CN104645997A - Preparation process of copper-based catalyst - Google Patents
Preparation process of copper-based catalyst Download PDFInfo
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- CN104645997A CN104645997A CN201510075631.4A CN201510075631A CN104645997A CN 104645997 A CN104645997 A CN 104645997A CN 201510075631 A CN201510075631 A CN 201510075631A CN 104645997 A CN104645997 A CN 104645997A
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Abstract
The invention discloses a preparation process of a copper-based catalyst. Hydroxyethyl cellulose is added as a pore forming agent when raw materials are smashed, and then, granulation is carried out. The preparation process comprises the steps of weighing the raw materials; placing the weighed fine granulated raw materials into a reaction tank; adding deionized water into the reaction tank to dissolve the raw materials; adding sodium carbonate into the reaction tank, and stirring; settling; standing; washing; carrying out vacuum filtration; drying the filtered sediment by using a drying oven; firing the dried solid substance by using a muffle furnace; adding graphite, pseudo-boehmite and the hydroxyethyl cellulose into the solid substance, and then, smashing by using a smasher; adding deionized water, and blending in a tray; prepressing the materials by using a prepress; granulating by using a granulator; drying the granules formed by using the granulator; forming by tabletting the dried granules by using a tablet press; and firing in the muffle furnace. By using the preparation process, the stacking density of the prepared granules can be reduced, the weight of the catalyst can be reduced, and the production cost of the catalyst can be lowered.
Description
Technical field
The invention belongs to catalyst preparation technical field, relate to a kind of catalyst preparation process, particularly relate to a kind of preparation technology of copper-based catalysts.
Background technology
In recent years, along with the development of Proton Exchange Membrane Fuel Cells, particularly it is applied to automobile and distributed power generation, in the urgent need to the mobile hydrogen making system of small-sized efficient, efficient, dispersion to supply feed hydrogen.So there is hydrogen generating system miscellaneous, also there is hydrogen production process miscellaneous simultaneously.
A kind of hydrogen production from methanol-steam reforming equipment that such as Chinese patent CN202519022U discloses, described equipment comprises liquid container, heat exchanger, vaporizer, reformer chamber, separation chamber.Described equipment comprises one or more heating unit, for hydrogen producer needs temperature controlled parts to carry out temperature control; The residual air that heating unit is exported by separation chamber is or/and obtained hydrogen heating.Transfer pipe between reformer chamber and separation chamber is through a preheating temperature control mechanism, and this preheating temperature control mechanism is in order to the gas of heating from reformer chamber output; Described preheating temperature control mechanism, as the buffering between reformer chamber and separation chamber, makes the temperature of the gas exported from reformer chamber identical with the temperature of separation chamber or close.
The and for example hydrogen production process that provides of China Patent Publication No. CN101033059, this hydrogen production process does not need outside heat supply due to it, and easy realization scene heats, so receive vast concern.Adopt off-gas to carry out heating system in the method, the result of generation is that each position of system is heated uneven, the most directly, is also that what to affect most is the catalytic activity of catalyst.
The bulk density of copper-based catalysts is in the market greater than 1.20g/mm3, and weight is large, is unfavorable for that portable hydrogen producer uses.
In view of this, nowadays in the urgent need to designing a kind of new hydrogen from methyl alcohol copper-based catalysts, to overcome the above-mentioned defect of existing catalyst.
