CN115072756A - Preparation method of irregular active alumina for hydrogen peroxide preparation process - Google Patents
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- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
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- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
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- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
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Abstract
The invention belongs to the technical field of activated alumina preparation, and particularly relates to a preparation method of irregular activated alumina for a hydrogen peroxide preparation process. Reacting alpha-Al (OH) 3 Drying and then crushing to obtain alpha-Al (OH) 3 Micro-powder; mixing high-temperature hot air with alpha-Al (OH) 3 The micro powder is mixed downstream, enters a tubular reactor for rapid dehydration, then is subjected to solid-gas separation, and is collected; mixing the powder with water, adding a forming additive into the mixture, and extruding flaky particles; oxidizing the flaky particles at 40-80 deg.C and humidity of 90-95%>Preparing pseudo-boehmite crystal form activated alumina after 48 hours; the pseudo-boehmite crystal form activated alumina is roasted to prepare the activated alumina used for the hydrogen peroxide preparation process. Prepared by the methodThe alumina has strong activity, can greatly reduce the loss of anthraquinone when being applied to a hydrogen peroxide process, and has strong regeneration capacity on anthraquinone degradation products.
Description
Technical Field
The invention belongs to the technical field of activated alumina preparation, and particularly relates to a preparation method of irregular activated alumina for a hydrogen peroxide preparation process.
Background
At present, the production of hydrogen peroxide at home and abroad mainly adopts an anthraquinone method, and in the cyclic process of anthraquinone hydrogenation and anthraquinone oxidation, part of effective anthraquinones can inevitably undergo deep reaction and are converted into hydrogen-free hydrogen 2 O 2 Productive anthraquinone degradation products. The long-term accumulation of anthraquinone degradation products reduces the total amount of effective anthraquinone in the working solution, changes the physical properties of viscosity, interfacial tension and the like of the working solution, brings difficulty to the operation of the device, and influences the product quality.
In industry, activated alumina is generally used as a regenerant to regenerate anthraquinone degradation products, and part of the degradation products can be regenerated into effective anthraquinone, and are generally placed in a clay bed of a post-treatment process or in a hydrogenation liquid clay bed. The regenerant can adsorb alkali solution and water and decompose residual H in raffinate 2 O 2 And filtering impurities in the working solution to regenerate the tetrahydro-2-ethylanthraquinone epoxy compound, the 2-ethylanthraene and the like. However, the alumina has low regeneration activity, is easy to deactivate, is frequently replaced and has great environmental pollution.
Therefore, how to prepare the active alumina regenerant with high efficiency and long service life to relieve the pressure of hydrogen peroxide production and environmental protection becomes a technical problem to be solved urgently.
Disclosure of Invention
The purpose of the invention is: provides a preparation method of irregular active alumina for a hydrogen peroxide preparation process. The alumina prepared by the method has strong activity, can greatly reduce the loss of anthraquinone when applied to a hydrogen peroxide process, and has strong regeneration capacity on anthraquinone degradation products.
The invention relates to a preparation method of irregular active alumina for a hydrogen peroxide preparation process, which comprises the following steps:
(1) reacting alpha-Al (OH) 3 Drying and then crushing to obtain alpha-Al (OH) 3 Micro-powder;
(2) high-temperature hot air and the alpha-Al (OH) prepared in the step (1) 3 The micro powder is mixed downstream, enters a tubular reactor for rapid dehydration, then is subjected to solid-gas separation, and is collected;
(3) mixing the powder obtained in the step (2) with water, adding a forming additive into the mixture, and extruding flaky particles;
(4) oxidizing the flaky-like particles prepared in the step (3) for more than 48 hours at 40-80 ℃ under the environment with the humidity of 90-95% to prepare pseudo-boehmite crystal form activated alumina;
(5) roasting the pseudo-boehmite crystal form activated alumina prepared in the step (4) to prepare irregular activated alumina for the hydrogen peroxide preparation process.
Wherein:
the drying temperature in the step (1) is 120-.
alpha-Al (OH) obtained by grinding in a Raymond mill in step (1) 3 The particle size of the fine powder is D50=8-12 μm.
