CN118002135B - Preparation method of aluminum-nickel alloy catalyst for preparing 1, 4-butanediol by catalytic hydrogenation - Google Patents
Preparation method of aluminum-nickel alloy catalyst for preparing 1, 4-butanediol by catalytic hydrogenation Download PDFInfo
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- CN118002135B CN118002135B CN202410412327.3A CN202410412327A CN118002135B CN 118002135 B CN118002135 B CN 118002135B CN 202410412327 A CN202410412327 A CN 202410412327A CN 118002135 B CN118002135 B CN 118002135B
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- 239000003054 catalyst Substances 0.000 title claims abstract description 64
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 title claims abstract description 44
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical class [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000009903 catalytic hydrogenation reaction Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 70
- 239000000956 alloy Substances 0.000 claims abstract description 70
- 239000002245 particle Substances 0.000 claims abstract description 32
- 238000001816 cooling Methods 0.000 claims abstract description 22
- 238000005406 washing Methods 0.000 claims abstract description 22
- 238000001354 calcination Methods 0.000 claims abstract description 19
- 238000003723 Smelting Methods 0.000 claims abstract description 17
- 238000012216 screening Methods 0.000 claims abstract description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 34
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 19
- 229910021641 deionized water Inorganic materials 0.000 claims description 19
- 239000007788 liquid Substances 0.000 claims description 13
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- 238000005470 impregnation Methods 0.000 claims description 10
- 238000007598 dipping method Methods 0.000 claims description 9
- 239000002699 waste material Substances 0.000 claims description 9
- 239000002351 wastewater Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 238000005507 spraying Methods 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 239000006227 byproduct Substances 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 27
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 37
- 229910000943 NiAl Inorganic materials 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 238000010586 diagram Methods 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 6
- 238000009826 distribution Methods 0.000 description 6
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 229910000838 Al alloy Inorganic materials 0.000 description 3
- 229910021645 metal ion Inorganic materials 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 230000000087 stabilizing effect Effects 0.000 description 3
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 229910000905 alloy phase Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
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Abstract
The invention is applicable to the technical field of catalyst preparation, and provides a preparation method of an aluminum-nickel alloy catalyst for preparing 1, 4-butanediol by catalytic hydrogenation, which comprises the following steps: (1) smelting; (2) cooling; (3) crushing and screening; (4) calcining; (5) immersing and washing. The beneficial effects are that: the invention improves the strength of the catalyst, so that the activity of the catalyst is durable and has good activity; the alloy particles have better strength and larger specific surface, so that the activity durability of the subsequent catalyst is improved, and the catalyst has good catalytic effect; realizes zero emission and protects the environment.
Description
Technical Field
The invention relates to the technical field of catalyst preparation, in particular to a preparation method of an aluminum-nickel alloy catalyst for preparing 1, 4-butanediol by catalytic hydrogenation.
Background
At present, two general methods for producing 1, 4-butanediol exist, one method is that 1, 4-diacetylene aldehyde is subjected to hydrogenation reaction in a fixed bed under the condition of the pressure of 30MPa and the temperature of 130-170 ℃ by adopting nickel-aluminum alloy as a catalyst (for example, aluminum-nickel catalyst disclosed in patent application number 200710021418.0); firstly, under low pressure, butynediol is hydrogenated to generate butylene glycol and 1, 4-butanediol, then, high-pressure hydrogenation is carried out on a fixed bed, the butylene glycol is hydrogenated to be converted into 1, 4-butanediol, the pressure is 18MPa, the temperature is 120-140 ℃, and the catalyst adopts Al 2O3 to load nickel; the nickel-aluminum alloy catalyst and the Al 2O3 supported nickel catalyst have insufficient average activity, so that the content of butanol which is a byproduct in the produced 1, 4-butanediol product is increased to 2.5 percent, and the catalyst has to be replaced after stopping; the activity of the catalyst is maintained for a short time, the later period can be maintained only by increasing the reaction temperature, but the catalyst is not maintained for a long time, the replacement period of the catalyst in the production process is 2-3 months on average, the catalyst is frequently stopped, and the production cost is high.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide the preparation method of the aluminum-nickel alloy catalyst for preparing the 1, 4-butanediol by catalytic hydrogenation, which has the advantages of high catalyst strength, lasting catalyst activity and good activity.
