CN118179227B - Zinc oxide composite desulfurizing agent and preparation method thereof - Google Patents
Zinc oxide composite desulfurizing agent and preparation method thereof Download PDFInfo
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Abstract
The invention provides a zinc oxide composite desulfurizing agent and a preparation method thereof. The zinc oxide composite desulfurizing agent is prepared from modified zinc oxide, ferric hydroxide, aluminosilicate, an adhesive and a filler. Sodium bicarbonate and sodium alginate are loaded into pores of zinc oxide, so that the sulfur capacity and desulfurization precision of the zinc oxide are enhanced, aluminosilicate has a mesoporous structure and becomes a carrier of the zinc oxide, the service time of the desulfurizing agent is prolonged, the iron oxyhydroxide is low in cost and good in desulfurization removal effect, the zinc oxide composite desulfurizing agent is prepared by dry mixing and grinding, the components are uniformly mixed according to a certain proportion, then a proper amount of water is added for full mixing and grinding to enable the components to have certain plasticity, then the components are shaped by a certain pressure, and finally the components are enabled to be finished after being roasted by a certain time of material awakening. The finished product prepared has long service life, good sulfur capacity and thermal stability.
Description
Technical Field
The invention relates to the field of desulfurizing agents, in particular to a zinc oxide composite desulfurizing agent and a preparation method thereof.
Background
The main use of desulfurizing agents is in industrial processes as agents for removing free sulfur or sulfur compounds from fuels, raw materials or other materials. In the field of environmental protection, it is mainly used for removing sulfur oxides, such as sulfur dioxide (SO 2) and sulfur trioxide (SO 3), from exhaust gases. Common desulfurizing agents include alkaline compounds such as lime, limestone, sodium carbonate, alkaline aluminum sulfate, and certain special complex desulfurizing agents such as calcium-manganese alloys. The desulfurizing agent not only helps to reduce scaling and corrosion of equipment, but also helps to improve reliability and stability of the desulfurization system. In addition, the desulfurizing agent can also improve the concentration of calcium ions in the liquid solution and accelerate the crystallization speed of sulfate ions, thereby improving the desulfurizing efficiency. The zinc oxide desulfurizing agent uses zinc oxide as main component, it is a solid desulfurizing agent for conversion absorption, and because zinc oxide can react with HS to produce ZnS which is difficult to be dissociated, the total sulfur of purified gas can be reduced to below 0.3ppm, and the weight sulfur capacity can be up to above 25%. H 2 S molecules in the zinc oxide desulfurization feed gas diffuse from the main body of the gas flow to the outer surface of the desulfurizing agent, H 2 S diffuses into pores of particles of the desulfurizing agent, znS is generated by reacting with ZnO on the surface HS of the desulfurizing agent, generated water vapor diffuses outwards in the pores of the particles of the desulfurizing agent, water molecules diffuse from the outer surface of the particles to the main body of the gas flow, ions must diffuse into crystal lattices, and oxygen ions diffuse to the surface of the solid. The change of crystal structure caused by the conversion of the hexagonal zinc oxide structure into the equiaxed zinc sulfide replaces the original oxide ion position with larger sulfide ions, so that the porosity is obviously reduced. The equilibrium is favorable for the generation of zinc sulfide under normal conditions, but the total reaction rate is controlled by pore diffusion before a ZnS coating film is formed on the surface, and is controlled by lattice diffusion after a ZnS film is formed, so that the conversion of all zinc oxide into zinc sulfide is impossible within a certain period of time. The total reaction rate can be improved by increasing the temperature and making the desulfurizing agent have proper specific surface, pore structure, grain size and particle size, the reaction between zinc oxide and hydrogen sulfide is facilitated by the larger specific surface and proper pore structure, the bed resistance can be reduced by increasing the strength, but the pore diameter and pore volume can be reduced by compacting the particles. The sulfur capacity is reduced by reducing the temperature, increasing the airspeed and increasing the water vapor content, and the form and concentration of sulfide in the process gas have a certain influence on the sulfur capacity. The zinc oxide desulfurizing agent has long development prospect in the desulfurizing technology, and in practical application, the desulfurizing agent can select proper products according to different working conditions so as to adapt to the desulfurizing requirements in different environments.
