[0023] The present invention will be further explained below in conjunction with specific embodiments.
[0024] refer to figure 1 , Example 1
[0025] In the present embodiment, a preparation method of a complex iron desulfurizer is proposed, comprising the following steps:
[0026] S1: Prepare the material of the complex iron desulfurizer. The material of the complex iron desulfurizer includes 31 parts of iron material, 42 parts of ethylenediaminetetraacetic acid, 13 parts of maltobiose, and 8 parts of polyethylene glycol monomethyl. Ether, 79 parts of mixed solution and 8 parts of modified additive, mixed solution includes two kinds of soda ash, ammonia water and caustic soda, modified additive includes cobalt salt and molybdenum salt, iron material includes iron salt, elemental iron ion, trioxide When one or two of iron and other iron-containing compounds, soda ash and caustic soda are mixed with ammonia water, the added deionized water accounts for 40% to 60% of the mixed solution. When soda ash and caustic soda are mixed, the added deionized water Ionized water accounts for 50% to 75% of the mixed solution. The preparation method of the mixed solution is to obtain two kinds of soda ash, ammonia water and caustic soda, then obtain the corresponding amount of deionized water according to the proportion, and add the deionized water to the reaction kettle. The temperature is heated to 30℃~45℃, the stirring speed is controlled at 120r/min~240r/min, then two kinds of soda ash, ammonia water and caustic soda are slowly added, and after stirring for 15 to 30 minutes, a mixed solution is obtained, and the modified additives include 40% to 60% of cobalt salt and 40% to 60% of molybdenum salt, preparation method of modified additive: get cobalt salt and molybdenum salt, pour it into a container equipped with a microwave transmitter, inject inert gas for protection, start The microwave transmitter emits microwaves, the output power of the microwave transmitter is 0-2kW, the microwave radiation power of the microwave transmitter is controlled at 1000W-1800W, and the frequency is controlled at 2.40GHz-2.50GHz. Sexual additives;
[0027] S2: Add the iron material and modified additives into the activation equipment, exhaust air and inject inert gas, and then inject water vapor at 105°C to 115°C from the bottom of the activation equipment to the inside of the equipment, and stir the iron materials and modification additives. After 15 minutes to 30 minutes of stirring reaction, the activated material is obtained. During the stirring process of the iron material and the modified additive, a stirring frame equipped with a helical blade is used, and the iron material and the modified additive are mixed by the stirring frame equipped with the helical blade. take up and drop;
[0028] S3: Add ethylenediaminetetraacetic acid, polyethylene glycol monomethyl ether and mixed solution into the reaction kettle for stirring, heat during stirring, heat the temperature to 95°C to 115°C, and control the stirring speed at 120r/min~240r /min, after 15 minutes to 30 minutes, a dissolving solution was obtained, and the reaction kettle was heated from room temperature to 95 ° C to 115 ° C for 5 minutes to 15 minutes, and then kept at 95 ° C to 115 ° C and continued to stir for 15 minutes to 30 minutes;
[0029] S4: Sprinkle the activated material into the dissolving solution, increase the stirring speed to 320r/min~440r/min, until all the activated materials are dissolved in the dissolving solution, start the ultrasonic generator inside the reactor, and continue the stirring reaction After 15 minutes to 30 minutes, the semi-finished product of complex iron desulfurizer is obtained. The power of the ultrasonic generator is controlled at 1000W to 1800W, and the ultrasonic generator stops working for 30 seconds every 2 minutes;
[0030] S5: Add maltobiose to the semi-finished product of the complex iron desulfurizer, stop heating, and reduce the stirring speed to 120r/min~230r/min, until the temperature inside the reactor is lowered to 45℃~60℃, export the reactor Internally mixed materials to obtain complex iron desulfurizer, which is dehydrated by vacuum dehydration equipment or sealed drying box, and then stored in vacuum seal or injected with inert gas.