In order to achieve the above purpose, the present invention provides the following technical solutions:
The preparation method of the aluminum-nickel alloy catalyst for preparing the 1, 4-butanediol by catalytic hydrogenation comprises the following steps:
(1) Smelting: mixing a certain proportion of metal nickel plates and metal aluminum ingots, smelting the mixture by an intermediate frequency furnace, stirring the mixture for 2 to 3 minutes after smelting the mixture into a solution, and fully and uniformly mixing the solution to obtain alloy liquid;
(2) And (3) cooling: pouring the alloy liquid in the step (1) into a mould, naturally cooling to 800-1200 ℃ to form an alloy block, spraying deionized water to cool the alloy block to 90-100 ℃ for 2-3min, demoulding, and naturally cooling to normal temperature to obtain a nickel alloy block;
(3) Crushing and screening: selecting, crushing and screening the nickel alloy blocks in the step (2) to obtain alloy particles with the granularity of 3-8 mm;
(4) Calcining: calcining the alloy particles in the step (2) in a roasting furnace at 400-500 ℃ for 8-12min, and introducing inert gas for protection during the calcining;
(5) Dipping and washing: immersing the alloy particles calcined in the step (4) in sodium hydroxide solution; washing the immersed alloy particles with deionized water to obtain the aluminum-nickel alloy catalyst.
Further: in the step (1), 42-50 parts of a metal nickel plate with the content of 99.95% and 50-58 parts of a metal aluminum ingot with the content of 99.85% are mixed according to parts by weight.
Further: the smelting temperature in the step (1) is 1650-2300 ℃ and the smelting time is 15-25min.
Further: the dipping temperature in the step (5) is 95-105 ℃ and the dipping time is 40-60min.
Further: the mass ratio of the alloy particles to the sodium hydroxide solution in the step (5) is 1:5.5; wherein the concentration of the sodium hydroxide solution is 20%.
Further: in step (5), the impregnated alloy particles are washed with deionized water until the pH is 8-11.
Further: in the step (5), the waste alkali liquor and meta-aluminate generated after impregnation are concentrated and sold as byproducts.
Further: in the step (5), the wastewater generated after washing is subjected to a water treatment process to obtain deionized water for impregnation and washing in the step (5).
The invention has the advantages that:
1. According to the invention, the smelted nickel-aluminum alloy is naturally cooled, quenched and naturally cooled to normal temperature, so that the content of Ni 2Al3 crystal phase in the alloy is 35-52% and the content of NiAl 3 crystal phase is 27-52%; the cooling mode improves the content of Ni 2Al3 crystal phase in the alloy, improves the strength of the catalyst, and increases the activity space, so that the activity of the catalyst is durable, and the NiAl 3 crystal phase still has good activity.
2. According to the invention, through calcining the alloy particles, the alloy particles have better strength and larger specific surface, so that the activity durability of the subsequent catalyst is improved, and the catalyst has good catalytic effect.
3. The invention has no waste water and waste discharge in the process of preparing the catalyst, realizes zero discharge and protects the environment.
Drawings
FIG. 1 is a block diagram of the process flow of examples 1-3 of the present invention.
FIG. 2 is an XRD pattern and a crystal phase content distribution diagram of a nickel alloy lump in example 1 of the present invention.
FIG. 3 is an XRD pattern and a crystal phase content distribution diagram of a nickel alloy lump in example 2 of the present invention.
FIG. 4 is an XRD pattern and a crystal phase content distribution diagram of a nickel alloy lump in example 3 of the present invention.