Summary of the invention
Technical problem to be solved by this invention is: the preparation technology providing a kind of copper-based catalysts, can reduce the bulk density of granulation, alleviates the weight of catalyst; Reduce the production cost of catalyst.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A preparation technology for copper-based catalysts, described preparation technology comprises the steps:
Step S1, raw material are weighed; Electronic balance is utilized to take copper nitrate, zinc nitrate, aluminum nitrate, the zirconium nitrate of set amount;
Step S2, throw in retort by the fine grained raw material after weighing, the volume of retort is 50L;
Step S3, in retort, add deionized water, raw material is dissolved; The rotating speed of setting retort is 450r/min, and temperature is 60 DEG C;
Step S3 ', add aluminium oxide as the nuclei of crystallization and carrier;
Step S4, in retort, add the sodium carbonate of 0.1Mol/l concentration with 23ml/min; Mixing speed 550r/min, temperature is set as constant temperature 60 DEG C;
Step S5, the solution continued in stirred tank; Mixing speed 550r/min, temperature is set as constant temperature 60 DEG C;
Step S6, by the temperature of retort from 60 DEG C of cool to room temperature, place 8 hours;
Step S7, sediment in retort is put into suction filtration, by washed with de-ionized water 3 ~ 6 times;
Step S8, utilize drying box by filter after drying precipitate, temperature is set as 120 DEG C, and drying time is 4 hours;
Step S9, Muffle furnace is utilized to carry out calcination to dried solid; Be warming up to 350 DEG C, the heating-up time is 30 minutes; Constant temperature is at 350 DEG C, and constant temperature time is 4 hours; Be cooled to 200 DEG C, temperature fall time is 3 hours;
Step S10, in solid, add graphite, boehmite, hydroxyethylcellulose, then utilize pulverizer to pulverize;
Step S11, in the powder after pulverizing, add the deionized water of powder gross mass 20% after pulverizing, adjust in pallet and mix 1 hour;
Step S12, the material mixed through toning with preformer precompressed;
Step S13, utilize comminutor according to setting specification carry out granulation;
Step S14, particle that comminutor is formed in drying box with the temperature of 120 DEG C dry 4 hours;
Step S15, utilize tablet press machine by shaping for dried granulation, axial strength is 250N/cm, and the speed of a motor vehicle is 4.0r/min;
Step S16, the material shaping through tablet press machine is put into Muffle furnace carry out calcination; Be warming up to 450 DEG C, the heating-up time is 30 minutes; Constant temperature is at 450 DEG C, and constant temperature time is 4 hours; Be cooled to 200 DEG C, temperature fall time is 3 hours;
Step S17, shaping material to be cooled.
A preparation technology for copper-based catalysts, add hydroxyethylcellulose when pulverizing raw material, hydroxyethylcellulose is as pore creating material; Then carry out granulation.
As a preferred embodiment of the present invention, described preparation technology comprises the steps:
Step S1, raw material are weighed; Electronic balance is utilized to take copper nitrate, zinc nitrate, aluminum nitrate, the zirconium nitrate of set amount;
Step S2, the fine grained raw material after weighing is thrown in retort;
Step S3, in retort, add deionized water, raw material is dissolved;
Step S3 ', add aluminium oxide as the nuclei of crystallization and carrier;
Step S4, in retort, add sodium carbonate, stir;
Step S5, the solution continued in stirred tank;
Step S6, by the temperature cool to room temperature of retort, place setting-up time;
Step S7, sediment in retort is put into suction filtration machine, with suction filtration machine suction filtration and by washed with de-ionized water;
Step S8, utilize drying box by filter after drying precipitate;
Step S9, Muffle furnace is utilized to carry out calcination to dried solid;
Step S10, in solid, add graphite, boehmite, hydroxyethylcellulose, then utilize pulverizer to pulverize;
Step S11, to pulverize after powder in add deionized water, in pallet, carry out tune mix; Preformer is utilized to expect precompressed;
Step S12, the material mixed through toning with preformer precompressed;
Step S13, utilize comminutor according to setting specification carry out granulation;
Step S14, the particle formed by comminutor are dry in drying box;
Step S15, utilize tablet press machine by shaping for dried granulation;
Step S16, the material shaping through tablet press machine is put into Muffle furnace carry out calcination;
Step S17, shaping material to be cooled.
As a preferred embodiment of the present invention, in step S2, the volume of retort is 50L.
As a preferred embodiment of the present invention, in step S8, utilize drying box by the drying precipitate after filtration, temperature is set as 110 ~ 130 DEG C; Drying time is 3 ~ 5 hours.
As a preferred embodiment of the present invention, in step S9, Muffle furnace is utilized to carry out calcination to dried solid; Be warming up to 300-400 DEG C, the heating-up time is 10-120 minute; Constant temperature is at 300-400 DEG C, and constant temperature time is 1-14 hour; Be cooled to 100-300 DEG C, temperature fall time is 1-10 hour.
