CN1380255A - Method and equipment for preparing basic carbonate nano particle by means of spray pyrolysis of ammonia complex liquor - Google Patents
Method and equipment for preparing basic carbonate nano particle by means of spray pyrolysis of ammonia complex liquor Download PDFInfo
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- CN1380255A CN1380255A CN 01141392 CN01141392A CN1380255A CN 1380255 A CN1380255 A CN 1380255A CN 01141392 CN01141392 CN 01141392 CN 01141392 A CN01141392 A CN 01141392A CN 1380255 A CN1380255 A CN 1380255A
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- ammonia complex
- ammonia
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- 238000000034 method Methods 0.000 title claims abstract description 60
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 37
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 title claims abstract description 34
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims description 164
- 229910021529 ammonia Inorganic materials 0.000 title claims description 76
- 238000005118 spray pyrolysis Methods 0.000 title claims description 28
- 239000007921 spray Substances 0.000 claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims description 77
- 238000004519 manufacturing process Methods 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 18
- 230000000536 complexating effect Effects 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 239000004744 fabric Substances 0.000 claims description 10
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 10
- 238000011084 recovery Methods 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 238000011112 process operation Methods 0.000 claims description 7
- 238000004064 recycling Methods 0.000 claims description 7
- 229910021645 metal ion Inorganic materials 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000005507 spraying Methods 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- IWLXWEWGQZEKGZ-UHFFFAOYSA-N azane;zinc Chemical compound N.[Zn] IWLXWEWGQZEKGZ-UHFFFAOYSA-N 0.000 claims description 3
- NBFQLHGCEMEQFN-UHFFFAOYSA-N N.[Ni] Chemical compound N.[Ni] NBFQLHGCEMEQFN-UHFFFAOYSA-N 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- QKSIFUGZHOUETI-UHFFFAOYSA-N copper;azane Chemical compound N.N.N.N.[Cu+2] QKSIFUGZHOUETI-UHFFFAOYSA-N 0.000 claims description 2
- 238000005516 engineering process Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 238000000746 purification Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims 2
- 238000000926 separation method Methods 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 23
- 229910002092 carbon dioxide Inorganic materials 0.000 description 15
- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O UOURRHZRLGCVDA-UHFFFAOYSA-D 0.000 description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 7
- 239000002245 particle Substances 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 4
- 238000012824 chemical production Methods 0.000 description 4
- 229940116318 copper carbonate Drugs 0.000 description 4
- GEZOTWYUIKXWOA-UHFFFAOYSA-L copper;carbonate Chemical compound [Cu+2].[O-]C([O-])=O GEZOTWYUIKXWOA-UHFFFAOYSA-L 0.000 description 4
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 description 4
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000007791 dehumidification Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910000010 zinc carbonate Inorganic materials 0.000 description 1
- 235000004416 zinc carbonate Nutrition 0.000 description 1
- 239000011667 zinc carbonate Substances 0.000 description 1
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The present invention utilizes ammino-complex liquor and hot air and special-purpose complete set of equipment, and adopting a series of suitable technological process and method to prepare basic carbonate nano particles. Its special-purpose equipment is formed from centrifugal spray dryer and cyclone separator, said complete set of equipment can integrated several process of mixing, reaction, drying and separation into one step, so that its technological process is short and its product quality is raised.
Description
The technical field is as follows:
the invention relates to a method and equipment for preparing basic carbonate nanoparticles by spray pyrolysis of ammonia complex liquid, belonging to the technical field of chemical production process and chemical production equipment, in particular to a process method and special equipment for preparing the basic carbonate nanoparticles by mixing the ammonia complex liquid with dry hot air and carrying out pyrolysis reaction in a spray dryer.