At present, the patent with the publication number of CN 105692685A discloses a zinc oxide desulfurizer and a preparation method thereof, and the mixed solution of ammonium bicarbonate and ammonium carbonate is adopted as a precipitator, so that the desulfurization performance of the desulfurizer is improved, but the sulfur capacity and the thermal stability of the zinc oxide desulfurizer are not improved; the patent with publication number of CN1895743A discloses a nanometer desulfurizing agent for gas desulfurization, a preparation method and application, wherein zinc nitrate and ferric nitrate are adopted as zinc sources and iron sources, citric acid or amino acetic acid or urea is adopted as a gelling agent, the obtained gel is heated to a certain temperature for spontaneous combustion, then the powder desulfurizing agent is obtained through high-temperature roasting, and finally the desulfurizing agent is obtained through high-temperature forming roasting.
Aiming at the problems existing in the prior art, how to provide a zinc oxide composite desulfurizer to solve the problems of short service life, low sulfur capacity, poor thermal stability and complex and time-consuming preparation process of the zinc oxide desulfurizer is a problem to be solved urgently.
Disclosure of Invention
The invention aims to: the invention aims to provide a zinc oxide composite desulfurizer and a preparation method thereof, which are used for solving the problems of low sulfur capacity, poor thermal stability, insufficient activity of the desulfurizer, short service life and the like of the zinc oxide composite desulfurizer.
The technical scheme of the invention is as follows:
A zinc oxide composite desulfurizing agent, the components of the zinc oxide composite desulfurizing agent comprising: modified zinc oxide, ferric hydroxide, aluminosilicate, binder and filler.
Further, the zinc oxide composite desulfurizer comprises the following components in parts by weight: 20-30 parts of modified zinc oxide, 40-62 parts of ferric hydroxide, 20-40 parts of aluminosilicate, 10-18 parts of adhesive and 10-20 parts of filler.
Further, the modified zinc oxide is prepared by modifying zinc oxide, sodium alginate and sodium carbonate solution.
Further, the mass of the sodium alginate is 5-20% of that of zinc oxide; the concentration of the sodium carbonate solution is 8-20%.
The preparation of the modified zinc oxide comprises the following steps:
(1) Adding a certain amount of sodium carbonate solution into a reaction kettle, heating to 50-60 ℃, slowly adding zinc oxide, fully reacting, filtering, washing and drying to obtain a zinc oxide precursor;
(2) Adding a proper amount of deionized water into the zinc oxide precursor prepared in the step (1), adding sodium alginate, uniformly stirring, and standing for 18-24 hours to prepare a mixture;
(3) And (3) putting the mixture prepared in the step (2) into a high-temperature box with the temperature of 100-120 ℃ to bake for 18-24 hours, so as to prepare the modified zinc oxide.
The preparation method of the aluminosilicate comprises the following steps:
(1) Adding sodium metaaluminate and sodium hydroxide into water, stirring until the sodium metaaluminate and the sodium hydroxide are dissolved, adding the sodium metaaluminate and the sodium hydroxide into a sodium silicate solution, stirring until the sodium metaaluminate and the sodium hydroxide are clear, and standing for a period of time to obtain a mixed liquid A;
(2) Dissolving alkyl trimethyl ammonium bromide in water, heating and stirring, then adding ammonia water, then adding the mixed liquid A prepared in the step (1), and uniformly stirring to prepare mixed liquid B;
(3) And (3) regulating the pH value of the mixed liquid B prepared in the step (2) to 9-10, uniformly stirring, then filling the mixed liquid B into a reaction kettle, reacting for 12-72 h at 100-110 ℃, and roasting the product after suction filtration and drying to obtain the aluminosilicate.
Further, the alkyl trimethyl ammonium bromide is one or more of octadecyl trimethyl ammonium bromide, hexadecyl trimethyl ammonium bromide and dodecyl trimethyl ammonium bromide.
Further, the industrial sulfur capacity of the iron oxyhydroxide is 5-30%.
Further, the binder is one or more of carboxymethyl cellulose, kaolin, clay, starch, and gum.
Further, the filler is one or more of copper oxide, copper nitrate, cobalt nitrate and nickel oxide.