As a preferred embodiment of the present invention, in step S14, the particle that comminutor is formed in drying box with the dry 1-14 hour of the temperature of 110-130 DEG C;
In step S15, utilize tablet press machine by shaping for dried granulation, axial strength is 200-300N/cm, and the speed of a motor vehicle is 1-14.0r/min.
As a preferred embodiment of the present invention, in step S16, the material shaping through tablet press machine is put into Muffle furnace and carries out calcination; Be warming up to 400-500 DEG C, the heating-up time is 1-60 minute; Constant temperature is at 400-500 DEG C, and constant temperature time is 1-10 hour; Be cooled to 100-300 DEG C, temperature fall time is 1-9 hour.
A preparation technology for copper-based catalysts, in the continuous pipeline of sealing, produce catalyst, described continuous pipeline is divided into settling zone, aging district, scrubbing section, dry section, roast area, disintegrating area, granulation zone, the second dry section, the second roast area successively;
Raw material comprises metal nitrate, precipitant solution; Metal nitrate comprises transition metal nitrate and rare-earth metal nitrate; Transition metal nitrate comprise in copper nitrate, zinc nitrate, aluminum nitrate, ferric nitrate one or more, rare-earth metal nitrate comprise in lanthanum nitrate, zirconium nitrate one or more; Precipitant solution comprise in ammoniacal liquor, sodium carbonate one or more;
Raw material dissolve after pump into pipeline respectively through measuring pump, successively through above-mentioned settling zone, aging district, scrubbing section, dry section, roast area, disintegrating area, granulation zone, the second dry section, the second roast area, finally obtain catalyst;
Described continuous pipeline comprises the first continuous pipeline, scrubbing section pipeline, the second continuous pipeline, disintegrating area pipeline, granulation zone pipeline, the 3rd continuous pipeline, first continuous pipeline comprises settling zone, aging district, second continuous pipeline comprises dry section, roast area, and the 3rd continuous pipeline comprises the second dry section, the second roast area; The outlet of the first continuous pipeline connects the entrance of scrubbing section pipeline by connecting line, the outlet of scrubbing section pipeline connects the entrance of the second continuous pipeline by connecting line, the outlet of the second continuous pipeline connects the entrance of disintegrating area pipeline, the outlet of disintegrating area pipeline connects the entrance of granulation zone pipeline, and the outlet of granulation zone pipeline connects the entrance of the 3rd continuous pipeline;
Described first continuous pipeline is provided with the first magnetic helical axis, and the second continuous pipeline is provided with the second magnetic helical axis, and the 3rd pipeline is provided with the 3rd magnetic helical axis; First magnetic helical axis, the second magnetic helical axis, the 3rd magnetic helical axis drive respectively by respective magnetic drive mechanism;
Scrubbing section is provided with multi-stage water power cyclone, solid-liquid blender, realizes Separation of Solid and Liquid by multi-stage water power cyclone, and solid and washings realize the object of pulling an oar by the powerful magnetic agitation of solid-liquid blender;
Described preparation technology specifically comprises the steps:
Settling step: the built-in pH meter Self-controlled pump in settling zone, controls flow thus control ph by pH meter Self-controlled pump, pH value is controlled 5 ~ 11, is stirred the homogeneous reaction realizing settling zone by the first magnetic helical axis; The temperature of settling zone controls at 35 ~ 85 DEG C;
Aging Step: be linear or snakelike or spirality in aging district slurry pipeline shape, adopts barrier to avoid precipitating slurry completely with settling zone and enters aging district; The temperature in aging district is set as 35 ~ 85 DEG C;
Washing step: realize Separation of Solid and Liquid by multi-stage water power cyclone at scrubbing section, solid and washings realize the object of pulling an oar by the powerful magnetic agitation of solid-liquid blender; The temperature of scrubbing section is set as 20 ~ 85 DEG C;
Drying steps: adopt the second magnetic force helical axis to promote material at dry section; The temperature of dry section is set as 100 ~ 160 DEG C;
Calcination steps: adopt in roast area the second magnetic force helical axis to promote material, finally discharge solid from tube outlet; The temperature of roast area is set as 160-850 DEG C;
Pulverising step: add graphite, boehmite, hydroxyethylcellulose in the solid through roast area roasting, then utilize pulverizer to pulverize;
Granulation step: the deionized water adding powder gross mass 20% after pulverizing in the powder after pulverizing, is adjusted by Tiao Ban mechanism and mixes setting-up time; With the material that preformer precompressed is mixed through toning; Prilling granulator is utilized to carry out granulation according to setting specification;
Second drying steps: adopt the 3rd magnetic force helical axis to promote material at the second dry section; The temperature of the second dry section is set as 100 ~ 160 DEG C;
Second calcination steps: adopt in roast area the second magnetic force helical axis to promote material, finally discharge solid from tube outlet; The temperature of roast area is set as: be warming up to 450 DEG C, and the heating-up time is 30 minutes; Constant temperature is at 450 DEG C, and constant temperature time is 4 hours; Be cooled to 200 DEG C, temperature fall time is 3 hours.