[0031] refer to figure 1 , Example 2
[0032] In the present embodiment, a preparation method of a complex iron desulfurizer is proposed, comprising the following steps:
[0033]S1: Prepare the material of the complex iron desulfurizer. The material of the complex iron desulfurizer includes 29 parts of iron material, 45 parts of ethylenediaminetetraacetic acid, 14 parts of maltobiose, and 7 parts of polyethylene glycol monomethyl. Ether, 91 parts of mixed solution and 9 parts of modified additives, the mixed solution includes two kinds of soda ash, ammonia water and caustic soda, the modified additives include cobalt salt and molybdenum salt, and the iron material includes iron salt, elemental iron ion, trioxide When one or two of iron and other iron-containing compounds, soda ash and caustic soda are mixed with ammonia water, the added deionized water accounts for 40% to 60% of the mixed solution. When soda ash and caustic soda are mixed, the added deionized water Ionized water accounts for 50% to 75% of the mixed solution. The preparation method of the mixed solution is to obtain two kinds of soda ash, ammonia water and caustic soda, then obtain the corresponding amount of deionized water according to the proportion, and add the deionized water to the reaction kettle. The temperature is heated to 30℃~45℃, the stirring speed is controlled at 120r/min~240r/min, then two kinds of soda ash, ammonia water and caustic soda are slowly added, and after stirring for 15 to 30 minutes, a mixed solution is obtained, and the modified additives include 40% to 60% of cobalt salt and 40% to 60% of molybdenum salt, preparation method of modified additive: get cobalt salt and molybdenum salt, pour it into a container equipped with a microwave transmitter, inject inert gas for protection, start The microwave transmitter emits microwaves, the output power of the microwave transmitter is 0-2kW, the microwave radiation power of the microwave transmitter is controlled at 1000W-1800W, and the frequency is controlled at 2.40GHz-2.50GHz. Sexual additives;
[0034] S2: Add the iron material and modified additives into the activation equipment, exhaust air and inject inert gas, and then inject water vapor at 105°C to 115°C from the bottom of the activation equipment to the inside of the equipment, and stir the iron materials and modification additives. After 15 minutes to 30 minutes of stirring reaction, the activated material is obtained. During the stirring process of the iron material and the modified additive, a stirring frame equipped with a helical blade is used, and the iron material and the modified additive are mixed by the stirring frame equipped with the helical blade. take up and drop;
[0035] S3: Add ethylenediaminetetraacetic acid, polyethylene glycol monomethyl ether and mixed solution to the reaction kettle for stirring, heat during stirring, heat the temperature to 95°C~115°C, and control the stirring speed at 120r/min~240r /min, after 15 minutes to 30 minutes, a dissolving solution was obtained, and the reaction kettle was heated from room temperature to 95 ° C to 115 ° C for 5 minutes to 15 minutes, and then kept at 95 ° C to 115 ° C and continued to stir for 15 minutes to 30 minutes;
[0036] S4: Sprinkle the activated material into the dissolving solution, increase the stirring speed to 320r/min~440r/min, until all the activated materials are dissolved in the dissolving solution, start the ultrasonic generator inside the reactor, and continue the stirring reaction 15 minutes to 30 minutes, the semi-finished product of complex iron desulfurizer is obtained, the power of the ultrasonic generator is controlled at 1000W to 1800W, and the ultrasonic generator stops working for 30 seconds every 2 minutes;
[0037] S5: Add maltobiose into the semi-finished product of complex iron desulfurizer, stop heating, and reduce the stirring speed to 120r/min~230r/min, until the temperature inside the reactor is reduced to 45℃~60℃, export the reactor Internally mixed materials to obtain complex iron desulfurizer, which is dehydrated by vacuum dehydration equipment or sealed drying box, and then stored in vacuum seal or injected with inert gas.