Secondly, background art:
the basic carbonate is prepared from ammine complex metal (such as zinc, copper, nickel, cadmium, etc.), and the purpose is to prepare each metal oxide by decomposition or reduction of the basic carbonate. Therefore, the former is just the front work of chemical production and is the production process method for preparing the basic carbonate by using the ammine metal solution and hot air spray pyrolysis equipment. The technological scheme of the present invention is that the technological process of preparing alkali carbonate through spray pyrolysis reaction of ammonia complex liquid and hot air is shortened and includes mixing, reaction, precipitation, separation, drying and other steps. Therefore, the production flow is shortened, the process is simplified, the production period is shortened, the production cost and the production time are reduced, good production benefit and economic benefit are brought, and a way is opened up for continuous large-scale production. As regards the spray pyrolysis drying apparatus, documents are found: chinese patent No.: 96208591, the name is: a gas dehumidification and enthalpy reduction centrifugal separation device; chinese patent No.: 96230889, the name is: a combined spray drying tower is composed of an atomizer, a dust filtering cloth bag and the like, and is also disclosed in Chinese patent numbers: 99245619 entitled structural improvement of spray dryer, which is composed of a spray dryer and a cyclone separator. Although the products produced by these three patents are different, the structure and construction of these devices for different uses will naturally vary greatly, which is a result of the practical needs and considerations. The spray pyrolysis drying process and the special equipment are improved in the aspects of the process method and the equipment to prepare the basic carbonate nanoparticles aiming at the aim of preparing the basic carbonate nanoparticles by using the ammonia complex solution and the hot air, and lay a good foundation for preparing the metal oxide nano material by using the basic carbonate nanoparticles in the next step. The crystal grain diameter of the basic carbonate prepared by us is 5 nm or less by observing through a transmission electron microscope.
Thirdly, the invention content:
the invention aims to disclose a process method and special equipment for preparing basic carbonate nanoparticles by spray pyrolysis of ammonia complex liquid to the society, and make some contributions to promoting the chemical production and progress in the field.
The technical scheme of the invention comprises the technical scheme about the process method and the technical scheme about special equipment.
The technical scheme of the process method of the invention is as follows: the method for preparing basic carbonate nano particles by ammonia complex liquid spray pyrolysis is characterized in that the ammonia complex liquid and dry hot air with a certain temperature are adopted, a practical process operation technology is adopted, and the process procedures and the operation method for preparing the basic carbonate nano particles by reaction, drying, separation and recovery in special complete equipment for spray pyrolysis are adopted. The technical key points are as follows: a. preparing materials and feeding: sufficiently preparing the ammonia complex solution after impurity removal and purification and hot air materials, and producing the ammonia complex solution and the hot air materials in a spray pyrolysis complete equipment consisting of a centrifugal spray dryer and a cyclone separator for standby; introducing the ammonia complex liquid for later use into a centrifugal spray dryer from a feed inlet, wherein the process operation conditions are as follows: the temperature is 30-50 ℃ under normal pressure, and the content of the metal ions in the ammonia complexing liquid is 3-20% (weight ratio); meanwhile, introducing standby hot air into the centrifugal spray dryer from another feeding hole, wherein the process operating conditions are as follows: the hot air temperature is 250 ℃ and 400 ℃, and the feeding amount of the hot air is matched according to the feeding amount of the ammonia complex liquidThe proper proportion, the proper feeding amount and the proper proportion thereof are very important, which can affect the production effect and the production quality of the process method, and the preferable proportion can be summarized from production experiments and production practice; b. atomizing and reacting: the ammonia complex liquid entering the centrifugal spray dryer from the two material ports and the hot air are fed into a centrifugal atomizing disk rotating at a high speed along a feeding guide pipe to be mixed, and then are atomized at a high speed along a tangent line according to a certain linear speed to be sprayed into a cylinder of the dryer, and after reaction and drying, the materials enter a cyclone separator, and the process operation conditions are as follows: the rotating speed of the centrifugal atomizing disk is 5000-30000 r/m, and the process is continuously carried out until the production is finished; c. separating and taking out: entering cyclone separators tangentiallyThe mixed material is settled along the cylinder cyclone of the separator, and the separated dry powder basic carbonate nano particles are taken out from the outlet at the bottom end of the separator and contain NH3、CO2And water vapor (H)2O) is discharged from a top exhaust pipe of the cyclone separator.
