JP7289584B1 - Large-capacity ultra-atomized spray-drying apparatus and large-capacity ultra-atomized spray-drying method - Google Patents

Abstract

A large-capacity ultra-atomizing spray drying apparatus capable of producing ultra-fine particles having an average particle diameter of 0.1 to 10 μm in a large capacity of 1,000 kg/hour or more is provided. A plurality of four-fluid type nozzles 10 for spraying ultra-atomized liquid droplets, and a hot air dispersion chamber 20 having a hot air flow path for drying the liquid droplets and an ejection port for ejecting the hot air. , a hot air pipe 40 for supplying hot air connected to the hot air dispersion chamber 20, and a plurality of nozzles 10 are arranged above, and the droplets sprayed from the nozzles 10 are dried to form Sauter mean particles. A droplet drying chamber 30 having a space for powder fine particles with a diameter of 0.1 to 10 μm is provided, a plurality of nozzles 10 are arranged in a row, and a hot air dispersion chamber 20 is installed for each nozzle 10. A large-capacity ultra-atomizing spray-drying apparatus 100 having a throughput of 1,000 to 40,000 kg/hour of raw material liquid to be droplets. [Selection drawing] Fig. 1

Description

TECHNICAL FIELD The present invention relates to a large-capacity ultra-atomized spray-drying apparatus and a large-capacity ultra-atomized spray-drying method. More particularly, it relates to a large-capacity ultra-atomized spray drying apparatus and a large-capacity ultra-atomized spray drying method capable of producing ultrafine particles in a large capacity of 1,000 kg/hour or more.

Ultrafine particles with an average particle size of about 0.1 to 10 μm are used in cathode and anode materials for secondary batteries such as electric vehicles and chemical product materials such as cosmetics in order to demonstrate their functions. there is

Recently, with the expansion of the market for secondary batteries such as electric vehicles and the market for chemical products such as cosmetics, the demand for ultrafine particles as described above is further increasing.

Here, a plurality of spray dryers for producing ultrafine particles having an average particle diameter of 0.1 to 10 μm are known (see, for example, Patent Documents 1 to 3). Further, as an atomization nozzle capable of producing ultrafine particles having an average particle diameter of 0.1 to 10 μm as in Patent Documents 1 to 3, a plurality of atomization nozzles of a four-fluid type nozzle system that blows atomization air are known. ing. In addition, at present, a device (spray drying device) that produces the above ultrafine particles using the atomization nozzle of the above four-fluid nozzle system with a spray amount (processing amount of raw material liquid) of less than 1,000 kg / hour is Okawara Kako. It is developed and sold by machine companies.

Patent Document 4 describes a two-stage drying type spray dryer device using a raw material liquid pressure spray nozzle, and this device is capable of increasing the capacity (1,000 to 12,000 kg/hour). Are listed.

JP-A-8-281155 JP-A-2003-117442 Japanese Patent Application Laid-Open No. 2006-068660 JP-A-10-26471

However, although Patent Document 1 describes obtaining droplets of fine particles with a particle diameter of 10 μm or less using a four-fluid nozzle, 1000 g of liquid is jetted per minute (i.e., throughput of 60 kg/hour). and the throughput is not sufficient.

Patent Document 2 describes that fine particles having an average particle diameter of 5 to 15 μm or less can be obtained by a four-fluid type nozzle. It also states that the liquid is supplied at a rate of 2 liters/minute (that is, the amount of liquid to be sprayed is 12 kg/hour), and that the maximum liquid amount to be sprayed is 100 kg/hour or more. This four-fluid type nozzle was developed for a processing amount of 50 kg/hour to 1000 kg/hour, and even in Patent Document 2, the liquid processing amount is not sufficient.

In Patent Document 3, a two-fluid nozzle having two channels with circular cross sections is used, and the thin film flows jetted from the two-fluid nozzle collide with each other at the center (external collision point) to form four fluids ( This is a special two-fluid nozzle, and although it is a two-fluid nozzle, it can also be called a "four-fluid nozzle"). It is described that fine particles having an average particle diameter of 5 to 15 μm or less (for example, 5 μm or less) can be obtained by doing so, and that the processing amount is 10 kg/hour. This four-fluid type nozzle was developed for a processing amount of 1 to 50 kg/hour, and the liquid processing amount is not sufficient in Patent Document 3 as well. The two-fluid nozzle has one gas channel and one liquid channel. It is a nozzle that sprays droplets in a shape.

