and adding proper water according to the dryness and wetness degrees in the kneading process to facilitate molding.
(2) And (2) extruding the mixture obtained in the step (1) into strips through a strip extruding machine to form a random lattice shape in the embodiment, and then drying the mixture for 40min at about 90 ℃ to obtain the high-precision high-sulfur capacity desulfurizer.
(3) The method comprises the steps of grinding the dried desulfurizer by using a mortar, screening the ground desulfurizer through an 80-mesh screen, weighing 1mL (about 0.8 g) of the ground desulfurizer as a sample, adding dropwise water to moisten the sample (the water addition amount is 7% -10% of the sample amount), uniformly filling the sample into a glass reaction tube, wherein the filling height is 3cm to 4cm, one end of the glass reaction tube is connected with a hydrogen sulfide gas steel cylinder and used for supplying hydrogen sulfide standard gas (the hydrogen sulfide content is 4.0 +/-0.2%, and the balance is nitrogen) to the glass reaction tube, the other end of the glass reaction tube is connected with a reactor of 0.02mol/L of silver nitrate solution, the reactor is finally connected to a wet gas flowmeter, recording the initial value of the wet gas flowmeter, then opening a valve of the hydrogen sulfide gas steel cylinder, controlling the flow rate to be 200 Nm/h-400 Nm/h, observing the condition of the glass reaction tube at any time in the test, the bubbling speed, closing the valve to stop the test when black precipitate appears in the reactor filled with the silver nitrate, recording the end value of the gas flowmeter, and measuring the difference between the end value of the wet gas flowmeter and the initial value of the wet gas flowmeter, namely, wherein the penetration rate of the desulfurizer in the wet gas flowmeter is just 47.5.5% of the wet desulfurizer.
Example 6:
(1) 230kg of iron oxide yellow desulfurization dry powder of a sample 3, 20kg of activated carbon powder and 9kg of sodium carboxymethylcellulose are respectively weighed and added into a kneader to be fully kneaded, and proper water is added according to the dryness and wetness degrees in the kneading process to facilitate molding.
(2) And (2) extruding the mixture obtained in the step (1) into a cylindrical shape in the embodiment through a strip extruding machine, and drying at about 90 ℃ for 40min to obtain the high-precision high-sulfur capacity desulfurizer.
(3) The method comprises the steps of grinding the dried desulfurizer by using a mortar, sieving the ground desulfurizer by using an 80-mesh sieve, weighing 1mL (about 0.8 g) of the desulfurizer as a sample, adding dropwise water to moisten the sample (the added water amount is 7% -10% of the sample amount), uniformly filling the sample into a glass reaction tube with the filling height of 3cm to 4cm, connecting one end of the glass reaction tube to a hydrogen sulfide gas steel cylinder for providing hydrogen sulfide standard gas (the hydrogen sulfide content is 4.0 +/-0.2%, and the balance is nitrogen) for the glass reaction tube, connecting the other end of the glass reaction tube to a reactor of 0.02mol/L silver nitrate solution, finally connecting the reactor to a wet gas flowmeter, recording the initial value of the wet gas flowmeter, then opening a valve of the hydrogen sulfide gas steel cylinder, controlling the flow rate to be 200 Nm/h-400 Nm/h, observing the condition of the glass reaction tube at any time in a test, observing the bubbling speed, closing the valve to stop the test when black precipitate just appears in the reactor filled with silver nitrate, and recording the end value of the gas flowmeter, wherein the difference between the end value of the wet gas flowmeter and the initial value is measured as the penetration rate of the sulfur capacity of the desulfurizer in this example, and the wet desulfurizer is 46.5.5% of the penetration of the sulfur.
Example 7:
(1) 200kg of iron oxide yellow desulfurization dry powder, 30kg of activated carbon powder and 7kg of sodium carboxymethylcellulose are respectively weighed and added into a kneader to be fully kneaded, and proper water is added according to the dryness and wetness degrees in the kneading process to facilitate molding.
(2) And (2) extruding the mixture obtained in the step (1) into strips through a strip extruding machine to form the strips, wherein the strips are hemp strips in the embodiment, and then drying the strips for 60min at the temperature of about 80 ℃ to obtain the high-precision high-sulfur capacity desulfurizer.