Beneficial effect of the present invention is: the preparation technology of the copper-based catalysts that the present invention proposes, and can reduce the bulk density of granulation, alleviate the weight of catalyst; Reduce the production cost of catalyst.By hydroxyethylcellulose as pore creating material, raw material easily obtains, and cost is low; Obtained catalyst is granular, is convenient to use as in small-sized hydrogen from methyl alcohol equipment.
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation technology of copper-based catalysts of the present invention.
Detailed description of the invention
The preferred embodiments of the present invention are described in detail below in conjunction with accompanying drawing.
Embodiment one
Refer to Fig. 1, present invention is disclosed a kind of preparation technology of copper-based catalysts, described preparation technology comprises the steps:
[step S1] raw material is weighed; Electronic balance is utilized to take copper nitrate, zinc nitrate, aluminum nitrate, the zirconium nitrate of set amount;
Fine grained raw material after weighing is thrown in retort by [step S2], and the volume of retort is 50L;
[step S3] adds deionized water in retort, is dissolved by raw material; The rotating speed of setting retort is 450r/min, and temperature is 60 DEG C;
[step S3 '] add aluminium oxide as the nuclei of crystallization and carrier;
[step S4] adds the sodium carbonate of 0.1Mol/l concentration in retort with 23ml/min; Mixing speed 550r/min, temperature is set as constant temperature 60 DEG C (can be also other temperature, as 50-75 DEG C);
[step S5] continues the solution in stirred tank; Mixing speed 550r/min, temperature is set as constant temperature 60 DEG C;
The temperature of retort from 60 DEG C of (can be also other temperature, as 50-75 DEG C) cool to room temperature, is placed 8 hours by [step S6];
Sediment in retort is put into suction filtration by [step S7], by washed with de-ionized water 3 ~ 6 times;
[step S8] utilizes drying box by the drying precipitate after filtration, temperature is set as 120 DEG C (can be also other temperature, as 105-130 DEG C), and drying time is 4 hours (also can be other times, as 3-5 hour), after dry, the thickness of solid can be set as 3cm;
[step S9] utilizes Muffle furnace to carry out calcination to dried solid; Be warming up to 350 DEG C (can be also other temperature, as 300-400 DEG C), the heating-up time is 30 minutes; Constant temperature is 350 DEG C (can be also other temperature, as 300-400 DEG C), and constant temperature time is 4 hours; Be cooled to 200 DEG C (can be also other temperature, as 150-250 DEG C), temperature fall time is 3 hours;
[step S10] adds graphite, boehmite, hydroxyethylcellulose in solid, then utilizes pulverizer to pulverize;
[step S11] adds the deionized water of powder gross mass 20% after pulverizing in the powder after pulverizing, and adjusts and mix 1 hour in pallet;
The material that [step S12] mixes through toning with preformer precompressed;
[step S13] utilizes comminutor to carry out granulation according to setting specification;
The particle that comminutor is formed by [step S14] in drying box with the temperature of 120 DEG C (can be also other temperature, as 100-150 DEG C) dry 4 hours;
[step S15] utilizes tablet press machine by shaping for dried granulation, and axial strength is 250N/cm, and the speed of a motor vehicle is 4.0r/min;
The material shaping through tablet press machine is put into Muffle furnace and is carried out calcination by [step S16]; Be warming up to 450 DEG C (can be also other temperature, as 400-500 DEG C), the heating-up time is 30 minutes; Constant temperature is 450 DEG C (can be also other temperature, as 400-500 DEG C), and constant temperature time is 4 hours; Be cooled to 200 DEG C (can be also other temperature, as 150-250 DEG C), temperature fall time is 3 hours.