In Patent Document 4, the raw material liquid pressure spray nozzle described atomizes the raw material liquid only by the pressure of the pump and injects it from the orifice (7th line of paragraph [0009], claims 1, 4, See paragraphs [0001] to [0008]). Such a raw material liquid pressure spray nozzle can form particles with an average particle size of 30 to 100 μm (for example, particles for food applications), but cannot produce ultrafine particles with an average particle size of 0.1 to 10 μm. . This is also described in Patent Documents 1 to 3 (Patent Document 1 (paragraphs [0001] to [0008] (especially see paragraph [0006]), Patent Document 2 (paragraphs [0002] to [0013 ] (see paragraphs [0002] and [0009] in particular), Patent Document 3 (paragraphs [0002] to [0017] (see paragraphs [0002] and [0009] in particular)).

In addition, Patent Document 4 also describes a two-fluid nozzle (see paragraph [0007]), but since the two-fluid nozzle uses pressure air to atomize the raw material liquid, power is required compared to the pressure spray nozzle. It takes several times. Therefore, in the case of ultra-atomization applications, it is used only with a small stock solution throughput (1 to 30 kg/hour).

That is, at present, ultrafine particles having an average particle diameter of 0.1 to 10 μm cannot be produced without using the four-fluid type nozzle using air for atomization described in Patent Documents 1 to 3. In this specification, the nozzles described in Patent Documents 1 to 3 may be collectively referred to as four-fluid nozzles.

In addition, as an ultra-atomization spray drying device currently being developed and sold, a four-fluid system atomization device described in Patent Document 1 and Patent Document 2 is used, and a design water amount of 50 kg / hour or more is on sale. It is However, in this 4-fluid system atomization device, the maximum design water spray amount was 1,000 kg/hour, and the maximum actual spray amount was 860 kg/hour during actual operation. For this reason, even the ultra-atomized spray-drying equipment that has been developed and sold does not have a sufficient throughput of liquid. The reason for this is that it is difficult to develop and manufacture an ultra-atomizing nozzle for producing ultra-fine particles with an average particle diameter of 0.1 to 10 μm, because it is difficult to spray a liquid amount of 1,000 kg / hour or more. It is a thing.

Therefore, as described above, with the expansion of the market for secondary batteries such as electric vehicles and the chemical product market such as cosmetics, 1,000 kg of ultrafine particles with an average particle size of 0.1 to 10 μm used in these fields It has been desired to develop a large-capacity ultra-atomized spray-drying apparatus capable of producing a large amount of powder per hour or more (more specifically, 1,000 to 40,000 kg/hour).

The present invention has been made to solve the problems of the prior art as described above, and can produce ultrafine particles having an average particle size of 0.1 to 10 μm at a large capacity of 1,000 kg / hour or more. A large-capacity ultra-atomized spray-drying apparatus and a large-capacity ultra-atomized spray-drying method are provided.

The present invention provides the following large-capacity ultra-atomized spray-drying apparatus and large-capacity ultra-atomized spray-drying method.

[1] A plurality of four-fluid nozzles that spray ultra-atomized droplets;
a hot air dispersion chamber having a hot air flow path for drying the droplets and having an ejection port for ejecting the hot air;
a hot air pipe connected to the hot air distribution chamber for supplying the hot air;
Further, a droplet drying chamber having a space in which a plurality of the nozzles are arranged above and the droplets sprayed from the nozzles are dried to become powder particles having a Sauter mean particle diameter of 0.1 to 10 μm. cage,
A plurality of said nozzles are arranged in one row,
The hot air dispersion chamber is installed for each nozzle,
A large-capacity ultra-atomized spray drying apparatus, wherein the processing amount of the raw material liquid to be droplets is 1,000 to 40,000 kg/hour.

[2] The large-capacity ultra-atomized spray drying according to [1], wherein the droplet drying chamber is a rectangular parallelepiped, and the ratio of the vertical length to the horizontal length is 1:2 to 1:40. Device.

[3] The large-capacity ultra-atomized spray drying apparatus according to [2], wherein the plurality of nozzles are arranged in a row along the lateral direction of the droplet drying chamber.

[4] The large-capacity ultra-atomized spray drying apparatus according to any one of [1] to [3], comprising hot air pipes for sending the hot air to each of the hot air dispersion chambers.

[5] The large-capacity ultra-atomized spray drying apparatus according to any one of [1] to [3], wherein the number of nozzles is 3 or more.