(3) The method comprises the steps of grinding the dried desulfurizer by using a mortar, sieving the ground desulfurizer by using a 80-mesh sieve, weighing 1mL (about 0.8 g) of the desulfurizer as a sample, adding dropwise water to moisten the sample (the added water amount is 7% -10% of the sample amount), uniformly filling the sample into a glass reaction tube with the filling height of 3cm to 4cm, connecting one end of the glass reaction tube to a hydrogen sulfide gas steel cylinder for providing hydrogen sulfide standard gas (the hydrogen sulfide content is 4.0 +/-0.2%, and the balance is nitrogen) for the glass reaction tube, connecting the other end of the glass reaction tube to a reactor of 0.02mol/L silver nitrate solution, finally connecting the reactor to a wet gas flowmeter, recording the initial value of the wet gas flowmeter, then opening a valve of the hydrogen sulfide gas steel cylinder, controlling the flow rate to be 200 Nm/h-400 Nm/h, observing the condition of the glass reaction tube at any time in a test, observing the bubbling speed, closing the valve to stop the test when black precipitate just appears in the reactor filled with silver nitrate, and recording the end value of the gas flowmeter, wherein the difference between the end value of the wet gas flowmeter and the initial value is the sulfur capacity penetrating through the desulfurizer is 45%.
Example 8:
(1) 200kg of iron oxide yellow desulfurization dry powder, 15kg of activated carbon powder and 6kg of sesbania gum are respectively weighed and added into a kneader for full kneading, and proper water is added according to the dryness and wetness degree in the kneading process to facilitate molding.
(2) And (2) extruding the mixture obtained in the step (1) into strips through a strip extruding machine to form the strip-shaped mixture in the embodiment, and then drying the strip-shaped mixture for 60min at the temperature of about 80 ℃ to obtain the high-precision high-sulfur capacity desulfurizer.
(3) The method comprises the steps of grinding the dried desulfurizer by using a mortar, screening the ground desulfurizer through an 80-mesh screen, weighing 1mL (about 0.8 g) of the ground desulfurizer as a sample, adding dropwise water to moisten the sample (the water addition amount is 7% -10% of the sample amount), uniformly filling the sample into a glass reaction tube, wherein the filling height is 3cm to 4cm, one end of the glass reaction tube is connected with a hydrogen sulfide gas steel cylinder and used for supplying hydrogen sulfide standard gas (the hydrogen sulfide content is 4.0 +/-0.2%, and the balance is nitrogen) to the glass reaction tube, the other end of the glass reaction tube is connected with a reactor of 0.02mol/L of silver nitrate solution, the reactor is finally connected to a wet gas flowmeter, recording the initial value of the wet gas flowmeter, then opening a valve of the hydrogen sulfide gas steel cylinder, controlling the flow rate to be 200 Nm/h-400 Nm/h, observing the condition of the glass reaction tube at any time in the test, observing the bubbling speed, closing the valve to stop the test when black precipitate appears in the reactor filled with the silver nitrate, recording the end value of the gas flowmeter, and measuring the difference between the end value of the wet gas flowmeter and the initial value of the wet gas flowmeter, namely the sulfur capacity of the desulfurizer, wherein the penetration rate is 44.5.44.5% of the wet desulfurizer in the embodiment.
Example 9:
(1) 200kg of iron oxide yellow desulfurization dry powder, 15kg of activated carbon powder and 6kg of sodium carboxymethylcellulose are respectively weighed and added into a kneader to be fully kneaded, and proper water is added according to the dryness and wetness degree in the kneading process to facilitate molding.
(2) And (2) extruding the mixture obtained in the step (1) into strips through a strip extruding machine to form the strips, wherein the strips are hemp strips in the embodiment, and then drying the strips for 60min at the temperature of about 80 ℃ to obtain the high-precision high-sulfur capacity desulfurizer.