The application also provides a preparation method of the zinc oxide composite desulfurizing agent, which is characterized by comprising the following steps:
step one: weighing modified zinc oxide, an adhesive and a filler, uniformly mixing, and adding water for fully mixing and grinding;
Step two: adding ferric hydroxide and aluminosilicate into the material prepared in the first step, mixing, extrusion molding, and curing the material after extrusion molding;
Step three: and uniformly arranging the cured materials in a material burning frame, and transferring the material burning frame to a roller kiln for roasting through a transmission device to prepare the zinc oxide composite desulfurizing agent.
Further, a high-speed wheel mill is adopted for mixing and grinding, and the discharge flow is 0.5-1 t/h; the extrusion molding adopts a four-column hydraulic press; the curing is carried out by standing for 18-30 h at the temperature of 70-80 ℃, the roasting temperature in the roller kiln is 1200-1400 ℃, and the roasting time is 12-24 h.
Further, the roller kiln is divided into a transportation area, a distributing area and a packaging area; the conveying area transfers the firing basket into the roller kiln for roasting through a transmission device, a supporting bottom is additionally arranged below the transmission device, the firing basket can contain 8-12 kg of desulfurizing agent, a distributing machine is additionally arranged in the distributing area, and an automatic discharging device is additionally arranged in the packaging area.
In the preparation process of the zinc oxide composite desulfurizer, 4 high-speed wheel mills are adopted for mixing and grinding, 2 tons of materials can be fully mixed within half an hour, the materials are conveyed to three four-column hydraulic presses through a transmission device after being uniformly mixed, the materials are extruded and molded according to the diameter size required by customers, the molded materials are unevenly distributed due to moisture, if the molded materials directly enter a roasting kiln for roasting, the quality of finished products can be influenced, the zinc oxide content is low, the quality difference and the desulfurization activity are low, so that the materials can be subjected to health maintenance after extrusion molding, the health maintenance materials are required to be placed in a plastic basket in a stacking manner and are transported by a forklift, the materials are placed in a health maintenance area for natural health maintenance after being transported to the health maintenance area, the materials placed in the plastic basket are uniformly arranged in a material burning frame by workers, the material burning basket is transported to a roller kiln for roasting through the transmission device, the roasted materials are conveyed to a material discharging hole, the finished product of the desulfurizer is poured into a ton bag by the workers, and the material burning disc can contain about 10Kg of desulfurization agent once, and the yield per ton is 4-5 tons.
Firstly, a distributing machine is additionally arranged in a distributing area of the roller kiln, so that manual distributing is not needed any more, and only workers are needed to pour the materials on the distributing machine; secondly, an automatic discharging device is additionally arranged in a packaging area, a worker is not required to take down a firing basket to pour a desulfurizing agent finished product into a ton package, the finished product directly enters the ton package through the automatic discharging device, the worker only needs to control the weight of the ton package, the ton package is sealed, and then the ton package is lifted to the finished product area through a carrier; thirdly, aiming at the loss of the desulfurizing agent in the transmission process, the bottom support is additionally arranged below the main transmission device, so that the abrasion powder is convenient to collect, the whole preparation process is simple, the loss of raw materials is less, and the method has good production prospect.
Advantageous effects
The invention provides a zinc oxide composite desulfurizer, sodium carbonate and sodium alginate are loaded into pores of zinc oxide, sulfur capacity and desulfurization precision of zinc oxide are enhanced, aluminosilicate has a mesoporous structure and becomes a carrier of zinc oxide, hydroxyl ferric oxide is low in cost and good in desulfurization and removal effects, the zinc oxide composite desulfurizer is prepared by dry mixing and grinding, the components are uniformly mixed according to a certain proportion, then a proper amount of water is added for full mixing and grinding to enable the components to have certain plasticity, then the components are shaped by a certain pressure, and finally the components are made into a final finished product after being roasted by a certain time of material awakening. The prepared finished product has good sulfur capacity, desulfurization precision, thermal stability and long service life, the preparation process of the zinc oxide composite desulfurizer is simple, the labor consumption is low, the loss of raw materials can be reduced, and the zinc oxide composite desulfurizer has good development prospect.