[6] The large-capacity ultra-atomized spray drying apparatus according to [5], wherein the number of nozzles is 6 or more.

[7] The large-capacity ultra-atomization according to any one of [1] to [3], wherein the shape of the ejection port of the droplet drying chamber is an annular slit shape centering on the nozzle. Spray drying equipment.

[8] Any one of [1] to [3] above, wherein the droplet drying chamber is rectangular parallelepiped, and the vertical length of the droplet drying chamber is 2 to 20 times the outer diameter of the nozzle. The large-capacity type ultra-atomized spray drying apparatus according to 1.

[9] A large-capacity ultra-atomized spray-drying method using the large-capacity ultra-atomized spray-drying apparatus according to any one of [1] to [3] above,
a raw material liquid supply step of supplying a raw material liquid of droplets to be ultra-atomized to the plurality of nozzles;
The hot air is ejected from the ejection port of the hot air dispersion chamber, and the droplets are dried in the space in the droplet drying chamber to obtain fine powder particles having a Sauter mean particle diameter of 0.1 to 10 μm. a process;
A large-capacity ultra-atomized spray-drying method in which the raw material liquid is processed at a throughput of 1,000 to 40,000 kg/hour.

The large-capacity ultra-atomizing spray-drying apparatus of the present invention has the effect of being able to produce ultra-fine particles having an average particle size of 0.1 to 10 μm at a large capacity of 1,000 kg/hour or more.

According to the large-capacity type ultra-atomization spray-drying method of the present invention, it is possible to produce ultra-fine particles having an average particle size of 0.1 to 10 μm at a large capacity of 1,000 kg/hour or more. .

BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a side view schematically showing a see-through part of an embodiment of a large-capacity ultra-atomized spray drying apparatus of the present invention; BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a top view schematically showing one embodiment of the large-capacity ultra-atomized spray drying apparatus of the present invention; FIG. 2 is a plan view schematically showing a droplet drying chamber in one embodiment of the large-capacity ultra-atomized spray drying apparatus of the present invention, viewed from the hot air pipe side. FIG. 2 is a partially enlarged view schematically showing an enlarged view of the vicinity of a nozzle and a hot-air dispersion chamber in one embodiment of the large-capacity ultra-atomizing spray drying apparatus of the present invention, partially see-through.

BEST MODE FOR CARRYING OUT THE INVENTION Embodiments for carrying out the present invention will be described below, but the present invention is not limited to the following embodiments. In other words, it is understood that any modifications, improvements, etc., made to the following embodiments based on the ordinary knowledge of those skilled in the art without departing from the gist of the present invention also belong to the scope of the present invention. should.

(1) Large-capacity ultra-atomized spray drying device:
One embodiment of the large-capacity ultra-atomization spray drying apparatus of the present invention is a large-capacity ultra-atomization spray drying apparatus 100 shown in FIGS. The large-capacity ultra-atomization spray drying apparatus 100 shown in FIGS. A hot air distribution chamber 20 having a flow path 21 and an ejection port 23 for ejecting hot air, and a hot air pipe 40 connected to the hot air distribution chamber 20 for supplying hot air. Furthermore, a droplet drying chamber 30 having a space 31 in which a plurality of nozzles 10 are arranged above and the droplets sprayed from the nozzles 10 are dried and become powder particles with a Sauter mean particle diameter of 0.1 to 10 μm. I have. A plurality of nozzles 10 are arranged in one row, and a hot air dispersion chamber 20 is installed for each nozzle 10 . The large-capacity ultra-atomizing spray-drying apparatus 100 has a throughput of 1,000 to 40,000 kg/hour of raw material liquid to be droplets.

This large-capacity ultra-atomizing spray drying apparatus 100 includes a plurality of ultra-atomizing nozzles 10, a hot air dispersion chamber 20, a hot air pipe 40, and a droplet drying chamber 30, so that the Sauter average particle diameter of 0.1 to 10 μm powder ultrafine particles can be produced in a large volume of 1,000 kg/hour or more (more specifically, 1,000 to 40,000 kg/hour).