(3) The method comprises the steps of grinding the dried desulfurizer by using a mortar, sieving the ground desulfurizer by using an 80-mesh sieve, weighing 1mL (about 0.8 g) of the desulfurizer as a sample, adding dropwise water to moisten the sample (the added water amount is 7% -10% of the sample amount), uniformly filling the sample into a glass reaction tube with the filling height of 3cm to 4cm, connecting one end of the glass reaction tube to a hydrogen sulfide gas steel cylinder for supplying hydrogen sulfide standard gas (the hydrogen sulfide content is 4.0 +/-0.2%, the carbonyl sulfide content is 500ppm, and the balance is nitrogen), connecting the other end of the glass reaction tube to a reactor of 0.02mol/L silver nitrate solution, finally connecting the reactor to a wet gas flowmeter, recording the initial value of the wet gas flowmeter, then opening a valve of the hydrogen sulfide gas steel cylinder, controlling the flow rate to be 200 Nm/h-400 Nm/h, observing the condition of the glass reaction tube at any time, and detecting the bubbling speed at any time when black precipitate just appears in the reactor filled with the silver nitrate, closing the valve to stop the test, recording the termination value of the wet gas flowmeter, wherein the difference between the termination value of the wet gas flowmeter and the initial value of the wet gas flowmeter is the start value of the sulfur penetration test of the sulfur capacity of the desulfurizer, and the sulfur penetration test is 975% of the sulfur penetration of the sulfur in the wet gas chromatograph, and the sulfur content detection instrument in this embodiment, wherein the sulfur detection is carried out by adopting a quantitative detection instrument, and the sulfur detection is carried out.
Comparison of data
Comparative example 1
(1) The difference from example 1 is that 200kg of iron oxide yellow coarse powder which is not oxidized and pretreated in an alkaline solution is directly weighed and added into a kneader (20 kg of fresh water is added in advance), then the kneader is started to knead for a plurality of minutes and then stopped, 10kg of activated carbon powder and 6kg of sodium carboxymethyl cellulose are respectively weighed and added into the kneader to be fully kneaded, and proper water is added according to the dry and wet degree during the kneading process to facilitate molding.
(2) And (2) extruding the mixture obtained in the step (1) into strips through a strip extruding machine to form the strips, wherein the strips are hemp strips in the embodiment, and then drying the strips for 60min at the temperature of about 80 ℃ to obtain the high-precision high-sulfur capacity desulfurizer.
(3) The method comprises the steps of grinding the dried desulfurizer by using a mortar, screening the ground desulfurizer through an 80-mesh screen, weighing 1mL (about 0.8 g) of the ground desulfurizer as a sample, adding dropwise water to moisten the sample (the water addition amount is 7% -10% of the sample amount), uniformly filling the sample into a glass reaction tube, wherein the filling height is 3cm to 4cm, one end of the glass reaction tube is connected with a hydrogen sulfide gas steel cylinder and used for supplying hydrogen sulfide standard gas (the hydrogen sulfide content is 4.0 +/-0.2%, and the balance is nitrogen) to the glass reaction tube, the other end of the glass reaction tube is connected with a reactor of 0.02mol/L of silver nitrate solution, the reactor is finally connected to a wet gas flowmeter, recording the initial value of the wet gas flowmeter, then opening a valve of the hydrogen sulfide gas steel cylinder, controlling the flow rate to be 200 Nm/h-400 Nm/h, observing the condition of the glass reaction tube at any time in the test, observing the bubbling speed, closing the valve to stop the test when black precipitate appears in the reactor filled with the silver nitrate, recording the end value of the gas flowmeter, and measuring the difference between the end value of the wet gas flowmeter and the initial value of the wet gas flowmeter, namely, wherein the penetration rate of the desulfurizer in the wet gas flowmeter is 27.8.8 penetrating through the wet desulfurizer in the example.
(II) comparative example 2
(1) The difference from the example 8 is that 200kg of iron oxide yellow coarse powder which is not oxidized and pretreated in an alkaline solution is directly weighed and added into a kneader (20 kg of fresh water is added in advance), then the kneader is started to knead for a plurality of minutes and then stopped, 15kg of activated carbon powder and 6kg of sodium carboxymethyl cellulose are respectively weighed and added into the kneader to be fully kneaded, and proper water is added according to the dry and wet degree in the kneading process to facilitate molding.
(2) And (2) extruding the mixture obtained in the step (1) into strips through a strip extruding machine to form the strips, wherein the strips are hemp strips in the embodiment, and then drying the strips for 60min at the temperature of about 80 ℃ to obtain the high-precision high-sulfur capacity desulfurizer.