Detailed Description
The invention will be described below in connection with specific embodiments. The following examples are illustrative of the present invention and are not intended to limit the present invention. Other combinations and various modifications within the spirit of the invention may be made without departing from the spirit or scope of the invention.
Zinc oxide was purchased from Shijia, a company of the hundred-peptide chemical industry, inc.; sodium alginate was purchased from tuozhou wuyi chemical technology limited; iron oxyhydroxide was purchased from hendakang water purification materials limited; sodium silicate solution was purchased from water glass plant in bergamot; octadecyl trimethyl ammonium bromide was purchased from rana white pharmaceutical chemicals; aluminosilicate 13X was purchased from the duckweed excellent filler market, inc, model 13X; the chemical reagents used in the invention are all common commercial analytical pure unless specified.
Preparation of modified zinc oxide A:
(1) Adding 500ml of sodium carbonate solution with the mass concentration of 10% into a reaction kettle, heating to 60 ℃, slowly adding 5g of zinc oxide, fully reacting, filtering, washing, and drying at 80 ℃ to obtain a zinc oxide precursor;
(2) Adding 500ml of deionized water into the zinc oxide precursor prepared in the step (1), adding 0.5g of sodium alginate, uniformly stirring, and standing for 18 hours to prepare a mixture;
(3) And (3) putting the mixture prepared in the step (2) into a high-temperature box at 120 ℃ to bake for 24 hours, and thus obtaining the modified zinc oxide A.
Preparation of modified zinc oxide B:
(1) Adding 500ml of sodium carbonate solution with mass concentration of 5% into a reaction kettle, heating to 60 ℃, slowly adding 5g of zinc oxide, fully reacting, filtering, washing, and drying at 80 ℃ to obtain a zinc oxide precursor;
(2) Adding 500ml of deionized water into the zinc oxide precursor prepared in the step (1), adding 0.5g of sodium alginate, uniformly stirring, and standing for 18 hours to prepare a mixture;
(3) And (3) putting the mixture prepared in the step (2) into a high-temperature box at 120 ℃ to bake for 24 hours, and preparing the modified zinc oxide B.
Preparation of modified zinc oxide C:
(1) Adding 500ml of sodium carbonate solution with the mass concentration of 10% into a reaction kettle, heating to 60 ℃, slowly adding 5g of zinc oxide, fully reacting, filtering, washing, and drying at 80 ℃ to obtain a zinc oxide precursor;
(2) Adding 500ml of deionized water into the zinc oxide precursor prepared in the step (1), adding 0.05g of sodium alginate, uniformly stirring, and standing for 18 hours to prepare a mixture;
(3) And (3) putting the mixture prepared in the step (2) into a high-temperature box at 120 ℃ to bake for 24 hours, and thus obtaining the modified zinc oxide C.
Preparation of aluminosilicate A:
(1) Adding 5g of sodium metaaluminate and 20g of sodium hydroxide into 500ml of water, stirring until the sodium metaaluminate and the sodium hydroxide are dissolved, adding the mixture into 1kg of sodium silicate solution, stirring until the sodium metaaluminate and the sodium hydroxide are clear, and standing for a period of time to prepare mixed liquid A;
(2) Dissolving 20g of octadecyl trimethyl ammonium bromide in 200ml of water, heating and stirring, then adding 10ml of ammonia water with 25% mass concentration, then adding the mixed liquid A prepared in the step (1), and uniformly stirring to prepare a mixed liquid B;
(3) And (3) regulating the pH value of the mixed liquid B prepared in the step (2) to 9, uniformly stirring, then filling the mixed liquid B into a reaction kettle, reacting for 48 hours at 100 ℃, and carrying out suction filtration and drying on the product, and roasting for 12 hours at 200 ℃ to obtain the aluminosilicate.
The preparation method of the zinc oxide composite desulfurizing agent comprises the following steps:
Step one: weighing modified zinc oxide, an adhesive and a filler, uniformly mixing, adding water, mixing and grinding, wherein the mixing and grinding flow is 1t/h, and mixing and grinding for 2h;
step two: adding ferric hydroxide and aluminosilicate into the material prepared in the first step, mixing for 2 hours, extruding into phi 0.8x2 cylinder, shaping, curing the material, and standing for 24 hours at 80 ℃;
Step three: and uniformly arranging the cured materials in a material burning frame, transferring the material burning frame into a roller kiln through a transmission device, and roasting at 1400 ℃ for 12 hours to obtain the nano zinc oxide desulfurizer.