Here, although the throughput of the raw material liquid is less than 1,000 kg/hour in spray drying equipment currently on the market, it is possible to increase the throughput by simultaneously operating a plurality of units. That is, for example, if 10 spray drying apparatuses are prepared and operated simultaneously, a throughput of 10 times can be achieved. However, space for installing 10 spray drying apparatuses is required. In addition, when a plurality of devices are prepared, many control panels for these devices are required, and moreover, a large number of operators are required to operate the devices. It is also possible to increase the throughput by increasing the size of the ultra-atomization nozzle itself, but it is necessary to start development and design of such an ultra-atomization nozzle from the beginning. Also, a super atomization nozzle with a throughput of 1,000 kg/hour already weighs as much as 150 kg. Due to this situation, there is a limit to further enlargement of the nozzle from the viewpoint of handling and maintenance, and accordingly there is a limit to the processing amount that can be increased. For these reasons, a throughput of 1,000 kg/hour or more has not been achieved using ultra-atomizing nozzles.

Under such circumstances, by installing a plurality of ultra-atomizing nozzles 10 in one hot-air dispersion chamber 20 as in the present invention, ultra-fine particles can be obtained and the processing amount of the raw material liquid can be reduced to 1,000. 000 kg/hour or more. And by doing in this way, it is not necessary to secure the space, without preparing a plurality of spray-drying apparatuses. Also, the conventional ultra-atomizing nozzle 10 can be used as it is.

(1-1) Nozzle:
The nozzles 10 are four-fluid type nozzles that spray ultra-atomized droplets, and are arranged in plurality. Specifically, it is an ultra-atomizing nozzle capable of spraying ultra-atomized droplets for producing ultra-fine particles having an average particle diameter of 0.1 to 10 μm. That is, the large-capacity ultra-atomizing spray drying apparatus 100 is equipped with an ultra-atomizing nozzle capable of spraying droplets having an average particle size of 0.1 to 10 μm.

Here, a four-fluid type nozzle is a nozzle having two gas flow paths and two liquid flow paths, and the fluids jetted from the gas flow paths and the liquid flow paths intersect and collide with each other. is.

The nozzle 10 is not particularly limited as long as it is a four-fluid ultra-atomizing nozzle capable of spraying droplets as described above, and any conventionally known four-fluid ultra-atomizing nozzle can be appropriately employed. In the present invention, the four-fluid nozzle described above can be used.

As the nozzle 10, a nozzle capable of spraying the raw material liquid as droplets at 500 to 1,000 kg/hour can be used. A nozzle having such a spray processing capability has an outer diameter of about 10 to 50 cm.

The number of nozzles 10 is not particularly limited as long as a plurality (two or more) of nozzles 10 are provided, and can be set in consideration of the required processing amount of the raw material liquid. For example, it can be two or more, preferably three or more, and more preferably six or more. The upper limit of the number of nozzles is not particularly limited, but may be 80, preferably 60, and more preferably 40. Specifically, the number of nozzles can be set to 2 to 80 in this way.

When the droplet drying chamber 30 is a rectangular parallelepiped, the nozzles 10 are arranged in a row along the lateral direction of the droplet drying chamber 30 (longitudinal direction in the cross section orthogonal to the height direction of the droplet drying chamber 30). preferably. By arranging the plurality of nozzles 10 in this manner, it is possible to satisfactorily dry the droplets with hot air while avoiding collision with the droplets sprayed from the adjacent nozzles 10 . As a result, fine particles having smaller particle diameters can be produced more uniformly. In this case, it is preferable to install a hot air dispersion chamber 20 for each nozzle 10 .

When a plurality of nozzles 10 are arranged in a line as described above, the interval between adjacent nozzles 10 can be 1,000 to 4,000 mm, preferably 1,500 to 3,000 mm. , 1,500 to 2,500 mm. With such a range, it is possible to satisfactorily dry the droplets with the hot air from the hot-air dispersion chamber 20 while avoiding collision with the droplets sprayed from the adjacent nozzles 10 . As a result, fine particles having smaller particle diameters can be produced more uniformly.

The raw material liquid that forms droplets is not particularly limited, and a raw material liquid that can be used in conventionally known spray drying techniques can be appropriately employed. For example, positive electrode materials and negative electrodes for secondary batteries such as electric vehicles It is possible to adopt raw materials for materials, chemical products such as cosmetics, and the like.

(1-2) Hot air dispersion chamber:
The hot-air dispersion chamber 20 has a hot-air flow path 21 for drying the liquid droplets, and an ejection port 23 for ejecting the hot air. The droplets sprayed from the nozzle 10 are dried by the hot air jetted from the hot air dispersion chamber 20 . In addition, the hot air can form a flow of droplets, so that the hot air acts as a so-called air curtain, and problems such as colliding with the droplets sprayed from the adjacent nozzles 10 can be avoided.