(3) The method comprises the steps of grinding the dried desulfurizer by using a mortar, screening the ground desulfurizer through an 80-mesh screen, weighing 1mL (about 0.8 g) of the ground desulfurizer as a sample, dripping water to moisten the sample (the water addition amount is 7% -10% of the sample amount), uniformly filling the sample into a glass reaction tube, wherein the filling height is 3cm to 4cm, one end of the glass reaction tube is connected with a hydrogen sulfide gas steel cylinder and used for supplying hydrogen sulfide standard gas (the hydrogen sulfide content is 4.0 +/-0.2%, and the balance is nitrogen) to the glass reaction tube, the other end of the glass reaction tube is connected with a reactor of 0.02mol/L of silver nitrate solution, the reactor is finally connected to a wet gas flowmeter, recording the initial value of the wet gas flowmeter, then opening a valve of the hydrogen sulfide gas steel cylinder, controlling the flow rate to be 200 Nm/h-400 Nm/h, observing the condition of the glass reaction tube at any time in the test, observing the bubbling speed, closing the valve to stop the test when black precipitate appears in the reactor filled with the silver nitrate, recording the end value of the gas flowmeter, and measuring the difference between the end value of the wet gas flowmeter and the initial value of the wet gas flowmeter, namely, wherein the penetration rate of the desulfurizer in the wet gas flowmeter is 28% of the wet desulfurizer.
(III) comparative example 3
According to the same conditions, a spherical desulfurizer product is purchased outside, the desulfurizer is dried for 60min at the temperature of about 80 ℃, then the dried desulfurizer is ground by a mortar and passes through an 80-mesh screen, 1mL (about 0.8 g) is weighed as a sample from the sample, water is added dropwise to moisten the sample (the added water amount is 7% -10% of the sample amount), then the sample is uniformly filled into a glass reaction tube, the filling height is 3cm to 4cm, one end of the glass reaction tube is connected with a hydrogen sulfide steel cylinder for providing hydrogen sulfide standard gas (the content of hydrogen sulfide is 4.0 +/-0.2%, and the balance is nitrogen) to the glass reaction tube, the other end of the glass reaction tube is connected with a reactor of 0.02mol/L silver nitrate solution, the reactor is finally connected to a wet gas flowmeter, the initial value of the wet gas flowmeter is recorded, then a valve of the hydrogen sulfide steel cylinder is opened, the flow rate of the hydrogen sulfide steel cylinder is controlled to be 200 Nm/h-400 Nm/h, the condition of the glass reaction tube is observed at any time in the test, the bubbling speed is the bubbling speed, when black precipitation just occurs in the reactor containing silver nitrate, the valve is closed, the ending value of the wet gas flowmeter, and the difference value of the wet desulfurizer is measured, and the difference value of the penetration difference between the wet gas flowmeter in the wet desulfurizer penetration rate measured in the wet gas flowmeter in the test is 35% of the wet gas flowmeter.
(IV) comparative example 4
According to the same conditions, a strip-shaped desulfurizer product is purchased outside, the desulfurizer is dried for 60min at the temperature of about 80 ℃, then the dried desulfurizer is ground by a mortar and passes through an 80-mesh screen, 1mL (about 0.8 g) is weighed as a sample from the sample, water is added dropwise to moisten the sample (the added water amount is 7% -10% of the sample amount), then the sample is uniformly filled into a glass reaction tube, the filling height is 3cm to 4cm, one end of the glass reaction tube is connected with a hydrogen sulfide steel cylinder for providing hydrogen sulfide standard gas (the content of hydrogen sulfide is 4.0 +/-0.2%, and the balance is nitrogen) to the glass reaction tube, the other end of the glass reaction tube is connected with a reactor of 0.02mol/L silver nitrate solution, the reactor is finally connected to a wet gas flowmeter, the initial value of the wet gas flowmeter is recorded, then a valve of the hydrogen sulfide steel cylinder is opened, the flow rate of the hydrogen sulfide steel cylinder is controlled to be 200 Nm/h to 400 Nm/h, the condition of the glass reaction tube is observed at any time in the test, the bubbling speed is the bubbling speed, when black precipitation just occurs in the reactor containing silver nitrate, the valve is closed, the ending value of the wet desulfurizer ending value, and the difference value of the wet gas flowmeter penetrating through the wet desulfurizer is measured, and the difference value measured in the wet gas flowmeter in the test is 20 percent.