According to the preparation method of the zinc oxide composite desulfurizer, table 1 is a batching table of zinc oxide composite desulfurizer of examples 1-6.
TABLE 1
According to the preparation method of the zinc oxide composite desulfurizer, table 2 is a batching table of the zinc oxide composite desulfurizer of comparative examples 1-6.
TABLE 2
Performance test: in order to prove the technical effects of the nano zinc oxide desulfurizer in the invention, the following experiments are designed to determine the performances of the nano zinc oxide desulfurizer in the above examples 1-6 and comparative examples 1-6.
Grinding the prepared nano zinc oxide composite desulfurizer into particles with 40-60 meshes, and carrying out hydrogen sulfide penetration experiment test under the following conditions: the inner diameter of the sample tube is 6mm, the filling height of the sample is 2cm, the gas flow is 100ml/min, the experimental temperature is 30 ℃, and the experimental pressure is normal. The experiment is stopped when the concentration of hydrogen sulfide at the air inlet is 800mg/m 3 and the concentration of hydrogen sulfide at the air outlet is 0.15mg/m 3, the content of hydrogen sulfide in the gas is measured by adopting a gas chromatography, the sulfur capacity is calculated by a chemical analysis method, the sulfur capacity is equal to the weight of hydrogen sulfide divided by the weight of the desulfurizing agent multiplied by 100%, and the service life of the desulfurizing agent when the desulfurizing agent reaches saturation is calculated by the sulfur capacity. The specific surface area of the desulfurizing agent is measured by adopting a BET method; crush resistance was measured using a particle strength tester, available from Dalianpenghui technology development Co., ltd., model: KQ-3; thermal stability, thermal stability is tested according to the thermal analysis test method of thermal stability of substances of national Standard GB/T13464-2008, a differential thermal analyzer is adopted for testing, the thermal stability of an electronic film is evaluated by purchasing from Beijing Heng Jiujiu laboratory device Co., model HCR-1 and peak temperature TP of substances, and the larger TP indicates the stronger thermal stability, and the weaker thermal stability is on the contrary.
Table 3: test results table
From the data, in the zinc oxide composite desulfurizer prepared by the application, the zinc oxide composite desulfurizer prepared by high-temperature reaction of modified zinc oxide, ferric hydroxide, aluminosilicate, adhesive and filler has long service life, high sulfur capacity and good thermal stability; specifically, as can be seen from comparison of example 4 and example 2, less sodium carbonate solution is added when nano zinc oxide is prepared, so that the crushing strength of the prepared zinc oxide composite desulfurizing agent is reduced; as can be seen from the comparison of the example 5 and the example 2, when the nano zinc oxide is prepared, less alginic acid is added, so that the crushing strength of the prepared zinc oxide composite desulfurizing agent is reduced, and the thermal stability is poor; from comparative example 1 and example 2, the use of zinc oxide, without using the modified zinc oxide prepared by the application, shows that the specific surface area, sulfur capacity, thermal stability and service life of the prepared zinc oxide composite desulfurizing agent are all good without using the modified zinc oxide; as can be seen from comparison of comparative example 2 with example 2, the desulfurizing agent prepared without adding modified zinc oxide has small specific area, poor crushing strength, low sulfur capacity, poor thermal stability and short service life; as can be seen from comparison of comparative example 3 and example 2, aluminosilicate is not added into the zinc oxide composite desulfurizer, the prepared zinc oxide composite desulfurizer has reduced crushing strength, reduced sulfur capacity and shortened service life; from comparative example 4 and example 2, it is understood that the zinc oxide composite desulfurizing agent prepared using aluminosilicate X13 commercially available has reduced crushing strength, poor thermal stability, and low sulfur capacity; as is clear from comparative example 5 and example 2, the zinc oxide composite desulfurizing agent prepared without adding iron oxyhydroxide has reduced sulfur capacity and shortened service life; from comparative example 6 and example 2, it is known that the zinc oxide composite desulfurizing agent is prepared without adding iron oxyhydroxide and aluminosilicate, and the prepared zinc oxide composite desulfurizing agent has reduced specific surface area, reduced crushing strength, reduced sulfur capacity, poor thermal stability, and shortened service life, and does not meet the expected standard.