The temperature of the hot air can be set appropriately, for example, 100 to 550°C.

The hot air dispersion chamber 20 is installed for each nozzle 10 as shown in FIG. By installing the hot air dispersion chamber 20 for each nozzle 10 in this way, the momentum of the hot air ejected from each hot air dispersion chamber 20 can be uniformly adjusted, and fine particles having a more uniform particle diameter can be produced. can do. In other words, since the hot air dispersion chamber 20 is installed for each nozzle 10 , it is possible to prevent the hot air from being unevenly distributed to the hot air dispersion chamber 20 . When the hot air is biased to the hot air dispersion chamber 20, the undried ultrafine particles easily collide with each other, and when they collide, the ultrafine particles stick to each other, resulting in particles with a Sauter average particle diameter of 10 to 20 μm (particle diameter large particles) are formed.

The shape of the jet port 23 of the hot air dispersion chamber 20 is not particularly limited, but as shown in FIG. The ejection port 23 having such a shape can satisfactorily heat the atomized liquid droplets sprayed from the ultra-atomizing nozzle. Furthermore, the flow of droplets can be formed satisfactorily, problems such as collision with droplets sprayed from adjacent nozzles 10 can be avoided, and powder particles with smaller particle diameters can be formed more uniformly. can be manufactured.

(1-3) Droplet drying chamber:
The droplet drying chamber 30 has a plurality of nozzles 10 arranged above, and one space ( internal space) 31. The droplets sprayed into the internal space 31 from the nozzle 10 are dried by the hot air ejected from the hot air dispersion chamber 20 while falling in this space 31, and are fine powder particles (Sauter average particle diameter is 0.1 to 10 μm). In the space 31 of the droplet drying chamber 30, the droplets sprayed from each of the adjacent nozzles 10 form a flow due to the hot air ejected from the hot air dispersion chamber 20, making it difficult for the droplets to collide with each other. It's becoming The internal space 31 of the droplet drying chamber 30 is one region without partition walls.

The shape of the droplet drying chamber 30 is not particularly limited, but it can be a rectangular parallelepiped. The ratio of the length in the hand direction) and the length in the lateral direction (length in the longitudinal direction) can be a rectangular parallelepiped with a ratio of 1:2 to 1:40, preferably a ratio of 1:2 to 1:30. , a ratio of 1:3 to 1:20 is more preferred. The space 31 of the rectangular parallelepiped droplet drying chamber 30 is also a rectangular parallelepiped.

When the droplet drying chamber 30 is a rectangular parallelepiped, the vertical length (the length in the lateral direction) of the droplet drying chamber 30 can be 3 to 20 times the outer diameter of the nozzle 10. It is preferably up to 15 times, more preferably 8 to 12 times. By setting the vertical length of the droplet drying chamber 30 with respect to the outer diameter of the nozzle 10 within the predetermined range, the droplets sprayed from the nozzle 10 are less likely to collide with the inner surface of the droplet drying chamber 30. In addition, the efficiency of drying with hot air is improved, and fine particles having smaller particle diameters can be produced more uniformly.

The droplet drying chamber 30 may be provided with one unit like the large-capacity ultra-atomized spray drying apparatus 100 shown in FIG. 2, or a plurality of units (specifically, 2 to 40 units). good too. In this manner, a plurality of droplet drying chambers 30 may be provided in consideration of the installation space. That is, for example, in the case of the rectangular parallelepiped liquid droplet drying chamber 30, since the horizontal width is long, an installation space corresponding to the long horizontal width is required. However, there are cases where sufficient installation space cannot be secured, and even in such cases, it is possible to arrange them according to the installation space by dividing them into a plurality of units.

(1-4) Hot air piping:
The hot air pipe 40 is connected to the hot air distribution chamber 20 to supply hot air. When the hot air distribution chamber 20 is installed for each nozzle 10, the hot air piping 40 can send hot air to each of the hot air distribution chambers 20 as shown in FIG. As shown in FIG. 3, it is connected to each of the hot air dispersion chambers 20 . The hot air pipes 40 must be installed for each of the hot air distribution chambers 20. If they are not installed in each of the hot air distribution chambers 20, the hot air blowing out from the hot air distribution chambers 20 will be uneven.

As shown in FIGS. 2 and 3, each hot air pipe 40 is branched from one hot air generating source (hot air generating furnace) and then connected to each of the hot air distribution chambers 20 . On the other hand, each hot-air pipe 40 may connect a plurality of hot-air generating sources corresponding to each hot-air pipe 40 and the hot-air dispersion chamber 20 .