The temperature of the high-temperature hot air in the step (2) is 750-850 ℃.
Step (2) high-temperature hot air and alpha-Al (OH) 3 The residence time of the micro powder in the tubular reactor is 0.4-0.9s, and the outlet temperature is controlled at 350-420 ℃.
The crystal form of the powder collected in the step (2) comprises rho-Al 2 O 3 、γ-Al 2 O 3 And a gibbsite phase; wherein, rho-Al 2 O 3 >80%。
The mixing mass ratio of the powder and the water in the step (3) is 60: 35-40.
The forming additive in the step (3) is a mixture of triisopropanolamine and diisopropanolamine, wherein the mass ratio of triisopropanolamine to diisopropanolamine is 1:1-1: 2.
During the extrusion molding in the step (3), rho-Al is adopted 2 O 3 Adding a mixture of triisopropanolamine and diisopropanolamine as a raw material to promote hydration and improve the speed of converting a product into a corresponding crystal form; the irregular active alumina prepared finally has high bulk density, thereby improving the compactness, reducing the bulk pores and avoiding the loss of working solution.
And (4) the mass of the forming additive in the step (3) accounts for 2-5% of the mass sum of the powder and the water.
And (3) extruding and molding under the pressure of 25-35MPa, mounting a cutting blade outside the die head, and directly breaking the extruded material to obtain an irregular product.
The pseudoboehmite crystal form activated alumina prepared in the step (4) has a crystal content of more than 80%, wherein the gibbsite phase is less than 5%.
The roasting temperature in the step (5) is 320-380 ℃, and the roasting time is 2-4 hours.
The specific surface area of the irregular active alumina for the hydrogen peroxide process prepared in the step (5)>300m 2 Strength/g>200N/grain; pore diameter<3.5 nm; pore volume<0.3 mL/g; the product bulk density is 0.95-0.98g/cm 3 (ii) a Regeneration capacity of working fluid>17g/L。
Compared with the prior art, the invention has the following beneficial effects:
(1) the preparation method of the irregular active alumina for the hydrogen peroxide preparation process adopts extrusion molding to directly break to obtain irregular products, does not need an additional crushing process, has a yield of more than 95 percent (and the yield in the crushing process is less than 75 percent), can reduce energy consumption, and reduces the power consumption of 50 to 60 degrees per ton of products compared with the crushing process.
(2) The irregular active alumina prepared by the method is applied to a hydrogen peroxide preparation process, the adsorption quantity of the active alumina is low, and compared with the traditional alumina product, the loss rate of anthraquinone can be reduced by 45-50%.
Drawings
FIG. 1 is an SEM photograph of activated alumina prepared in example 1.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
The preparation method of the irregular active alumina for the hydrogen peroxide preparation process in this embodiment 1 comprises the following steps:
(1) reacting alpha-Al (OH) 3 Drying and then crushing to obtain alpha-Al (OH) 3 Micro powder;
(2) High-temperature hot air and the alpha-Al (OH) prepared in the step (1) 3 The micro powder is mixed downstream, enters a tubular reactor for rapid dehydration, then is subjected to solid-gas separation, and is collected;
(3) mixing the powder obtained in the step (2) with water, adding a forming additive into the mixture, and extruding flaky particles;
(4) oxidizing the flaky-like particles prepared in the step (3) for 55 hours at 65 ℃ under the environment with the humidity of 93% to prepare pseudo-boehmite crystal form activated alumina;
(5) and (5) roasting the pseudo-boehmite crystal form activated alumina prepared in the step (4) to prepare irregular activated alumina for a hydrogen peroxide preparation process.
Wherein:
in the step (1), the drying temperature is 160 ℃, and the drying time is 5 min.
In the step (1), alpha-Al (OH) is obtained by grinding with a Raymond mill 3 The particle size of the fine powder was D50=10 μm.
The temperature of the high-temperature hot air in the step (2) is 800 ℃.
Step (2) high-temperature hot air and alpha-Al (OH) 3 The residence time of the micropowder in the tubular reactor was 0.7s, and the outlet temperature was controlled at 380 ℃.