[0038] refer to figure 1 , Example three
[0039] In the present embodiment, a preparation method of a complex iron desulfurizer is proposed, comprising the following steps:
[0040] S1: Prepare the material of the complex iron desulfurizer. The material of the complex iron desulfurizer includes 34 parts of iron material, 48 parts of ethylenediaminetetraacetic acid, 13 parts of maltobiose, and 7 parts of polyethylene glycol monomethyl. Ether, 83 parts of mixed solution and 7 parts of modified additive, mixed solution includes two kinds of soda ash, ammonia water and caustic soda, modified additive includes cobalt salt and molybdenum salt, iron material includes iron salt, elemental iron ion, trioxide When one or two of iron and other iron-containing compounds, soda ash and caustic soda are mixed with ammonia water, the added deionized water accounts for 40% to 60% of the mixed solution. When soda ash and caustic soda are mixed, the added deionized water Ionized water accounts for 50% to 75% of the mixed solution. The preparation method of the mixed solution is to obtain two kinds of soda ash, ammonia water and caustic soda, then obtain the corresponding amount of deionized water according to the proportion, and add the deionized water to the reaction kettle. The temperature is heated to 30℃~45℃, the stirring speed is controlled at 120r/min~240r/min, then two kinds of soda ash, ammonia water and caustic soda are slowly added, and after stirring for 15 to 30 minutes, a mixed solution is obtained, and the modified additives include 40% to 60% of cobalt salt and 40% to 60% of molybdenum salt, preparation method of modified additive: get cobalt salt and molybdenum salt, pour it into a container equipped with a microwave transmitter, inject inert gas for protection, start The microwave transmitter emits microwaves, the output power of the microwave transmitter is 0-2kW, the microwave radiation power of the microwave transmitter is controlled at 1000W-1800W, and the frequency is controlled at 2.40GHz-2.50GHz. Sexual additives;
[0041] S2: Add the iron material and modified additives into the activation equipment, exhaust air and inject inert gas, and then inject water vapor at 105°C to 115°C from the bottom of the activation equipment to the inside of the equipment, and stir the iron materials and modification additives. After 15 minutes to 30 minutes of stirring reaction, the activated material is obtained. During the stirring process of the iron material and the modified additive, a stirring frame equipped with a helical blade is used, and the iron material and the modified additive are mixed by the stirring frame equipped with the helical blade. take up and drop;
[0042] S3: Add ethylenediaminetetraacetic acid, polyethylene glycol monomethyl ether and mixed solution to the reaction kettle for stirring, heat during stirring, heat the temperature to 95°C~115°C, and control the stirring speed at 120r/min~240r /min, after 15 minutes to 30 minutes, a dissolving solution was obtained, and the reaction kettle was heated from room temperature to 95 ° C to 115 ° C for 5 minutes to 15 minutes, and then kept at 95 ° C to 115 ° C and continued to stir for 15 minutes to 30 minutes;
[0043] S4: Sprinkle the activated material into the dissolving solution, increase the stirring speed to 320r/min~440r/min, until all the activated materials are dissolved in the dissolving solution, start the ultrasonic generator inside the reactor, and continue the stirring reaction 15 minutes to 30 minutes, the semi-finished product of complex iron desulfurizer is obtained, the power of the ultrasonic generator is controlled at 1000W to 1800W, and the ultrasonic generator stops working for 30 seconds every 2 minutes;
[0044] S5: Add maltobiose into the semi-finished product of complex iron desulfurizer, stop heating, and reduce the stirring speed to 120r/min~230r/min, until the temperature inside the reactor is reduced to 45℃~60℃, export the reactor Internally mixed materials to obtain complex iron desulfurizer, which is dehydrated by vacuum dehydration equipment or sealed drying box, and then stored in vacuum seal or injected with inert gas.