(1-5) Other components:
The large-capacity ultra-atomization spray-drying apparatus 100 can be provided with other components in addition to the plurality of nozzles 10 , the hot-air dispersion chamber 20 , and the droplet drying chamber 30 .

Specifically, the large-capacity ultra-atomized spray drying apparatus 100 shown in FIG. and a blower 53 for Furthermore, as shown in FIGS. 1 and 2, this large-capacity ultra-atomized spray drying apparatus 100 includes two dust collectors 55 for collecting powder particles obtained in the droplet drying chamber 30, and these dust collectors 55 and an exhaust fan 57 connected to each of the dust collectors 55 for exhausting air. Furthermore, the large-capacity ultra-atomizing spray drying apparatus 100 includes a raw material liquid tank (not shown) connected to each nozzle 10 and storing a raw material liquid serving as a raw material for droplets.

These other components (the hot air generator 51, the blower 53, the dust collector 55, the exhaust fan 57, and the raw material liquid tank) can be appropriately selected and adopted from conventionally known ones.

(2) Large-capacity ultra-atomized spray drying method:
The large-capacity ultra-atomized spray-drying method of the present invention is a large-capacity ultra-atomized spray-drying method using the large-capacity ultra-atomized spray-drying apparatus of the present invention. /hour (that is, a large volume) to obtain fine powder particles having a Sauter mean particle size of 0.1 to 10 μm. The method of the present invention has a raw material liquid supply step and a droplet drying step.

According to this large-capacity type ultra-atomization spray drying method, since the large-capacity type ultra-atomization spray drying apparatus of the present invention is used, ultra-fine particles having an average particle size of 0.1 to 10 μm are produced at a rate of 1,000 kg/hour or more. Can be manufactured in volume.

(2-1) Raw material liquid supply step:
The source liquid supply step is a step of supplying the source liquid of droplets to be ultra-atomized to the nozzle 10 . In this step, when the raw material liquid stored in the raw material liquid tank of the large-capacity ultra-atomized spray drying apparatus 100 is supplied to each nozzle 10, the raw material liquid sprayed from these nozzles 10 is ultra-atomized droplets becomes.

For the plurality of nozzles 10, the same nozzles as those used in the above-described large-capacity ultra-atomized spray drying apparatus of the present invention can be adopted. Ultra-atomized liquid droplets (average particle diameter of 0.1 to 10 μm) can be obtained by these nozzles 10 .

The raw material liquid is not particularly limited, and a raw material liquid that can be used in a conventionally known spray drying technique can be appropriately employed. Chemical product materials such as cosmetics can be used.

(2-2) Droplet drying step:
In the droplet drying process, hot air is ejected from the ejection port 23 of the hot air dispersion chamber 20, and the droplets are dried in the space 31 in the droplet drying chamber 30 to obtain powder particles having a Sauter average particle diameter of 0.1 to 10 μm. It is a process to

The hot air dispersion chamber 20 can employ the same one as that used in the above-described large-capacity ultra-atomized spray drying apparatus of the present invention.

Conventionally known methods can be suitably adopted for the temperature and ejection conditions of the hot air. For example, the temperature of the hot air can be 100 to 500°C.

(2-3) Other steps:
In the large-volume ultra-atomized spray-drying method of the present invention, other processes can be employed in addition to the raw material liquid supply process and the liquid droplet drying process. As another process, a dust collection process can be adopted in which the powder particles obtained in the droplet drying process are collected by a dust collector 55 connected to the droplet drying chamber 30 .

EXAMPLES The present invention will be specifically described below based on Examples and Comparative Examples, but the present invention is not limited to these Examples and Comparative Examples.

(Example 1)
A drying system 1 was prepared by fabricating a large-capacity ultra-atomized spray drying apparatus as shown in FIG. Ten TJ1000 type ultra-atomizing nozzles (manufactured by Okawara Kakoki Co., Ltd.), which are 4-fluid type nozzles, were prepared as nozzles. 0m, height 10.0m) were installed in a row in the horizontal direction. Then, the drying system 1 was operated under the following conditions. The ultrafine particles (powder particles) obtained in this drying system 1 had a product average particle size (Sauter average particle size) of 7.8 μm.
Raw material liquid name: Lithium-based secondary battery positive electrode raw material liquid Raw material liquid amount: 10,005 kg/hour Moisture evaporation amount: 5,005 kg/hour Dry product amount: 5,000 kg/hour Gas amount required for drying: 170,700 m ³ /hr (200°C)
Required power: Total 390kW

A hot-air dispersion chamber was installed for each nozzle, and hot-air pipes were provided to send hot air to each of the hot-air dispersion chambers. The shape of the hot-air dispersion chamber was an annular slit with the nozzle at the center.