FIG. 5 is an XRD pattern and a crystal phase content distribution diagram of a nickel alloy lump in comparative example 1 of the present invention.
FIG. 6 is an XRD pattern and a crystal phase content distribution diagram of a nickel alloy lump in comparative example 2 of the present invention.
FIG. 7 is an XRD pattern and a crystal phase content distribution diagram of a nickel alloy lump in comparative example 3 of the present invention.
Detailed Description
It should be noted that, without conflict, the embodiments of the present application and features of the embodiments may be combined with each other. The application will be described in detail below with reference to the drawings in connection with embodiments.
It is noted that all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs unless otherwise indicated.
In the present invention, unless otherwise indicated, the terms "upper" and "lower" are used generally with respect to the directions shown in the drawings, or with respect to the vertical, vertical or gravitational directions; also, for ease of understanding and description, "left, right" is generally directed to the left, right as shown in the drawings; "inner and outer" refer to inner and outer relative to the outline of the components themselves, but the above-described orientation terms are not intended to limit the present invention.
Example 1: referring to fig. 1, the present invention provides the following technical solutions: the preparation method of the aluminum-nickel alloy catalyst for preparing the 1, 4-butanediol by catalytic hydrogenation comprises the following steps:
(1) Smelting: mixing 100Kg of metal nickel plate with the content of more than 99.95 percent with 138.1Kg of metal aluminum ingot with the content of more than 99.85 percent, smelting for 20 minutes by an intermediate frequency furnace with the temperature of 1700 ℃, stirring for 2-3 minutes after smelting into a solution, and fully and uniformly mixing to obtain alloy liquid.
(2) And (3) cooling: pouring the alloy liquid in the step (1) into a mould, naturally cooling to 900 ℃ to form an alloy block, and then spraying deionized water to cool the alloy block to 90-100 ℃ in 3min, namely stabilizing free metal ions in the alloy block to obtain more Ni 2Al3 crystal phases; demoulding, and naturally cooling to normal temperature to obtain a nickel alloy block; wherein the content of Ni 2Al3 crystal phase in the nickel alloy block is 62.1%, the content of NiAl 3 crystal phase is 34.4%, and the content of Al crystal phase is 3.4% (shown in figure 2); the cooling mode improves the content of the Ni 2Al3 crystal phase in the alloy, namely improves the strength of the catalyst, and also increases the activity space, so that the activity of the catalyst is durable, and the Ni1Al 3 crystal phase still has good activity.
(3) Crushing and screening: and (3) selecting, crushing and screening the nickel alloy blocks in the step (2) to obtain alloy particles with the granularity of 3-8 mm.
(4) Calcining: and (3) calcining the alloy particles in the step (2) in a roasting furnace at 400 ℃ for 12min, and introducing inert gas for protection during the calcination, so that the alloy particles have better strength and larger specific surface, further the activity durability of the subsequent catalyst is improved, and the catalyst has good catalytic effect.
(5) Dipping and washing: placing 100Kg of the alloy particles calcined in the step (4) in 550Kg of 20% sodium hydroxide solution, and soaking at 95 ℃ for 60min; washing the immersed alloy particles with deionized water until the pH value is 8-11, and obtaining the aluminum-nickel alloy catalyst.
Concentrating the waste alkali liquor and meta-aluminate generated after impregnation, and selling as byproducts; the deionized water is obtained from the wastewater generated after washing through a water treatment process and is used for the impregnation and washing in the step (5), no wastewater or waste is discharged, zero discharge is realized, and the environment is protected.
Example 2: referring to fig. 1, the present invention provides the following technical solutions: the preparation method of the aluminum-nickel alloy catalyst for preparing the 1, 4-butanediol by catalytic hydrogenation comprises the following steps:
(1) Smelting: 100Kg of metal nickel plate with 99.95 percent of content and 138.1Kg of metal aluminum ingot with 99.85 percent of content are mixed and then are smelted by an intermediate frequency furnace with the temperature of 1800 ℃ for 15min, and are stirred for 2-3min after being smelted into solution, so that the alloy liquid is obtained by fully and uniformly mixing the metal nickel plate with the solution.