Shaping material cools by [step S17].
Embodiment two
The present invention discloses a kind of preparation technology of copper-based catalysts, in the continuous pipeline of sealing, produce catalyst, described continuous pipeline is divided into settling zone, aging district, scrubbing section, dry section, roast area, disintegrating area, granulation zone, the second dry section, the second roast area successively.
Raw material comprises metal nitrate, precipitant solution; Metal nitrate comprises transition metal nitrate and rare-earth metal nitrate; Transition metal nitrate comprise in copper nitrate, zinc nitrate, aluminum nitrate, ferric nitrate one or more, rare-earth metal nitrate comprise in lanthanum nitrate, zirconium nitrate one or more; Precipitant solution comprise in ammoniacal liquor, sodium carbonate one or more.
Raw material dissolve after pump into pipeline respectively through measuring pump, successively through above-mentioned settling zone, aging district, scrubbing section, dry section, roast area, disintegrating area, granulation zone, the second dry section, the second roast area, finally obtain catalyst.
Described continuous pipeline comprises the first continuous pipeline, scrubbing section pipeline, the second continuous pipeline, disintegrating area pipeline, granulation zone pipeline, the 3rd continuous pipeline, first continuous pipeline comprises settling zone, aging district, second continuous pipeline comprises dry section, roast area, and the 3rd continuous pipeline comprises the second dry section, the second roast area; The outlet of the first continuous pipeline connects the entrance of scrubbing section pipeline by connecting line, the outlet of scrubbing section pipeline connects the entrance of the second continuous pipeline by connecting line, the outlet of the second continuous pipeline connects the entrance of disintegrating area pipeline, the outlet of disintegrating area pipeline connects the entrance of granulation zone pipeline, and the outlet of granulation zone pipeline connects the entrance of the 3rd continuous pipeline.
Described first continuous pipeline is provided with the first magnetic helical axis, and the second continuous pipeline is provided with the second magnetic helical axis, and the 3rd pipeline is provided with the 3rd magnetic helical axis; First magnetic helical axis, the second magnetic helical axis, the 3rd magnetic helical axis drive respectively by respective magnetic drive mechanism.
Scrubbing section is provided with multi-stage water power cyclone, solid-liquid blender, realizes Separation of Solid and Liquid by multi-stage water power cyclone, and solid and washings realize the object of pulling an oar by the powerful magnetic agitation of solid-liquid blender.
Described preparation technology specifically comprises the steps:
Settling step: the built-in pH meter Self-controlled pump in settling zone, controls flow thus control ph by pH meter Self-controlled pump, pH value is controlled 5 ~ 11, is stirred the homogeneous reaction realizing settling zone by the first magnetic helical axis; The temperature of settling zone controls at 35 ~ 85 DEG C;
Aging Step: be linear or snakelike or spirality in aging district slurry pipeline shape, adopts barrier to avoid precipitating slurry completely with settling zone and enters aging district; The temperature in aging district is set as 35 ~ 85 DEG C;
Washing step: realize Separation of Solid and Liquid by multi-stage water power cyclone at scrubbing section, solid and washings realize the object of pulling an oar by the powerful magnetic agitation of solid-liquid blender; The temperature of scrubbing section is set as-20 ~ 85 DEG C;
Drying steps: adopt the second magnetic force helical axis to promote material at dry section; The temperature of dry section is set as 100 ~ 160 DEG C;
Calcination steps: adopt in roast area the second magnetic force helical axis to promote material, finally discharge solid from tube outlet; The temperature of roast area is set as 160-850 DEG C;
Pulverising step: add graphite, boehmite, hydroxyethylcellulose in the solid through roast area roasting, then utilize pulverizer to pulverize;
Granulation step: the deionized water adding powder gross mass 20% after pulverizing in the powder after pulverizing, is adjusted by Tiao Ban mechanism and mixes setting-up time; With the material that preformer precompressed is mixed through toning; Prilling granulator is utilized to carry out granulation according to setting specification;
Second drying steps: adopt the 3rd magnetic force helical axis to promote material at the second dry section; The temperature of the second dry section is set as 100 ~ 160 DEG C;
Second calcination steps: adopt in roast area the second magnetic force helical axis to promote material, finally discharge solid from tube outlet; The temperature of roast area is set as: be warming up to 450 DEG C, and the heating-up time is 30 minutes; Constant temperature is at 450 DEG C, and constant temperature time is 4 hours; Be cooled to 200 DEG C, temperature fall time is 3 hours.