In this drying system 1, as described above, the powder fine particles satisfy the Sauter mean particle diameter of 0.1 to 10 μm, and the processing amount of the raw material liquid satisfies 1,000 to 40,000 kg / hour. .

(Example 2)
A drying system 2 was prepared by fabricating a large-capacity ultra-atomized spray drying apparatus as shown in FIG. Two rectangular parallelepiped droplet drying chambers (depth (length) 4.0 m, width 22.0 m, height 10.0 m) were prepared, and each droplet drying chamber was equipped with a 4-fluid type nozzle TJ1000 or more. Ten atomization nozzles (manufactured by Okawara Kakoki Co., Ltd.) were installed. These nozzles were installed in a row across each droplet drying chamber. The total number of nozzles used is 20. Then, the drying system 2 was operated under the following conditions. The ultrafine particles (powder particles) obtained in this drying system 2 had a product average particle size (Sauter average particle size) of 7.7 μm.
Raw material liquid name: Lithium secondary battery positive electrode raw material liquid Raw material liquid amount: 20,020 kg/hour Moisture evaporation amount: 10,020 kg/hour Dry product amount: 10,000 kg/hour Gas amount required for drying: 341,000 m ³ /hr (200°C)
Required power: Total 780kW

A hot-air dispersion chamber was installed for each nozzle, and hot-air pipes were provided to send hot air to each of the hot-air dispersion chambers. The shape of the hot-air dispersion chamber was an annular slit with the nozzle at the center.

In this drying system 2, as described above, the powder fine particles satisfy the Sauter mean particle diameter of 0.1 to 10 μm, and the processing amount of the raw material liquid satisfies 1,000 to 40,000 kg / hour. .

(Example 3)
A large-capacity ultra-atomized spray drying apparatus as shown in FIG. Two rectangular parallelepiped droplet drying chambers (depth (vertical) 4.0 m, width 42.0 m, height 10.0 m) were prepared, and each droplet drying chamber was equipped with a 4-fluid nozzle TJ1000 type or more. Twenty atomization nozzles (manufactured by Okawara Kakoki Co., Ltd.) were installed. These nozzles were installed in a row across each droplet drying chamber. The total number of nozzles used is 40. Then, the drying system 3 was operated under the following conditions. The ultrafine particles (powder particles) obtained in this drying system 3 had a product average particle size (Sauter average particle size) of 7.7 μm.
Raw material liquid name: Lithium-based secondary battery positive electrode raw material liquid Raw material liquid amount: 40,000 kg/hour Moisture evaporation amount: 20,000 kg/hour Dry product amount: 20,000 kg/hour Gas amount required for drying: 682,000 m ³ /hr (200°C)
Required power: Total 1560kW

A hot-air dispersion chamber was installed for each nozzle, and hot-air pipes were provided to send hot air to each of the hot-air dispersion chambers. The shape of the hot-air dispersion chamber was an annular slit with the nozzle at the center.

In this drying system 3, as described above, the powder fine particles satisfy the Sauter mean particle diameter of 0.1 to 10 μm, and the processing amount of the raw material liquid satisfies 1,000 to 40,000 kg / hour. .

(Comparative example 1)
A drying system 5 was prepared by fabricating a large-capacity ultra-atomized spray drying apparatus. A rectangular parallelepiped droplet drying chamber (depth (length) 4.0 m, width 22.0 m, height 10.0 m) was prepared, and each droplet drying chamber was equipped with a 4-fluid type nozzle TJ1000 or more. Ten atomization nozzles (manufactured by Okawara Kakoki Co., Ltd.) were installed. These nozzles were arranged in a row across each droplet drying chamber. The total number of nozzles used is ten. In Comparative Example 1, one hot air distribution chamber was installed for ten nozzles, and one hot air pipe for sending hot air was connected to the hot air distribution chamber. Then, the drying system 4 was operated under the following conditions. The ultrafine particles (powder particles) obtained in this drying system 4 had a product average particle size (Sauter average particle size) of 11 μm. In addition, uneven hot air generated undried deposits, and continuous operation was possible only for 3 days in this comparative example 1, although normal continuous operation was 30 days.
Raw material liquid name: Lithium-based secondary battery positive electrode raw material liquid Raw material liquid amount: 10,003 kg/hour Moisture evaporation amount: 5,003 kg/hour Dry product amount: 5,000 kg/hour Gas amount required for drying: 170,695 m ³ /hr (200°C)
Required power: Total 390kW

In addition, the shape of the ejection port of the hot air dispersion chamber was an annular slit shape arranged at the center of the nozzle.