(2) And (3) cooling: pouring the alloy liquid in the step (1) into a mould, naturally cooling to 900 ℃ to form an alloy block, and then spraying deionized water to cool the alloy block to 90-100 ℃ in 2min, namely stabilizing free metal ions in the alloy block to obtain more Ni 2Al3 crystal phases; demoulding, and naturally cooling to normal temperature to obtain a nickel alloy block; wherein the content of Ni 2Al3 crystal phase in the nickel alloy block is 63.2%, the content of NiAl 3 crystal phase is 33.1%, and the content of Al crystal phase is 3.7% (shown in figure 3); the cooling mode improves the content of Ni 2Al3 crystal phase in the alloy, namely improves the strength of the catalyst, and also increases the activity space, so that the activity of the catalyst is durable, and the NiAl 3 crystal phase still has good activity.
(3) Crushing and screening: and (3) selecting, crushing and screening the nickel alloy blocks in the step (2) to obtain alloy particles with the granularity of 3-8 mm.
(4) Calcining: and (3) calcining the alloy particles in the step (2) in a roasting furnace at 500 ℃ for 8min, and introducing inert gas for protection during the calcination, so that the alloy particles have better strength and larger specific surface, further the activity durability of the subsequent catalyst is improved, and the catalyst has good catalytic effect.
(5) Dipping and washing: placing 100Kg of the alloy particles calcined in the step (4) in 550Kg of 20% sodium hydroxide solution, and soaking for 40min at the temperature of 105 ℃; washing the immersed alloy particles with deionized water until the pH value is 8-11, and obtaining the aluminum-nickel alloy catalyst.
Concentrating the waste alkali liquor and meta-aluminate generated after impregnation, and selling as byproducts; the deionized water is obtained from the wastewater generated after washing through a water treatment process and is used for the impregnation and washing in the step (5), no wastewater or waste is discharged, zero discharge is realized, and the environment is protected.
Example 3: referring to fig. 1, the present invention provides the following technical solutions: the preparation method of the aluminum-nickel alloy catalyst for preparing the 1, 4-butanediol by catalytic hydrogenation comprises the following steps:
(1) Smelting: 100Kg of metal nickel plate with 99.95 percent of content and 138.1Kg of metal aluminum ingot with 99.85 percent of content are mixed and then are smelted by an intermediate frequency furnace with the temperature of 1750 ℃ for 18min, and are stirred for 2-3min after being smelted into solution, so that the alloy liquid is obtained after the mixture is fully and uniformly mixed.
(2) And (3) cooling: pouring the alloy liquid in the step (1) into a mould, naturally cooling to 900 ℃ to form an alloy block, and then spraying deionized water to cool the alloy block to 90-100 ℃ in 2min, namely stabilizing free metal ions in the alloy block to obtain more Ni 2Al3 crystal phases; demoulding, and naturally cooling to normal temperature to obtain a nickel alloy block; wherein the content of Ni 2Al3 crystal phase in the nickel alloy block is 69.7%, the content of NiAl 3 crystal phase is 27.5%, and the content of Al crystal phase is 2.7% (as shown in figure 4); the cooling mode improves the content of Ni 2Al3 crystal phase in the alloy, namely improves the strength of the catalyst, and also increases the activity space, so that the activity of the catalyst is durable, and the NiAl 3 crystal phase still has good activity.
(3) Crushing and screening: and (3) selecting, crushing and screening the nickel alloy blocks in the step (2) to obtain alloy particles with the granularity of 3-8 mm.
(4) Calcining: calcining the alloy particles in the step (2) in a roasting furnace at 450 ℃ for 10min, and introducing inert gas for protection during the calcination, so that the alloy particles have better strength and larger specific surface, further the activity durability of the subsequent catalyst is improved, and the catalyst has good catalytic effect.