The detailed technical content of the process method also comprises the following steps: a. the preferred rotating speed of the atomizing disc is as follows: according to the different diameters of the atomizing disk, the rotating speed of the atomizing disk is selected between 5000 and 30000 revolutions per minute, and the rotating speed of the sprayed droplets at 1-5 mu m is taken as the preferred rotating speed; b. the content of the complexing metal ions in the feed ammonia complexing liquid is not more than 20 percent (weight ratio); c. the feed proportioning is as follows: the feeding proportion of the ammonia complex liquid and the hot air is different according to the diameter of the dryer, and the proportion is preferably that the mixture at the outlet of the lower end of the spray dryer is completely vaporized without liquid drops; d. gas recovery: the special complete equipment can be used for feeding gas recovery device, namely a pulse cloth bag catcher, a gas outlet at the upper end of a cyclone separator is connected to a feeding pipe of the pulse cloth bag catcher, a suction fan is used for sucking air through a cloth bag to recover partial basic carbonate nano particles escaping from the cyclone separator, and separated gas NH3、CO2Water vapor (H)2And O), collecting the waste water from the catcher, entering a condensation spraying device, and recycling the waste water for production. This not only saves raw material NH3、CO2Etc. and is also beneficial to environmental protection.
The technical scheme of the special equipment of the invention is as follows: the equipment for preparing basic carbonate nano particles by using ammonia complex liquid and dry hot air through spray pyrolysis is a special complete equipment for preparing basic carbonate nano particles by using ammonia complex liquid and dry hot air according to an applicable technological operation method, wherein the ammonia complex liquid comprises zinc ammonia complex liquid, copper ammonia complex liquid, nickel ammonia complex liquid and the like, and metal ammonia complex liquid which can be subjected to complex reaction with ammonia or can be subjected to complex reaction with ammonia after being treated by acertain physical and chemical method, and the technical method is characterized in that the metal ammonia complex liquid is prepared by using the ammonia complex liquid and the dry hot airThe key points of the technique are as follows: the special equipment is formed by combining a centrifugal spray dryer and a cyclone separator in a set: a. the centrifugal spray dryer takes charge of the processes of feeding, mixing, reacting and drying, the centrifugal spray dryer is cylindrical, and the upper part of the centrifugal spray dryer is provided with a high-speed rotating impellerThe atomizing disc is uniformly provided with vertical blades along the radial direction and is sealed at the upper part and the lower part, the outer edge of the disc forms an atomizing opening, the central part of the upper cover of the disc is upwards provided with a feeding conduit, the conduit extends out of the top of the cylinder, the upper end of the conduit forms two feeding holes for ammonia complex liquid and hot air, the atomizing disc is driven by a power shaft or a transmission shaft extending into the center of the feeding conduit, the cylindrical lower part of the dryer is contracted into a horn mouth shape with a large upper part and a small lower part, and the bottom end of the dryer forms an outlet pipe which can be communicated with; feeding conditions of ammonia complex liquid: the liquid temperature is 30-50 ℃ under normal pressure, the ammonia complex liquid enters a spray dryer from a feed inlet of the ammonia complex liquid, the content of the complex metal in the ammonia complex liquid is 3-20% (weight ratio), and the feeding conditions of the dry hot air are as follows: the temperature is 250 ℃ plus 400 ℃, the mixture enters a spray dryer from an air feeding hole, the mixture ratio of hot air feeding and ammonia complex liquid is proper, the rotation speed of an atomizing disc is 5000 plus 30000 r/min, and the material after reaction and drying is conveyed into a feeding pipe of a cyclone separator from an outlet pipe at the bottom end of the dryer and enters the cyclone separator along the tangential feeding hole; b. the cyclone separator is cylindrical, a feed inlet at the upper part of the cyclone separator is arranged in the tangential direction with the cylindrical circular surface, the lower part of the cyclone separator is also in a bell mouth shape with a large upper part and a small lower part, a pipe is arranged at the bottom end of the cyclone separator to form an outlet, another gas outlet pipe vertically extends into the cylinder from the center of the top of the cylinder, and an inverted bell-shaped cover is arranged at the middle lower part in the cylinder; the process conditions are as follows: naturally cooling and separating under micro-negative pressure, taking out the basic carbonate from the outlet at the lower part of the separator, and reacting to generate gas NH3、CO2And the gas is discharged from a gas outlet for recycling.