In the large-capacity ultra-atomizing spray drying apparatus of Comparative Example 1, one hot air dispersion chamber is installed for a plurality of nozzles, so that the average particle diameter of the obtained fine particles is more than 10 μm (11 μm). rice field. Furthermore, as described above, the result was that a sufficient continuous operation period could not be obtained.

As described above, according to the large-capacity ultra-atomization spray drying apparatus and the large-capacity ultra-atomization spray drying method of Examples 1 to 3, 1,000 kg / hour of ultrafine particles having an average particle diameter of 0.1 to 10 μm It can be seen that it is possible to manufacture in a large capacity as described above.

The large-capacity ultra-atomized spray drying apparatus of the present invention can be used as a spray drying apparatus for producing ultra-fine particles used in secondary batteries for electric vehicles and chemical products such as cosmetics. The large-capacity ultra-atomized spray-drying method of the present invention can be employed as a spray-drying method for producing ultra-fine particles used in secondary batteries for electric vehicles and chemical products such as cosmetics.

10: nozzle, 20: hot air dispersion chamber, 21: flow path, 23: spout, 30: droplet drying chamber, 31: space (internal space), 40: hot air pipe, 51: hot air generator, 53: blower, 55: Dust collector 57: Exhaust fan, 100: Large-capacity ultra-atomized spray drying device.

Claims (9)

a plurality of four-fluid nozzles for spraying ultra-atomized droplets;
a hot air dispersion chamber having a hot air flow path for drying the droplets and having an ejection port for ejecting the hot air;
a hot air pipe connected to the hot air distribution chamber for supplying the hot air;
Further, a droplet drying chamber having a space in which a plurality of the nozzles are arranged above and the droplets sprayed from the nozzles are dried and turned into powder particles having a Sauter mean particle diameter of 0.1 to 10 μm. cage,
A plurality of said nozzles are arranged in one row,
The hot air dispersion chamber is installed for each nozzle,
A large-capacity ultra-atomized spray drying apparatus, wherein the processing amount of the raw material liquid to be droplets is 1,000 to 40,000 kg/hour. 2. The large-capacity ultra-atomized spray drying apparatus according to claim 1, wherein the droplet drying chamber is rectangular parallelepiped and has a length to width ratio of 1:2 to 1:40. 3. The large-capacity ultra-atomized spray drying apparatus according to claim 2, wherein a plurality of said nozzles are arranged in a row along the lateral direction of said droplet drying chamber. The large-capacity ultra-atomized spray drying apparatus according to any one of claims 1 to 3, comprising hot air pipes for sending the hot air to each of the hot air dispersion chambers. The large-capacity ultra-atomized spray drying apparatus according to any one of claims 1 to 3, wherein the number of nozzles is 3 or more. 6. The large-capacity ultra-atomized spray drying apparatus according to claim 5, wherein the number of nozzles is 6 or more. The large-capacity ultra-atomized spray drying apparatus according to any one of claims 1 to 3, wherein the shape of the ejection port of the droplet drying chamber is an annular slit-like shape centered on the nozzle. The droplet drying chamber according to any one of claims 1 to 3, wherein the droplet drying chamber has a rectangular parallelepiped shape, and the vertical length of the droplet drying chamber is 2 to 20 times the outer diameter of the nozzle. Volumetric ultra-atomized spray drying equipment. A large-capacity ultra-atomized spray drying method using the large-capacity ultra-atomized spray drying apparatus according to any one of claims 1 to 3,
a raw material liquid supply step of supplying a raw material liquid of droplets to be ultra-atomized to the plurality of nozzles;
The hot air is ejected from the ejection port of the hot air dispersion chamber, and the droplets are dried in the space in the droplet drying chamber to obtain fine powder particles having a Sauter mean particle diameter of 0.1 to 10 μm. a process;
A large-capacity ultra-atomized spray-drying method in which the raw material liquid is processed at a throughput of 1,000 to 40,000 kg/hour.

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