(5) Dipping and washing: placing 100Kg of the alloy particles calcined in the step (4) in 550Kg of 20% sodium hydroxide solution, and soaking for 50min at the temperature of 100 ℃; washing the immersed alloy particles with deionized water until the pH value is 8-11, and obtaining the aluminum-nickel alloy catalyst.
Concentrating the waste alkali liquor and meta-aluminate generated after impregnation, and selling as byproducts; the deionized water is obtained from the wastewater generated after washing through a water treatment process and is used for the impregnation and washing in the step (5), no wastewater or waste is discharged, zero discharge is realized, and the environment is protected.
Comparative example 1: the overall process is the same as in example 3, except that step (2) is cooled: pouring the alloy liquid in the step (1) into a mould, and naturally cooling to 90-100 ℃ to obtain a nickel alloy block; wherein the content of Ni 2Al3 crystal phase in the nickel alloy block is 30.5%, the content of NiAl 3 crystal phase is 55.7%, and the content of Al crystal phase is 13.8% (as shown in FIG. 5).
Comparative example 2: the overall process is the same as in example 3, except that step (2) is cooled: pouring the alloy liquid obtained in the step (1) into a die at 1350 ℃, and directly spraying deionized water to cool the alloy block to normal temperature for 5min to obtain a nickel alloy block; wherein the content of Ni 2Al3 crystal phase in the nickel alloy block is 34.8%, the content of NiAl 3 crystal phase is 58%, and the content of Al crystal phase is 7.2% (as shown in FIG. 6).
Comparative example 3: the overall process is the same as in example 3, except that step (2) is cooled: pouring the alloy liquid in the step (1) into a mould, naturally cooling to 900 ℃ to form an alloy block, and then spraying deionized water to cool the alloy block to normal temperature for 3min to obtain a nickel alloy block; wherein the content of Ni 2Al3 crystal phase in the nickel alloy block is 43.3%, the content of NiAl 3 crystal phase is 52.8%, and the content of Al crystal phase is 4% (as shown in FIG. 7).
Comparative example 4: the overall process was the same as in example 3, except that the alloy particles after crushing and sieving in step (3) were directly subjected to the immersing and washing treatment in step (5) without performing the calcination step.
Experiment: the catalysts prepared in examples 1 to 3 and comparative examples 1 to 4, respectively, were used to produce 1, 4-butanediol by a first existing process; wherein the service life of the catalyst and the purity of the prepared 1, 4-butanediol product are shown in the following table 1:
TABLE 1
As can be seen from the above table, the catalysts prepared in examples 1 to 3 have longer service lives than those prepared in comparative examples 1 to 3, and it is fully proved that the catalyst lives are closely related to the content of Ni 2Al3 in the alloy block, the higher the content of Ni 2Al3 is, the higher the strength of the catalyst is, and the activity space is also increased, so that the activity of the catalyst is durable, the service life of the catalyst prepared in example 3 is the highest, and the butanol content in the obtained product is controlled below 2.5%, so that the product requirements are fully met; meanwhile, as can be seen from examples 1-3, the content of the Ni 2Al3 alloy phase obtained in the obvious example 3 is highest, the smelting temperature can influence the formation of the alloy, the alloy structure can be damaged when the temperature is too high, and the alloy reaction effect can be influenced when the temperature is too low; and the service life of the catalyst of the comparative example 4 is lower than that of the catalyst of the example 3, so that the calcining procedure can ensure that the alloy particles have better strength and larger specific surface, further improve the activity durability of the subsequent catalyst and have good catalytic effect.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above examples, and all technical solutions belonging to the concept of the present invention belong to the protection scope of the present invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.