The detailed technical contents of the special equipment are as follows: a. rotating speed of the atomizing disc: according to the different diameters of the atomizing disk, the rotating speed of the atomizing disk is selected between 5000-30000 r/min, and the rotating speed of the sprayed droplets at 1-5 mu m is taken as the preferred rotating speed; b. the content of the complexing metal ions in the feed ammonia complexing liquid is not more than 20 percent (weight ratio); c. the proportion of the hot air feeding amount and the ammonia complex liquid is preferably that the mixture at the outlet of the lower end of the spray dryer is completely gasified without liquid drops according to different diameters of the dryer; d. diameter of the dryer: the diameter can be between 500mm and 5000mm or more according to the requirements of the rotating speed and the production capacity of the atomizing diskSmaller and larger; e. the complete equipment can also be added with a clothbag catcher and a gas recovery device, a gas outlet at the upper end of the cyclone separator is connected with a feeding pipe of the pulse cloth bag catcher, partial basic carbonate nano particles escaping from the cyclone separator and separated gas NH are recovered by using an exhaust fan to exhaust3、CO2And H2O (water vapor) is discharged from an outlet pipe after passing through a catcher, enters a condensation spraying device, and is recycled for use in production.
The method and the equipment for preparing the basic carbonate nano particles by the spray pyrolysis of the ammonia complex solution have the advantages that: the spray pyrolysis process method integrates multiple process procedures of mixing, reacting, precipitating, separating, drying and the like, shortens the process flow, reduces production equipment, saves investment and time, improves the production efficiency and brings good production benefit. The quality of the product can be improved by adopting the process and the equipment. It is emphasized that: the basic zinc carbonate product prepared by the production process method and the complete special equipment has good stability and repeatability, and the particle size of the prepared basic zinc carbonate is below 5 nanometers by field inspection and measurement of amplifying one hundred thousand times by using an H-600 transmission electron microscope.
Fourthly, explanation of the attached drawings:
the attached figures of the specification of the invention are 2.
FIG. 1 is a schematic flow diagram of the production process of the present invention;
FIG. 2 is a schematic diagram of the spray dryer configuration of one of the apparatus used in the present invention;
in each figure: 1. an ammonia complexing liquid tank; 2. an ammonia complex liquid pump; 3. an air filter; 4. an air blower; 5. a hot blast stove; 6. a spray dryer; 7. a cyclone separator; 8. a pulse bag type trap; 9. a screw conveyor; 10. a tail gas blower; 11. an absorption tower; 12. a circulating liquid tank; 13. a circulating liquid pump; 14. a motor; 15. feeding ammonia complex liquid; 16. feeding hot air; 17. the resultant basic carbonate; 18. recovered NH3、CO2(ii) a 19. Exhaust air, water vapor, etc.; 20. a motor; 21. a speed increaser; 22. a main shaft; 23. a hot air inlet; 24. ammonia complexA liquid combination inlet; 25. a guide vane; 26. an atomizing disk; 27. a barrel; 28. a cone; 29. and (4) a discharge port.
The fifth embodiment is as follows:
the non-limiting examples of the technical scheme of the invention are as follows:
the first method and equipment for preparing basic zinc carbonate nano particle by spray pyrolysis of ammonia complex liquid.