The crystal form of the powder collected in the step (2) comprises rho-Al 2 O 3 、γ-Al 2 O 3 And a gibbsite phase; wherein, rho-Al 2 O 3 The content was 95%.
The mixing mass ratio of the powder and the water in the step (3) is 60: 40.
The forming additive in the step (3) is a mixture of triisopropanolamine and diisopropanolamine, wherein the mass ratio of triisopropanolamine to diisopropanolamine is 1: 1.5.
And (3) the mass of the forming additive accounts for 3% of the mass sum of the powder and the water.
And (4) in the step (3), the extrusion molding pressure is 30MPa, a cutting blade is arranged outside the die head, and the extruded material is directly broken to obtain an irregular product.
The pseudoboehmite crystal form activated alumina prepared in the step (4) has a crystal content of 92%, wherein the gibbsite phase is 2%.
The roasting temperature in the step (5) is 350 ℃, and the roasting time is 3 hours.
The specific surface area of the irregular active alumina for the hydrogen peroxide process prepared in the step (5) is 313m 2 (iv)/g, strength 225N/pellet; the aperture is 3.0 nm; the pore volume is 0.26 mL/g; the bulk density of the product is 0.98g/cm 3 (ii) a The regeneration capacity of the working solution is 19.1 g/L; the yield was 97%.
The active alumina prepared in the embodiment 1 is used in a hydrogen peroxide process, so that the loss rate of anthraquinone can be reduced by 50%.
SEM tests were carried out on the prepared activated alumina, and the SEM image is shown in FIG. 1, from which a large amount of agglomerated pseudoboehmite phase could be observed.
Example 2
The preparation method of the irregular active alumina for the hydrogen peroxide preparation process described in this embodiment 2 comprises the following steps:
(1) reacting alpha-Al (OH) 3 Drying and then crushing to obtain alpha-Al (OH) 3 Micro-powder;
(2) high-temperature hot air and the alpha-Al (OH) prepared in the step (1) 3 The micro powder is mixed downstream, enters a tubular reactor for rapid dehydration, then is subjected to solid-gas separation, and is collected;
(3) mixing the powder obtained in the step (2) with water, adding a forming additive into the mixture, and extruding flaky particles;
(4) oxidizing the flaky-like particles prepared in the step (3) for 60 hours at 40 ℃ under the environment of 90% humidity to prepare pseudo-boehmite crystal form activated alumina;
(5) roasting the pseudo-boehmite crystal form activated alumina prepared in the step (4) to prepare irregular activated alumina for the hydrogen peroxide preparation process.
Wherein:
in the step (1), the drying temperature is 120 ℃, and the drying time is 10 min.
alpha-Al (OH) obtained by grinding in a Raymond mill in step (1) 3 The particle size of the fine powder was D50=12 μm.
The temperature of the high-temperature hot air in the step (2) is 750 ℃.
Step (2) high-temperature hot air and alpha-Al (OH) 3 The residence time of the micropowder in the tubular reactor was 0.4s, and the outlet temperature was controlled at 350 ℃.
The crystal form of the powder collected in the step (2) comprises rho-Al 2 O 3 、γ-Al 2 O 3 And a gibbsite phase; wherein, rho-Al 2 O 3 The content was 87%.
The mixing mass ratio of the powder and the water in the step (3) is 60: 35.
The forming additive in the step (3) is a mixture of triisopropanolamine and diisopropanolamine, wherein the mass ratio of triisopropanolamine to diisopropanolamine is 1:1.
During the extrusion molding in the step (3), rho-Al is adopted 2 O 3 Adding a mixture of triisopropanolamine and diisopropanolamine as a raw material to promote hydration and improve the speed of converting a product into a corresponding crystal form; the irregular active alumina prepared finally has high bulk density, thereby improving the compactness, reducing the bulk pores and avoiding the loss of working solution.
And (3) the mass of the forming additive accounts for 2% of the mass sum of the powder and the water.