(V) comparative example 5
(1) The difference from the embodiment 3 is that the addition of the activated carbon powder is cancelled, and the other formulas, working procedures and drying temperature are the same;
(2) The method comprises the steps of grinding the dried desulfurizer by using a mortar, screening the ground desulfurizer by using an 80-mesh screen, weighing 1mL (about 0.8 g) of the ground desulfurizer as a sample, dripping water to moisten the sample (the water addition amount is 7% -10% of the sample amount), uniformly filling the sample into a glass reaction tube, wherein the filling height is 3cm to 4cm, one end of the glass reaction tube is connected with a hydrogen sulfide gas steel cylinder and used for supplying hydrogen sulfide standard gas (the hydrogen sulfide content is 4.0 +/-0.2%, and the balance is nitrogen) to the glass reaction tube, the other end of the glass reaction tube is connected with a reactor of 0.02mol/L of silver nitrate solution, the reactor is finally connected to a wet gas flowmeter, recording the initial value of the wet gas flowmeter, then opening a valve of the hydrogen sulfide gas steel cylinder, controlling the flow rate to be 200 Nm/h-400 Nm/h, observing the condition of the glass reaction tube at any time in the test, observing the bubbling speed, closing the valve to stop the test when black precipitate appears in the reactor filled with the silver nitrate, recording the end value of the gas flowmeter, and measuring the difference between the end value of the wet gas flowmeter and the initial value of the wet gas flowmeter, namely, wherein the penetration rate of the sulfur capacity of the desulfurizer in the example is just 46.4.4% of the wet desulfurizer.
The above-mentioned embodiments are merely illustrative of the concept and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the content of the present invention and to implement the invention, and not to limit the scope of the present invention, and all equivalent changes or modifications made according to the spirit of the present invention should be covered by the scope of the present invention.
Claims (7)
1. A preparation method of a desulfurizer with high precision and high sulfur capacity at normal temperature is characterized by comprising the following steps:
a. carrying out oxidation pretreatment on the iron oxide yellow coarse powder and a dispersing agent in an alkaline solution, and washing, filter-pressing and drying the pretreated iron oxide yellow to obtain a desulfurization dry base;
b. fully mixing the activated carbon powder and the binder to obtain a mixture;
c. b, putting the desulfurization dry basis obtained in the step a into a mixture for kneading;
d. fully kneading the mixture evenly and easily forming the mixture to prepare a forming object with the required specification;
e. and drying and screening the formed product to obtain a desulfurizer product.
2. The method for preparing a desulfurizing agent with high precision and high sulfur capacity at normal temperature according to claim 1, wherein in step a, the alkaline solution is a solution prepared from one or more of sodium hydroxide, sodium carbonate and ammonium bicarbonate, and the dispersing agent is one or more of sodium sulfonate and disodium hydrogen phosphate.
3. The method for preparing the desulfurizer with high precision and high sulfur capacity at normal temperature according to claim 1, wherein in the step b, the activated carbon powder: the specific surface area is more than or equal to 800 square meters per gram.
4. The method for preparing the desulfurizing agent with high precision and high sulfur capacity at normal temperature according to claim 1, wherein in the step b, the binder is one or more of sesbania gum and cellulose powder.
5. The method for preparing desulfurizer with high precision and high sulfur capacity at normal temperature as claimed in claim 1, wherein the weight ratio of the activated carbon powder, the binder and the iron oxide yellow coarse powder in steps a and b is (10-30): (2-10): 180-240).
6. The method for preparing the desulfurizing agent with high precision and high sulfur capacity at normal temperature according to claim 1, wherein in the step d, the specification is one or more of a cylinder shape, a hemp strip shape and an irregular shape.
7. The method for preparing the desulfurizer with high precision and high sulfur capacity at normal temperature according to claim 1, wherein in the step e, the drying temperature is 60 ℃ to 90 ℃ and the drying time is 40 minutes to 120 minutes.
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