1. The technical specification and the operation method of the embodiment are as follows:
the production process flow of this example is shown in FIG. 1. The technological process and the operation method are as follows:
preparing materials and feeding: ammonia complex liquid with zinc ion content of 20 wt% and at 30-50 deg.c is pumped into the material liquid pipe of the spray drier and flows downwards to the atomizing disc; the filtered air is pressurized by a blower and enters a hot blast stove, and hot air with the temperature of 350-400 ℃ from the hot blast stove enters from a hot blast pipe at the top of the spray dryer and fully atomizes and contacts with the ammonia complex liquid at an atomizing disc.
Atomizing and reacting: the zinc-ammonia complex liquid entering the centrifugal atomizing disc with the rotating speed of 20000 revolutions per minute or 30000 revolutions per minute is atomized at high speed along the tangential direction, sprayed into the circular cylinder of the dryer and contacted with high-temperature hot air around the atomizing disc in a parallel flow manner, the moisture is rapidly evaporated, and the following pyrolysis reaction occurs:
basic zinc carbonate particles having a particle size of 5 nm or less are produced.
Separating and taking out: and gas containing basic zinc carbonate particles, ammonia gas, carbon dioxide and water vapor is discharged from the bottom of the spray dryer and enters a cyclone separator, then basic zinc carbonate nanoparticles are separated from an outlet at the bottom of the separator, and the ammonia gas, the carbon dioxide, the water vapor and other gases are discharged from an outlet at the top of the cyclone separator.
Gas recovery: the gas discharged from the top outlet of the cyclone separator can also enter a cloth bag catcher to further separate and recover the residual alkaliThe zinc carbonate nanoparticles are then pumped with gaseous NH by an exhaust blower3、CO2And entering a condensation spraying device to recycle ammonia and carbon dioxide.
2. The special equipment of this example, which is composed of centrifugal spray dryer and cyclone separator, and can be added with bag catcher and gas recovery device, is shown in figure 1, wherein the centrifugal spray dryer is used to complete the processes of feeding, atomizing, mixing, reacting, drying, etc., and then the cyclone separator is used to complete the reaction product basic zinc carbonate nano particlesand gas NH3、CO2Water, waterSteam (H)2O), if a cloth bag trap is added for matching use, the trap can further separate and recover reactant basic zinc carbonate particles, and gas condensing, spraying and other recovery devices are combined for use, so that NH is generated3、CO2The gas is further recycled and reused, and the effect is better. The spray dryer is shown in figure 2, the height of the cylinder of the centrifugal spray dryer is 2000mm, the diameter of the section of the cylinder is 1500mm, the lower part of the cylinder is in a shape of a big-end-up cone (inverted trumpet), the height of the cone is 1000mm, the lower part of the cone is a reactant outlet and can be connected with an inlet of a cyclone separator, a hot air inlet pipe and an ammonia complexing liquid inlet pipe are arranged in the top of the centrifugal spray dryer, a motor-driven or transmission shaft is vertically arranged in the central part of the inlet pipe, a high-speed rotating atomizing disk is arranged at the lower end of the shaft, the spray dryer is a parallel flow type centrifugal spray dryer, the diameter of the atomizing disk is 30mm-50mm, blades are radially arranged in the disk, the rotating atomizing disk forms an atomized liquid outlet at the periphery of the cylindrical disk, the rotating disk rotates at 20000 revolutions/or 30000 revolutions/. The temperature of the hot air is 350-. The concentration of complex zinc ions in the feeding ammonia complex liquid is 20% (weight ratio), and the amount of hot air feeding is proper according to the feeding amount of the ammonia complex liquid. The reacted material enters a cyclone separator from a discharge port at the lower part of a centrifugal sprayer, and the upper part of the cyclone separator is provided with a cyclone separatorThe reaction material entering the separator is rotationally settled in the separator by a feeding pipe along the tangential direction of the circular section of theseparator, the separated basic zinc carbonate nano particles are taken out from the bottom of the separator, and gas NH is generated3、CO2With water vapor (H)2O), etc. from the exhaust pipe at the top of the separator to a bag catcher to further separate the residual basic zinc carbonate particles and gas NH3、CO2Continuously recycling NH by recycling devices such as condensation and spraying3、CO2Used in reproduction. The cyclone separator may be installed and used with any suitable commercially available product.