The present invention is capable of other and further embodiments and its several details are capable of modification and variation in light of the present invention, as will be apparent to those skilled in the art, without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. The zinc oxide composite desulfurizing agent is characterized by comprising the following components: modified zinc oxide, iron oxyhydroxide, aluminosilicate, binder, and filler;
The preparation of the modified zinc oxide comprises the following steps:
(1) Adding a certain amount of sodium carbonate solution into a reaction kettle, heating to 50-60 ℃, slowly adding zinc oxide, fully reacting, filtering, washing and drying to obtain a zinc oxide precursor;
(2) Adding a proper amount of deionized water into the zinc oxide precursor prepared in the step (1), adding sodium alginate, uniformly stirring, and standing for a period of time to prepare a mixture;
(3) Putting the mixture prepared in the step (2) into a high-temperature box with the temperature of 100-120 ℃ for baking to prepare modified zinc oxide;
the preparation method of the aluminosilicate comprises the following steps:
(1) Adding sodium metaaluminate and sodium hydroxide into water, stirring until the sodium metaaluminate and the sodium hydroxide are dissolved, adding the sodium metaaluminate and the sodium hydroxide into a sodium silicate solution, stirring until the sodium metaaluminate and the sodium hydroxide are clear, and standing for a period of time to obtain a mixed liquid A;
(2) Dissolving alkyl trimethyl ammonium bromide in water, heating and stirring, then adding ammonia water, then adding the mixed liquid A prepared in the step (1), and uniformly stirring to prepare mixed liquid B;
(3) And (3) regulating the pH value of the mixed liquid B prepared in the step (2) to 9-10, uniformly stirring, then filling the mixed liquid B into a reaction kettle, reacting for 12-72 h at 100-110 ℃, and roasting the product after suction filtration and drying to obtain the aluminosilicate.
2. The zinc oxide composite desulfurizing agent according to claim 1, wherein the components of the zinc oxide composite desulfurizing agent comprise, in parts by weight: 20-30 parts of modified zinc oxide, 40-62 parts of ferric hydroxide, 20-40 parts of aluminosilicate, 10-18 parts of adhesive and 10-20 parts of filler.
3. The zinc oxide composite desulfurizing agent according to claim 1, wherein the mass of the sodium alginate is 5-20% of that of zinc oxide; the mass concentration of the sodium carbonate solution is 8-20%.
4. The zinc oxide composite desulfurizing agent according to claim 1, wherein the binder is one or more of carboxymethyl cellulose, kaolin, clay, starch, gum.
5. The zinc oxide composite desulfurizing agent according to claim 1, wherein the filler is one or more of copper oxide, copper nitrate, cobalt nitrate and nickel oxide.
6. The method for preparing the zinc oxide composite desulfurizing agent according to any one of claims 1 to 5, which is characterized by comprising the following steps:
step one: weighing modified zinc oxide, an adhesive and a filler, uniformly mixing, and adding water for fully mixing and grinding;
Step two: adding ferric hydroxide and aluminosilicate into the material prepared in the first step, mixing, extrusion molding, and curing the material after extrusion molding;
Step three: and uniformly arranging the cured materials in a firing basket, and transferring the firing basket to a roller kiln for roasting through a transmission device to prepare the zinc oxide composite desulfurizing agent.
7. The method for preparing the zinc oxide composite desulfurizer according to claim 6, wherein the mixing and grinding are carried out by a high-speed wheel mill, and the discharge flow is 0.5-1 t/h; the extrusion molding adopts a four-column hydraulic press; the curing is carried out by standing for 18-30 h at the temperature of 70-80 ℃, the roasting temperature in the roller kiln is 1200-1400 ℃, and the roasting time is 12-24 h.
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| US20020052291A1 (en) * | 1999-09-30 | 2002-05-02 | Ranjani Siriwardane | Low temperature sorbents for removal of sulfur compounds from fluid feed streams |
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