And (4) in the step (3), the extrusion molding pressure is 25MPa, a cutting blade is arranged outside the die head, and the extruded materials are directly broken to obtain irregular products.
The pseudoboehmite crystal form activated alumina prepared in the step (4) has a crystal content of more than 82%, wherein the gibbsite phase is 3%.
The roasting temperature in the step (5) is 320 ℃, and the roasting time is 4 hours.
The specific surface area of the irregular active alumina for the hydrogen peroxide process prepared in the step (5) is 302m 2 (ii)/g, strength 214N/pellet; hole(s)The diameter is 3.3 nm; the pore volume is 0.28 mL/g; the bulk density of the product is 0.95g/cm 3 (ii) a The regeneration capacity of the working solution is 17.7 g/L; the yield was 95%.
The active alumina prepared in the embodiment 2 is used in the hydrogen peroxide process, so that the loss rate of anthraquinone can be reduced by 45%.
Example 3
The preparation method of the irregular active alumina for the hydrogen peroxide preparation process in this embodiment 3 comprises the following steps:
(1) reacting alpha-Al (OH) 3 Drying and then crushing to obtain alpha-Al (OH) 3 Micro-powder;
(2) high-temperature hot air and the alpha-Al (OH) prepared in the step (1) 3 The micro powder is mixed downstream, enters a tubular reactor for rapid dehydration, then is subjected to solid-gas separation, and is collected;
(3) mixing the powder obtained in the step (2) with water, adding a forming additive into the mixture, and extruding flaky particles;
(4) oxidizing the flaky-like particles prepared in the step (3) for 53 hours at 80 ℃ under the environment with the humidity of 95% to prepare pseudo-boehmite crystal form activated alumina;
(5) roasting the pseudo-boehmite crystal form activated alumina prepared in the step (4) to prepare irregular activated alumina for the hydrogen peroxide preparation process.
Wherein:
in the step (1), the drying temperature is 200 ℃, and the drying time is 2 min.
alpha-Al (OH) obtained by grinding in a Raymond mill in step (1) 3 The particle size of the fine powder was D50=12 μm.
The temperature of the high-temperature hot air in the step (2) is 850 ℃.
Step (2) high-temperature hot air and alpha-Al (OH) 3 The residence time of the micropowder in the tubular reactor was 0.9s, and the outlet temperature was controlled at 420 ℃.
The crystal form of the powder collected in the step (2) comprises rho-Al 2 O 3 、γ-Al 2 O 3 And a gibbsite phase; wherein, rho-Al 2 O 3 The content was 93%.
The mixing mass ratio of the powder and the water in the step (3) is 60: 40.
The forming additive in the step (3) is a mixture of triisopropanolamine and diisopropanolamine, wherein the mass ratio of triisopropanolamine to diisopropanolamine is 1: 2.
During the extrusion molding in the step (3), rho-Al is adopted 2 O 3 Adding a mixture of triisopropanolamine and diisopropanolamine as a raw material to promote hydration and improve the speed of converting a product into a corresponding crystal form; the irregular active alumina prepared finally has high bulk density, thereby improving the compactness, reducing the bulk pores and avoiding the loss of working solution.
And (4) the mass of the forming additive in the step (3) accounts for 5% of the mass sum of the powder and the water.
And (4) in the step (3), the extrusion molding pressure is 35MPa, a cutting blade is arranged outside the die head, and the extruded material is directly broken to obtain an irregular product.
The pseudoboehmite crystal form activated alumina prepared in the step (4) has a crystal content of more than 89%, wherein the gibbsite phase is 2%.
The roasting temperature in the step (5) is 380 ℃, and the roasting time is 2 hours.
The specific surface area of the irregular active alumina for the hydrogen peroxide process prepared in the step (5) is 305m 2 (iv)/g, strength 223N/pellet; the aperture is 3.2 nm; the pore volume is 0.27 mL/g; the bulk density of the product is 0.97g/cm 3 (ii) a The regeneration capacity of the working solution is 18.5 g/L; the yield was 95%.
The active alumina prepared in the embodiment 3 is used in the hydrogen peroxide process, so that the loss rate of anthraquinone can be reduced by 48%.