Claims (7)
1. A preparation method of an aluminum-nickel alloy catalyst for preparing 1, 4-butanediol by catalytic hydrogenation is characterized by comprising the following steps of: which comprises the following steps:
(1) Smelting: according to parts by weight, mixing 42-50 parts of metal nickel plate with the content of 99.95% with 50-58 parts of metal aluminum ingot with the content of 99.85%, smelting by an intermediate frequency furnace after mixing, stirring for 2-3min after smelting into a solution, and fully and uniformly mixing to obtain alloy liquid;
(2) And (3) cooling: pouring the alloy liquid in the step (1) into a mould, naturally cooling to 800-1200 ℃ to form an alloy block, spraying deionized water to cool the alloy block to 90-100 ℃ for 2-3min, demoulding, and naturally cooling to normal temperature to obtain a nickel alloy block;
(3) Crushing and screening: selecting, crushing and screening the nickel alloy blocks in the step (2) to obtain alloy particles with the granularity of 3-8 mm;
(4) Calcining: calcining the alloy particles in the step (2) in a roasting furnace at 400-500 ℃ for 8-12min, and introducing inert gas for protection during the calcining;
(5) Dipping and washing: immersing the alloy particles calcined in the step (4) in sodium hydroxide solution; washing the immersed alloy particles with deionized water to obtain the aluminum-nickel alloy catalyst.
2. The method for preparing the aluminum-nickel alloy catalyst for preparing 1, 4-butanediol by catalytic hydrogenation according to claim 1, which is characterized by comprising the following steps: the smelting temperature in the step (1) is 1650-2300 ℃ and the smelting time is 15-25min.
3. The method for preparing the aluminum-nickel alloy catalyst for preparing 1, 4-butanediol by catalytic hydrogenation according to claim 1, which is characterized by comprising the following steps: the dipping temperature in the step (5) is 95-105 ℃ and the dipping time is 40-60min.
4. The method for preparing the aluminum-nickel alloy catalyst for preparing 1, 4-butanediol by catalytic hydrogenation according to claim 1, which is characterized by comprising the following steps: the mass ratio of the alloy particles to the sodium hydroxide solution in the step (5) is 1:5.5; wherein the concentration of the sodium hydroxide solution is 20%.
5. The method for preparing the aluminum-nickel alloy catalyst for preparing 1, 4-butanediol by catalytic hydrogenation according to claim 1, which is characterized by comprising the following steps: in step (5), the impregnated alloy particles are washed with deionized water until the pH is 8-11.
6. The method for preparing the aluminum-nickel alloy catalyst for preparing 1, 4-butanediol by catalytic hydrogenation according to claim 1, which is characterized by comprising the following steps: in the step (5), the waste alkali liquor and meta-aluminate generated after the impregnation are concentrated to be used as byproducts.
7. The method for preparing the aluminum-nickel alloy catalyst for preparing 1, 4-butanediol by catalytic hydrogenation according to claim 1, which is characterized by comprising the following steps: in the step (5), the wastewater generated after washing is subjected to a water treatment process to obtain deionized water for impregnation and washing in the step (5).
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| CN115193443A (en) * | 2022-06-21 | 2022-10-18 | 苏州彼定新材料科技有限公司 | High-activity nickel-aluminum alloy hydrogenation catalyst and preparation method thereof |
| CN116408087A (en) * | 2023-05-11 | 2023-07-11 | 天津理工大学 | Nano porous nickel-based intermetallic compound catalyst and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20220040669A (en) * | 2020-09-24 | 2022-03-31 | 한국과학기술연구원 | A hydrogen generation catalyst comprising a nickel-aluminum intermetallic compound and the method for producing the same |
| CN112479906A (en) * | 2020-12-12 | 2021-03-12 | 弘健制药(上海)有限公司 | Production process of meglumine |
| CN115193443A (en) * | 2022-06-21 | 2022-10-18 | 苏州彼定新材料科技有限公司 | High-activity nickel-aluminum alloy hydrogenation catalyst and preparation method thereof |
| CN116408087A (en) * | 2023-05-11 | 2023-07-11 | 天津理工大学 | Nano porous nickel-based intermetallic compound catalyst and preparation method thereof |
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