CN113226529A

CN113226529A - Batch reactor

Info

Publication number: CN113226529A
Application number: CN201980083638.7A
Authority: CN
Inventors: 李惠媛; 柳贤澈; 韩基道
Original assignee: Han Huasiluxin Zhu
Current assignee: Han Huasiluxin Zhu; Hanwha Solutions Corp
Priority date: 2018-12-21
Filing date: 2019-12-16
Publication date: 2021-08-06
Also published as: KR20200078221A; JP2022514854A; WO2020130539A1

Abstract

A batch reactor according to an embodiment of the present disclosure includes: a cylindrical reactor body including a side wall portion, a bottom portion, and a lid portion; one or more supply nozzles for supplying the raw material; one or more impellers; and a rotating shaft connected to the impellers and extending in a height direction, wherein the supply nozzle includes a connection pipe extending from a side wall portion toward an inside of the cylindrical reactor body, and an injection port located at one end of the connection pipe and configured to inject the raw material, and wherein a height from the bottom portion to the injection port is equal to or less than a height from the bottom portion to an impeller located at a lowermost end among the one or more impellers.

Description

Batch reactor

Technical Field

Cross Reference to Related Applications

The present application claims the benefit of korean patent application No. 10-2018-0167914, which was filed on 21.12.2018 with the korean intellectual property office, the disclosure of which is incorporated herein by reference in its entirety.

The present disclosure relates to a batch reactor, and more particularly, to a batch reactor equipped with an impeller.

Background

Among the isocyanates used as starting materials for polythiourethanes, xylylene diisocyanate is generally prepared from xylylenediamine by using phosgene (COCl)₂) Or non-phosgene processes, and are commercially effectively utilized in a very wide range of fields.

In the process for preparing xylene diisocyanate, the process using phosgene includes carrying out a phosgenation reaction, and for this purpose, a batch reactor equipped with an impeller may be used.

A typical batch reactor comprises: a reactor body comprising reactants; an impeller installed inside the reactor main body to stir the reactant; and a drive motor that rotates the impeller.

Generally, for a batch reaction process, it is important to produce a uniform product, improve productivity, and improve stability of product quality.

In particular, in a reaction system between gas and liquid such as a phosgenation reaction, since a supply nozzle supplying a raw material or refluxing to the inside of a batch reactor affects the effective supply of the raw material and the uniformity of a reaction region, it plays a very important role in improving the productivity and stability of the batch reactor.

Therefore, studies have been made to improve the reaction rate in the batch reactor by adjusting the type, position, angle, and the like of the supply nozzle.

Disclosure of Invention

[ problem ] to provide a method for producing a semiconductor device

Embodiments of the present disclosure are designed to solve the above-mentioned problems, and it is an object of the present disclosure to provide a batch reactor having an improved reaction rate by increasing gas retention in the batch reactor.

[ technical solution ] A

According to an embodiment of the present disclosure, there is provided a batch reactor including: a cylindrical reactor body including a side wall portion, a bottom portion, and a lid portion; one or more supply nozzles for supplying the raw material; one or more impellers; and a rotating shaft connected to the impellers and extending in a height direction, wherein the supply nozzle includes a connection pipe extending from a side wall portion toward an inside of the cylindrical reactor body, and an injection port located at one end of the connection pipe and configured to inject the raw material, and wherein a height from the bottom portion to the injection port is equal to or less than a height from the bottom portion to an impeller located at a lowermost end among the one or more impellers.

The connection pipe may be inclined such that the injection inlet is positioned lower than a portion of the connection pipe connected to the sidewall part.

The connection pipe may form an angle of 10 to 45 degrees with a width direction perpendicular to the rotation axis.

The supply nozzle may include a first supply nozzle and a second supply nozzle positioned spaced apart from each other about the axis of rotation.

The height from the bottom portion to the injection port of the first supply nozzle and the injection port of the second supply nozzle may be equal to the height from the bottom portion to the impeller located at the lowermost end, and the distance between the injection port of the first supply nozzle and the injection port of the second supply nozzle may be greater than the rotation diameter of the impeller located at the lowermost end.