Comparative example 1
The preparation method of the active alumina for the hydrogen peroxide solution process in the comparative example 1 is the same as that in the example 1, and the only difference is that the forming additive added in the step (3) is different, and the forming additive in the step (3) in the comparative example 1 is triisopropanolamine. And (3) the mass of the forming additive accounts for 3% of the mass sum of the powder and the water.
The specific surface area of the irregular active alumina for the hydrogen peroxide process prepared in the comparative example 1 is 273m 2 (ii)/g, intensity of 191N/pellet; the aperture is 3.7 nm; the pore volume is 0.33 mL/g; the bulk density of the product is 0.95g/cm 3 (ii) a The regeneration capacity of the working solution is 14.8 g/L.
The active alumina prepared in the comparative example 1 is used in the hydrogen peroxide process, so that the loss rate of anthraquinone can be reduced by 39%.
Comparative example 2
The preparation method of the activated alumina for the hydrogen peroxide process in the comparative example 2 is the same as that in the example 1, and the only difference is that the forming additive added in the step (3) is different, and the forming additive in the step (3) in the comparative example 2 is diisopropanolamine. And (3) the mass of the forming additive accounts for 3% of the mass sum of the powder and the water.
The specific surface area of the irregular active alumina for the hydrogen peroxide process prepared in the comparative example 2 is 281m 2 (iv)/g, strength 184N/pellet; the aperture is 3.5 nm; the pore volume is 0.32 mL/g; the bulk density of the product is 0.96g/cm 3 (ii) a The regeneration capacity of the working solution is 16.1 g/L.
The active alumina prepared in the comparative example 2 is used in the hydrogen peroxide process, so that the loss rate of anthraquinone can be reduced by 42%.
Comparative example 3
The preparation method of the active alumina for the hydrogen peroxide solution process in the comparative example 3 is the same as that in the example 1, and the only difference is that the amount of the forming additive added in the step (3) is different, and the forming additive in the comparative example 3 is a mixture of triisopropanolamine and diisopropanolamine, wherein the mass ratio of triisopropanolamine to diisopropanolamine is 1: 3.
And (4) the mass of the forming additive in the step (3) accounts for 7% of the mass sum of the powder and the water.
The specific surface area of the irregular active alumina for the hydrogen peroxide process prepared in the comparative example 3 is 269m 2 (ii)/g, strength is 195N/pellet; the aperture is 3.8 nm; the pore volume is 0.37 mL/g; the bulk density of the product is 0.96g/cm 3 (ii) a Working fluidThe generating capacity is 15.3 g/L.
The active alumina prepared in the comparative example 3 is used in the hydrogen peroxide process, so that the loss rate of anthraquinone can be reduced by 40%.
Comparative example 4
The preparation method of the active alumina for the hydrogen peroxide solution process, which is described in the comparative example 4, is the same as that in the example 1, and the only difference is that the amount of the forming additive added in the step (3) is different, and the forming additive in the comparative example 4 is a mixture of triisopropanolamine and diisopropanolamine, wherein the mass ratio of triisopropanolamine to diisopropanolamine is 1: 0.5. And (4) the mass of the forming additive in the step (3) accounts for 1% of the mass sum of the powder and the water.
The specific surface area of the irregular active alumina for the hydrogen peroxide process prepared in the comparative example 4 is 254m 2 (ii)/g, strength 178N/pellet; the aperture is 4.0 nm; the pore volume is 0.35 mL/g; the bulk density of the product is 0.94g/cm 3 (ii) a The regeneration capacity of the working solution was 13.3 g/L.
The active alumina prepared in the comparative example 4 is used in the hydrogen peroxide process, so that the loss rate of anthraquinone can be reduced by 37%.
The following can be clearly seen from examples 1 to 3 and comparative examples 1 to 4 of the present application: when the added forming agent is one of triisopropanolamine or diisopropanolamine, or the mass ratio of triisopropanolamine to diisopropanolamine does not meet the range value of 1:1-1:2, the specific surface area of the prepared activated alumina is reduced, the strength is reduced, the pore diameter and the pore volume are increased, and the regeneration capacity of the working solution is reduced.