[0045] refer to figure 1 , Example four
[0046] In the present embodiment, a preparation method of a complex iron desulfurizer is proposed, comprising the following steps:
[0047] S1: Prepare the material of complex iron desulfurizer, the material of complex iron desulfurizer includes 29 parts of iron material, 47 parts of ethylenediaminetetraacetic acid, 11 parts of maltobiose, and 6 parts of polyethylene glycol monomethyl Ether, 79 parts of mixed solution and 9 parts of modified additive, mixed solution includes two kinds of soda ash, ammonia water and caustic soda, modified additive includes cobalt salt and molybdenum salt, iron material includes iron salt, elemental iron ion, trioxide When one or two of iron and other iron-containing compounds, soda ash and caustic soda are mixed with ammonia water, the added deionized water accounts for 40% to 60% of the mixed solution. When soda ash and caustic soda are mixed, the added deionized water Ionized water accounts for 50% to 75% of the mixed solution. The preparation method of the mixed solution is to obtain two kinds of soda ash, ammonia water and caustic soda, then obtain the corresponding amount of deionized water according to the proportion, and add the deionized water to the reaction kettle. The temperature is heated to 30℃~45℃, the stirring speed is controlled at 120r/min~240r/min, then two kinds of soda ash, ammonia water and caustic soda are slowly added, and after stirring for 15 to 30 minutes, a mixed solution is obtained, and the modified additives include 40% to 60% of cobalt salt and 40% to 60% of molybdenum salt, preparation method of modified additive: get cobalt salt and molybdenum salt, pour it into a container equipped with a microwave transmitter, inject inert gas for protection, start The microwave transmitter emits microwaves, the output power of the microwave transmitter is 0-2kW, the microwave radiation power of the microwave transmitter is controlled at 1000W-1800W, and the frequency is controlled at 2.40GHz-2.50GHz. Sexual additives;
[0048] S2: Add the iron material and modified additives into the activation equipment, exhaust air and inject inert gas, and then inject water vapor at 105°C to 115°C from the bottom of the activation equipment to the inside of the equipment, and stir the iron materials and modification additives. After 15 minutes to 30 minutes of stirring reaction, the activated material is obtained. During the stirring process of the iron material and the modified additive, a stirring frame equipped with a helical blade is used, and the iron material and the modified additive are mixed by the stirring frame equipped with the helical blade. take up and drop;
[0049] S3: Add ethylenediaminetetraacetic acid, polyethylene glycol monomethyl ether and mixed solution into the reaction kettle for stirring, heat during stirring, heat the temperature to 95°C to 115°C, and control the stirring speed at 120r/min~240r /min, after 15 minutes to 30 minutes, a dissolving solution was obtained, and the reaction kettle was heated from room temperature to 95 ° C to 115 ° C for 5 minutes to 15 minutes, and then kept at 95 ° C to 115 ° C and continued to stir for 15 minutes to 30 minutes;
[0050] S4: Sprinkle the activated material into the dissolving solution, increase the stirring speed to 320r/min~440r/min, until all the activated materials are dissolved in the dissolving solution, start the ultrasonic generator inside the reactor, and continue the stirring reaction After 15 minutes to 30 minutes, the semi-finished product of complex iron desulfurizer is obtained. The power of the ultrasonic generator is controlled at 1000W to 1800W, and the ultrasonic generator stops working for 30 seconds every 2 minutes;
[0051] S5: Add maltobiose to the semi-finished product of the complex iron desulfurizer, stop heating, and reduce the stirring speed to 120r/min~230r/min, until the temperature inside the reactor is lowered to 45℃~60℃, export the reactor Internally mixed materials to obtain complex iron desulfurizer, which is dehydrated by vacuum dehydration equipment or sealed drying box, and then stored in vacuum seal or injected with inert gas.