The present embodiment can realize Automated condtrol continuous seepage, reduces power consumption, enhances productivity, reduce costs, can produce high-quality catalyst prod; Can effectively avoid harmful gases diffusion in air, environmental protection more simultaneously.
In sum, the preparation technology of the copper-based catalysts that the present invention proposes, can reduce the bulk density of granulation, alleviate the weight of catalyst; Reduce the production cost of catalyst.By hydroxyethylcellulose as pore creating material, raw material easily obtains, and cost is low; Obtained catalyst is granular, is convenient to use as in small-sized hydrogen from methyl alcohol equipment.
Here description of the invention and application is illustrative, not wants by scope restriction of the present invention in the above-described embodiments.Distortion and the change of embodiment disclosed are here possible, are known for the replacement of embodiment those those of ordinary skill in the art and the various parts of equivalence.Those skilled in the art are noted that when not departing from spirit of the present invention or substantive characteristics, the present invention can in other forms, structure, layout, ratio, and to realize with other assembly, material and parts.When not departing from the scope of the invention and spirit, can other distortion be carried out here to disclosed embodiment and change.
Claims (9)
1. a preparation technology for copper-based catalysts, is characterized in that, described preparation technology comprises the steps:
Step S1, raw material are weighed; Electronic balance is utilized to take copper nitrate, zinc nitrate, aluminum nitrate, the zirconium nitrate of set amount;
Step S2, throw in retort by the fine grained raw material after weighing, the volume of retort is 50L;
Step S3, in retort, add deionized water, raw material is dissolved; The rotating speed of setting retort is 450r/min, and temperature is 60 DEG C;
Step S3 ', add aluminium oxide as the nuclei of crystallization and carrier;
Step S4, in retort, add the sodium carbonate of 0.1Mol/l concentration with 23ml/min; Mixing speed 550r/min, temperature is set as constant temperature 60 DEG C;
Step S5, the solution continued in stirred tank; Mixing speed 550r/min, temperature is set as constant temperature 60 DEG C;
Step S6, by the temperature of retort from 60 DEG C of cool to room temperature, place 8 hours;
Step S7, sediment in retort is put into suction filtration, by washed with de-ionized water 3 ~ 6 times;
Step S8, utilize drying box by filter after drying precipitate, temperature is set as 120 DEG C, and drying time is 4 hours;
Step S9, Muffle furnace is utilized to carry out calcination to dried solid; Be warming up to 350 DEG C, the heating-up time is 30 minutes; Constant temperature is at 350 DEG C, and constant temperature time is 4 hours; Be cooled to 200 DEG C, temperature fall time is 3 hours;
Step S10, in solid, add graphite, boehmite, hydroxyethylcellulose, then utilize pulverizer to pulverize;
Step S11, in the powder after pulverizing, add the deionized water of powder gross mass 20% after pulverizing, adjust in pallet and mix 1 hour;
Step S12, the material mixed through toning with preformer precompressed;
Step S13, utilize comminutor according to setting specification carry out granulation;
Step S14, particle that comminutor is formed in drying box with the temperature of 120 DEG C dry 4 hours;
Step S15, utilize tablet press machine by shaping for dried granulation, axial strength is 250N/cm, and the speed of a motor vehicle is 4.0r/min;
Step S16, the material shaping through tablet press machine is put into Muffle furnace carry out calcination; Be warming up to 450 DEG C, the heating-up time is 30 minutes; Constant temperature is at 450 DEG C, and constant temperature time is 4 hours; Be cooled to 200 DEG C, temperature fall time is 3 hours;
Step S17, shaping material to be cooled.