Claims (10)
1. A preparation method of irregular active alumina for a hydrogen peroxide preparation process is characterized by comprising the following steps: the method comprises the following steps:
(1) reacting alpha-Al (OH) 3 Drying and then crushing to obtain alpha-Al (OH) 3 Micro-powder;
(2) high-temperature hot air and the alpha-Al (OH) prepared in the step (1) 3 The micro powder is mixed downstream, enters a tubular reactor for rapid dehydration, then is subjected to solid-gas separation, and is collected;
(3) mixing the powder obtained in the step (2) with water, adding a forming additive into the mixture, and extruding flaky particles;
(4) oxidizing the flaky-like particles prepared in the step (3) for more than 48 hours at 40-80 ℃ under the environment with the humidity of 90-95% to prepare pseudo-boehmite crystal form activated alumina;
(5) and (5) roasting the pseudo-boehmite crystal form activated alumina prepared in the step (4) to prepare irregular activated alumina for a hydrogen peroxide preparation process.
2. The method for preparing the irregular activated alumina used for the hydrogen peroxide preparation process according to claim 1, which is characterized by comprising the following steps: the drying temperature in the step (1) is 120-; alpha-Al (OH) obtained by grinding in a Raymond mill in step (1) 3 The particle size of the fine powder is D50=8-12 μm.
3. The method for preparing the irregular activated alumina used for the hydrogen peroxide preparation process according to claim 1, which is characterized by comprising the following steps: the temperature of the high-temperature hot air in the step (2) is 750-850 ℃.
4. The method for preparing the irregular activated alumina used for the hydrogen peroxide preparation process according to claim 1, which is characterized by comprising the following steps: step (2) high-temperature hot air and alpha-Al (OH) 3 The residence time of the micropowder in the tubular reactor is 0.4-0.9s, and the outlet temperature is controlled at 350-420 ℃.
5. The method for preparing the irregular activated alumina used for the hydrogen peroxide preparation process according to claim 1, which is characterized by comprising the following steps: the crystal form of the powder collected in the step (2) comprises rho-Al 2 O 3 、γ-Al 2 O 3 And a gibbsite phase; wherein, rho-Al 2 O 3 >80%。
6. The method for preparing the irregular activated alumina used for the hydrogen peroxide preparation process according to claim 1, which is characterized by comprising the following steps: the mixing mass ratio of the powder and the water in the step (3) is 60: 35-40.
7. The method for preparing the irregular activated alumina used for the hydrogen peroxide preparation process according to claim 1, which is characterized by comprising the following steps: the forming additive in the step (3) is a mixture of triisopropanolamine and diisopropanolamine, wherein the mass ratio of triisopropanolamine to diisopropanolamine is 1:1-1: 2; the mass of the forming additive in the step (3) accounts for 2-5% of the mass sum of the powder and the water.
8. The method for preparing irregular active alumina for hydrogen peroxide preparation process according to claim 1, wherein the method comprises the following steps: and (3) extruding and molding under the pressure of 25-35MPa, mounting a cutting blade outside the die head, and directly breaking the extruded material to obtain an irregular product.
9. The method for preparing the irregular activated alumina used for the hydrogen peroxide preparation process according to claim 1, which is characterized by comprising the following steps: the pseudoboehmite crystal form activated alumina prepared in the step (4) has a crystal content of more than 80%, wherein the gibbsite phase is less than 5%.
10. The method for preparing irregular active alumina for hydrogen peroxide preparation process according to claim 1, wherein the method comprises the following steps: the roasting temperature in the step (5) is 320-380 ℃, and the roasting time is 2-4 hours; the specific surface area of the irregular active alumina for the hydrogen peroxide process prepared in the step (5)>300m 2 Strength/g>200N/grain; pore diameter<3.5 nm; pore volume<0.3 mL/g; the bulk density of the product is 0.95-0.98g/cm 3 (ii) a Regeneration capacity of working fluid>17g/L。
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