[0052] refer to figure 1 , Example 5
[0053] In the present embodiment, a preparation method of a complex iron desulfurizer is proposed, comprising the following steps:
[0054]S1: Prepare the material of the complex iron desulfurizer. The material of the complex iron desulfurizer includes 27 parts of iron material, 39 parts of ethylenediaminetetraacetic acid, 11 parts of maltobiose, and 7 parts of polyethylene glycol monomethyl. Ether, 78 parts of mixed solution and 6 parts of modified additive, mixed solution includes two kinds of soda ash, ammonia water and caustic soda, modified additive includes cobalt salt and molybdenum salt, iron material includes iron salt, elemental iron ion, trioxide When one or two of iron and other iron-containing compounds, soda ash and caustic soda are mixed with ammonia water, the added deionized water accounts for 40% to 60% of the mixed solution. When soda ash and caustic soda are mixed, the added deionized water Ionized water accounts for 50% to 75% of the mixed solution. The preparation method of the mixed solution is to obtain two kinds of soda ash, ammonia water and caustic soda, and then obtain the corresponding amount of deionized water according to the proportion. The temperature is heated to 30℃~45℃, the stirring speed is controlled at 120r/min~240r/min, then two kinds of soda ash, ammonia water and caustic soda are slowly added, and after stirring for 15 minutes to 30 minutes, a mixed solution is obtained, and the modified additives include 40% to 60% of cobalt salt and 40% to 60% of molybdenum salt, preparation method of modified additive: get cobalt salt and molybdenum salt, pour it into a container equipped with a microwave transmitter, inject inert gas for protection, start The microwave transmitter emits microwaves, the output power of the microwave transmitter is 0-2kW, the microwave radiation power of the microwave transmitter is controlled at 1000W-1800W, and the frequency is controlled at 2.40GHz-2.50GHz. Sexual additives;
[0055] S2: Add the iron material and modified additives into the activation equipment, exhaust air and inject inert gas, and then inject water vapor at 105°C to 115°C from the bottom of the activation equipment to the inside of the equipment, and stir the iron materials and modification additives. After 15 minutes to 30 minutes of stirring reaction, the activated material is obtained. During the stirring process of the iron material and the modified additive, a stirring frame equipped with a helical blade is used, and the iron material and the modified additive are mixed by the stirring frame equipped with the helical blade. take up and drop;
[0056] S3: Add ethylenediaminetetraacetic acid, polyethylene glycol monomethyl ether and mixed solution into the reaction kettle for stirring, heat during stirring, heat the temperature to 95°C to 115°C, and control the stirring speed at 120r/min~240r /min, after 15 minutes to 30 minutes, a dissolving solution was obtained, and the reaction kettle was heated from room temperature to 95 ° C to 115 ° C for 5 minutes to 15 minutes, and then kept at 95 ° C to 115 ° C and continued to stir for 15 minutes to 30 minutes;
[0057] S4: Sprinkle the activated material into the dissolving solution, increase the stirring speed to 320r/min~440r/min, until all the activated materials are dissolved in the dissolving solution, start the ultrasonic generator inside the reactor, and continue the stirring reaction After 15 minutes to 30 minutes, the semi-finished product of complex iron desulfurizer is obtained. The power of the ultrasonic generator is controlled at 1000W to 1800W, and the ultrasonic generator stops working for 30 seconds every 2 minutes;
[0058] S5: Add maltobiose to the semi-finished product of the complex iron desulfurizer, stop heating, and reduce the stirring speed to 120r/min~230r/min, until the temperature inside the reactor is lowered to 45℃~60℃, export the reactor Internally mixed materials to obtain complex iron desulfurizer, which is dehydrated by vacuum dehydration equipment or sealed drying box, and then stored in vacuum seal or injected with inert gas.
[0059] Contrast conventional complex iron desulfurizers and the complex iron desulfurizers prepared in Examples 1 to 5, the complex iron desulfurizers prepared in Examples 1 to 5 are as follows:
[0060]
[0061] It can be seen from the above table that the desulfurization liquid sulfur capacity and desulfurization rate of the complex iron desulfurizer prepared by the present invention are significantly improved, and no secondary salts are produced, and implementation 2 is the best embodiment.
[0062] The above description is only a preferred embodiment of the present invention, but the protection scope of the present invention is not limited to this. The equivalent replacement or change of the inventive concept thereof shall be included within the protection scope of the present invention.