2. a preparation technology for copper-based catalysts, is characterized in that, add hydroxyethylcellulose when pulverizing raw material, hydroxyethylcellulose is as pore creating material; Then carry out granulation.
3. the preparation technology of copper-based catalysts according to claim 2, is characterized in that:
Described preparation technology comprises the steps:
Step S1, raw material are weighed; Electronic balance is utilized to take copper nitrate, zinc nitrate, aluminum nitrate, the zirconium nitrate of set amount;
Step S2, the fine grained raw material after weighing is thrown in retort;
Step S3, in retort, add deionized water, raw material is dissolved;
Step S3 ', add aluminium oxide as the nuclei of crystallization and carrier;
Step S4, in retort, add sodium carbonate, stir;
Step S5, the solution continued in stirred tank;
Step S6, by the temperature cool to room temperature of retort, place setting-up time;
Step S7, sediment in retort is put into suction filtration machine, with suction filtration machine suction filtration and by washed with de-ionized water;
Step S8, utilize drying box by filter after drying precipitate;
Step S9, Muffle furnace is utilized to carry out calcination to dried solid;
Step S10, in solid, add graphite, boehmite, hydroxyethylcellulose, then utilize pulverizer to pulverize;
Step S11, to pulverize after powder in add deionized water, in pallet, carry out tune mix; Preformer is utilized to expect precompressed;
Step S12, the material mixed through toning with preformer precompressed;
Step S13, utilize comminutor according to setting specification carry out granulation;
Step S14, the particle formed by comminutor are dry in drying box;
Step S15, utilize tablet press machine by shaping for dried granulation;
Step S16, the material shaping through tablet press machine is put into Muffle furnace carry out calcination;
Step S17, shaping material to be cooled.
4. the preparation technology of copper-based catalysts according to claim 2, is characterized in that:
In step S2, the volume of retort is 50L.
5. the preparation technology of copper-based catalysts according to claim 2, is characterized in that:
In step S8, utilize drying box by the drying precipitate after filtration, temperature is set as 110 ~ 130 DEG C; Drying time is 3 ~ 5 hours.
6. the preparation technology of copper-based catalysts according to claim 2, is characterized in that:
In step S9, Muffle furnace is utilized to carry out calcination to dried solid; Be warming up to 300-400 DEG C, the heating-up time is 10-120 minute; Constant temperature is at 300-400 DEG C, and constant temperature time is 1-14 hour; Be cooled to 100-300 DEG C, temperature fall time is 1-10 hour.
7. the preparation technology of copper-based catalysts according to claim 2, is characterized in that:
In step S14, the particle that comminutor is formed in drying box with the dry 1-14 hour of the temperature of 110-130 DEG C;
In step S15, utilize tablet press machine by shaping for dried granulation, axial strength is 200-300N/cm, and the speed of a motor vehicle is 1-14.0r/min.
8. the preparation technology of copper-based catalysts according to claim 2, is characterized in that:
In step S16, the material shaping through tablet press machine is put into Muffle furnace and carries out calcination; Be warming up to 400-500 DEG C, the heating-up time is 1-60 minute; Constant temperature is at 400-500 DEG C, and constant temperature time is 1-10 hour; Be cooled to 100-300 DEG C, temperature fall time is 1-9 hour.