Example II A method and apparatus for preparing basic copper carbonate nanoparticles by spray pyrolysis of ammonia complex solution.
The technological process for preparing basic copper carbonate nano particles by spray pyrolysis of ammonia complex liquid in the example is the same as the first example, the difference of the first example is that the basic copper carbonate nano particles are prepared by spray pyrolysis of the ammonia complex liquid of complex copper, the ammonia complex liquid entering a sprayer contains 11 percent (weight ratio) of complex copper ions, the hot air temperature is 250-300 ℃, the diameter of a centrifugal atomizing disk is 160mm, and the rotating speed is 10000 r/min or 15000 r/min. The equation for the chemical reaction of the materials is:
the equipment for preparing basic copper carbonate by spray pyrolysis of ammonia complex liquid in the example is the same as that described in the example I, and different from the example I, the centrifugal sprayer, the cyclone separator and the like in the example I can select or design equipment with different sizes according to factors such as the amount of production or the like or according to the example I. The rest is notdescribed, is all used for the description in the example one and is not repeated.
EXAMPLE III method and apparatus for preparing basic nickel carbonate nano particles by spray pyrolysis of ammonia complex liquid
The technological process for preparing the basic nickel carbonate nano particles by spray pyrolysis of the ammonia complex liquid is the same as the first example, and is different from the first example in that the basic nickel carbonate nano particles are prepared by spray pyrolysis of the ammonia complex liquid of nickel, the content of complex nickel ions in the ammonia complex liquid entering a sprayer is 3 percent (weight ratio), the temperature of hot air is 300-350 ℃, the diameter of a centrifugal atomizing disk is 300mm, and the rotating speed is 5000 r/min or 8000 r/min or 10000 r/min. The equation for the chemical reaction of the materials is:
the equipment for preparing basic nickel carbonate by spray pyrolysis of ammonia complex liquid in the example is the same as that described in the example I, and different from the example I, the centrifugal sprayer, the cyclone separator and the like in the example I can select or design equipment with different sizes according to factors such as the amount of production or the like or according to the technical contents described in the example I. The rest of the description is not repeated, which is identical to that in the first and second examples.
Claims (4)
1. A method for preparing basic carbonate nano particles by ammonia complex liquid spray pyrolysis is characterized in that the ammonia complex liquid and dry hot air with certain temperature react, dry, separate and recover in special complete equipment for spray pyrolysis to prepare the basic carbonate nano particles by adopting a practical process operation technology, wherein the ammonia complex liquid comprises zinc ammonia complex liquid, copper ammonia complex liquid, nickel ammonia complex liquid and metal ammonia complex liquid which can carry out complex reaction with ammonia or can carry out complex reaction with ammonia through certain treatment, and the method is characterized in that:
a. preparing materials and feeding: sufficiently preparing ammonia complex solution after impurity removal and purification and hot air materials for later use; introducing the ammonia complex liquid for later use into a centrifugal spray dryer from a feed inlet, wherein the process operation conditions are as follows: the temperature is 30-50 ℃ under normal pressure, and the content of the metal ions in the ammonia complexing liquid is 3-20% (weight ratio); meanwhile, introducing standby hot air into the centrifugal spray dryer from another feeding hole, wherein the process operating conditions are as follows: the temperature of the hot air is 250 ℃ and 400 ℃, and the feeding amount is proper according to the feeding amount of the ammonia complex liquid;
b. atomizing and reacting: the ammonia complex liquid entering the centrifugal spray dryer from the two material ports and the hot air are fed into a centrifugal atomizing disk rotating at a high speed along a feeding guide pipe to be mixed, and then are atomized at a high speed along a tangent line according to a certain linear speed, and are sprayed into a cylinder of the dryer to react and dry, and then the materials enter a cyclone separator, and the process operation conditions are as follows: the rotating speed of the centrifugal atomizing disk is 5000-;
c. separating and taking out: the mixed material entering the cyclone separator along the tangent line is settled along the cylinder cyclone of the separator, the separated dry powder basic carbonate nano particles are taken out from the outlet at the bottom end of the separator, and the separated gas NH3、CO2And H2And O (water vapor) is discharged from an exhaust pipe at the top of the cyclone separator for recycling.