9. the preparation technology of a copper-based catalysts, it is characterized in that, in the continuous pipeline of sealing, produce catalyst, described continuous pipeline is divided into settling zone, aging district, scrubbing section, dry section, roast area, disintegrating area, granulation zone, the second dry section, the second roast area successively;
Raw material comprises metal nitrate, precipitant solution; Metal nitrate comprises transition metal nitrate and rare-earth metal nitrate; Transition metal nitrate comprise in copper nitrate, zinc nitrate, aluminum nitrate, ferric nitrate one or more, rare-earth metal nitrate comprise in lanthanum nitrate, zirconium nitrate one or more; Precipitant solution comprise in ammoniacal liquor, sodium carbonate one or more;
Raw material dissolve after pump into pipeline respectively through measuring pump, successively through above-mentioned settling zone, aging district, scrubbing section, dry section, roast area, disintegrating area, granulation zone, the second dry section, the second roast area, finally obtain catalyst;
Described continuous pipeline comprises the first continuous pipeline, scrubbing section pipeline, the second continuous pipeline, disintegrating area pipeline, granulation zone pipeline, the 3rd continuous pipeline, first continuous pipeline comprises settling zone, aging district, second continuous pipeline comprises dry section, roast area, and the 3rd continuous pipeline comprises the second dry section, the second roast area; The outlet of the first continuous pipeline connects the entrance of scrubbing section pipeline by connecting line, the outlet of scrubbing section pipeline connects the entrance of the second continuous pipeline by connecting line, the outlet of the second continuous pipeline connects the entrance of disintegrating area pipeline, the outlet of disintegrating area pipeline connects the entrance of granulation zone pipeline, and the outlet of granulation zone pipeline connects the entrance of the 3rd continuous pipeline;
Described first continuous pipeline is provided with the first magnetic helical axis, and the second continuous pipeline is provided with the second magnetic helical axis, and the 3rd pipeline is provided with the 3rd magnetic helical axis; First magnetic helical axis, the second magnetic helical axis, the 3rd magnetic helical axis drive respectively by respective magnetic drive mechanism;
Scrubbing section is provided with multi-stage water power cyclone, solid-liquid blender, realizes Separation of Solid and Liquid by multi-stage water power cyclone, and solid and washings realize the object of pulling an oar by the powerful magnetic agitation of solid-liquid blender;
Described preparation technology specifically comprises the steps:
Settling step: the built-in pH meter Self-controlled pump in settling zone, controls flow thus control ph by pH meter Self-controlled pump, pH value is controlled 5 ~ 11, is stirred the homogeneous reaction realizing settling zone by the first magnetic helical axis; The temperature of settling zone controls at 35 ~ 85 DEG C;
Aging Step: be linear or snakelike or spirality in aging district slurry pipeline shape, adopts barrier to avoid precipitating slurry completely with settling zone and enters aging district; The temperature in aging district is set as 35 ~ 85 DEG C;
Washing step: realize Separation of Solid and Liquid by multi-stage water power cyclone at scrubbing section, solid and washings realize the object of pulling an oar by the powerful magnetic agitation of solid-liquid blender; The temperature of scrubbing section is set as 20 ~ 85 DEG C;
Drying steps: adopt the second magnetic force helical axis to promote material at dry section; The temperature of dry section is set as 100 ~ 160 DEG C;
Calcination steps: adopt in roast area the second magnetic force helical axis to promote material, finally discharge solid from tube outlet; The temperature of roast area is set as 160-850 DEG C;
Pulverising step: add graphite, boehmite, hydroxyethylcellulose in the solid through roast area roasting, then utilize pulverizer to pulverize;
Granulation step: the deionized water adding powder gross mass 20% after pulverizing in the powder after pulverizing, is adjusted by Tiao Ban mechanism and mixes setting-up time; With the material that preformer precompressed is mixed through toning; Prilling granulator is utilized to carry out granulation according to setting specification;
Second drying steps: adopt the 3rd magnetic force helical axis to promote material at the second dry section; The temperature of the second dry section is set as 100 ~ 160 DEG C;
Second calcination steps: adopt in roast area the second magnetic force helical axis to promote material, finally discharge solid from tube outlet; The temperature of roast area is set as: be warming up to 450 DEG C, and the heating-up time is 30 minutes; Constant temperature is at 450 DEG C, and constant temperature time is 4 hours; Be cooled to 200 DEG C, temperature fall time is 3 hours.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4091086A (en) * | 1976-12-20 | 1978-05-23 | Engelhard Minerals & Chemicals Corporation | Process for production of hydrogen |
| CN103816945A (en) * | 2014-01-29 | 2014-05-28 | 上海摩醇动力技术有限公司 | Continuous catalyst production process and equipment |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4091086A (en) * | 1976-12-20 | 1978-05-23 | Engelhard Minerals & Chemicals Corporation | Process for production of hydrogen |
| CN103816945A (en) * | 2014-01-29 | 2014-05-28 | 上海摩醇动力技术有限公司 | Continuous catalyst production process and equipment |
Non-Patent Citations (1)
| Title |
|---|
| 雷乐成 著: "《水处理高级氧化技术》", 31 December 2001 * |
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