2. The method for preparing basic carbonate nanoparticles by spray pyrolysis of ammonia complex solution according to claim 1, characterized in that:
a. the preferred rotating speed of the atomizing disc is as follows: according to the different diameters of the atomizing disks, the rotating speed of the sprayed droplets at 1-5 mu m is taken as the preferred rotating speed;
b. the content of the complexing metal ions in the feed ammonia complexing liquid is not more than 20 percent (weight ratio);
c. the feed proportioning is as follows: the feeding proportion of the ammonia complex liquid and the hot air is different according to the diameter of the dryer, and the proportion is preferably that the mixture at the outlet of the lower end of the spray dryer is completely gasified without liquid drops;
d. gas recovery: a special complete equipment or a device for recovering the addable raw materials, namely a pulse cloth bag catcher, wherein a gas outlet at the upper end of a cyclone separator is connected to a feeding pipe of the pulse cloth bag catcher, a suction fan is used for sucking air by a cloth bag to recover partial basic carbonate nano particles escaping from the cyclone separator, and a separated gas substance NH3、CO2Water vapor (H)2And O), collecting from the catcher, entering a condensation spraying device, and recycling for production.
3. The equipment for preparing the basic carbonate nano particles by the spray pyrolysis of the ammonia complex liquid is special complete equipment for preparing the basic carbonate nano particles by using the ammonia complex liquid and dry hot air according to an applicable process operation method, and is characterized in that: the special equipment is formed by combining a centrifugal spray dryer and a cyclone separator in a set:
a. the centrifugal spray dryer undertakes the processes of feeding, mixing, reacting and drying, and the feeding conditions of the ammonia complex liquid are as follows: under normal pressure, the liquid temperature is 30-50 ℃, the ammonia solution enters a spray dryer from an ammonia solution feeding port, the content of the complexing metal in the ammonia complexing solution is 3-20% (weight ratio), and the feeding conditions of the dry hot air are as follows: at the temperature of 250-;
b. the cyclone separator completes the subsequent process of separating the basic carbonate nano particles from the gas, and the process conditions are as follows: naturally cooling and separating under micro-negative pressure, taking out the basic carbonate nanoparticles from the outlet at the lower part of the separator, and reacting to generate gas NH3、CO2And is discharged from an outlet at the top of the separator for recycling.
4. The apparatus for preparing basic carbonate nanoparticles by spray pyrolysis of ammonia complex solution according to claim 3, wherein:
a. rotating speed of the atomizing disc: according to the different diameters of the atomizing disk, the rotating speed of the sprayed droplets at 1-5 mu m is taken as the preferred rotating speed;
b. the content of the complex metal ions in the feed ammonia complex liquid is not more than 20 percent (weight ratio);
c. the proportion of the hot air feeding amount and the ammonia complex liquid is preferably that the mixture at the outlet of the lower end of the spray dryer is completely gasified without liquid drops according to different diameters of the dryer;
d. diameter of the dryer: the diameter can be 500mm-5000mm according to the rotating speed and the production capacity of the atomizing disk;
e. the complete equipment can also be added with a bag catcher and a gas recovery device.
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| CNB011413921A CN1170774C (en) | 2001-10-26 | 2001-10-26 | Method and equipment for preparing basic carbonate nano particle by means of spray pyrolysis of ammonia complex liquor |
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| CN106395882A (en) * | 2016-12-06 | 2017-02-15 | 杜宗鑫 | Device and process using ammonia method to produce metal compounds |
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