The height from the bottom portion to the injection port of the first supply nozzle and the injection port of the second supply nozzle may be lower than the height from the bottom portion to the impeller located at the lowermost end, and the distance between the injection port of the first supply nozzle and the injection port of the second supply nozzle may be smaller than the rotation diameter of the impeller located at the lowermost end.

The connection pipe may be a pipe-shaped pipe, and the injection port may include a plurality of holes for injecting the raw material.

The impeller may include at least one of a radial type impeller and an axial type impeller.

The lowermost impeller may be a radial type impeller.

The liquid solvent may be contained in the cylindrical reactor body, and the feedstock may comprise a gaseous material.

The feedstock may comprise phosgene.

[ PROBLEMS ] the present invention

According to the embodiments of the present disclosure, it is possible to provide a batch reactor capable of increasing a reaction rate by optimizing the position and angle of a supply nozzle that supplies a raw material into the reactor.

Drawings

Fig. 1 is a schematic illustration of a batch reactor according to one embodiment of the present disclosure.

Fig. 2 is a schematic illustration of a batch reactor according to another embodiment of the present disclosure.

FIG. 3 is a schematic illustration of a batch reactor according to a comparative example.

Detailed Description

Hereinafter, various embodiments of the present disclosure will be described in detail with reference to the accompanying drawings so that those skilled in the art can easily implement them. The present disclosure may be modified in various different ways and is not limited to the embodiments set forth herein.

Portions irrelevant to the description will be omitted to clearly describe the present disclosure, and like reference numerals denote like elements throughout the specification.

Further, in the drawings, the size and thickness of each element are arbitrarily shown for convenience of description, and the present disclosure is not limited to those shown in the drawings. The thickness of layers, regions, etc. are exaggerated in the figures for clarity. For convenience of description, the thicknesses of some layers and regions in the drawings are exaggerated.

In addition, it will be understood that when an element such as a layer, film, region, or panel is referred to as being "on" or "over" another element, it can be directly on the other element or intervening elements may also be present. In contrast, when an element is referred to as being "directly on" another element, it is intended that no intervening elements are present. Furthermore, the words "on.

Further, throughout the specification, when a part is referred to as "including" a certain component, it means that it may further include other components without excluding other components, unless otherwise specified.

In addition, throughout the specification, when referring to "plane", it means that the target site is observed from above; when referring to a "cross section", it means that the target site is observed from the side of the cross section cut perpendicularly.

Referring to fig. 1, a batch reactor 100 according to an embodiment of the present disclosure includes: a cylindrical reactor body 120, one or

more supply nozzles

140 and 150 for supplying a raw material 160, one or

more impellers

131, 132, and 133, and a rotary shaft 130 connected to the

impellers

131, 132, and 133 and extending in a height direction (Y direction).

Further, the cylindrical reactor body 120 includes a side wall portion 121, a bottom portion 122, and a lid portion 123.

Further, the

supply nozzles

140 and 150 include

connection pipes

141 and 151 extending from the side wall part 121 to the inside of the cylindrical reactor body 120, and

injection ports

142 and 152 located at one ends of the

connection pipes

141 and 151 and configured to inject the raw material 160.

The

connection pipes

141 and 151 are pipe-shaped pipes, and the

injection ports

142 and 152 may be in the form of openings for discharging the raw material 160 or may be in the form of a plurality of holes included to easily inject the gaseous raw material 160. This is configured as follows: the raw material 160 moves through the pipe-

shaped connection pipes

141 and 151 and is injected through a plurality of holes formed in the

injection ports

142 and 152, so that the injection position of the raw material 160 can be freely adjusted inside the cylindrical reactor body 120.

In addition,

multiple orifices

142 and 152 in the form of multiple orifices may be provided to introduce, for example, phosgene (COCl)₂) The gaseous raw material 160 is uniformly supplied into the solvent.

In fig. 1, two

supply nozzles

140 and 150 are shown, but may consist of one nozzle, or of more than two nozzles, if desired. However, in the batch reactor 100, it is important to produce a uniform product in each zone, and for this purpose, it is important to uniformly supply the raw material 160 to the entire batch reactor 100. Accordingly, it is preferable that the

supply nozzles

140 and 150 include a first supply nozzle 140 and a second supply nozzle 150 which are positioned spaced apart from each other around the rotation shaft 130.

On the other hand, the height H2 from the bottom portion 122 to the

injection ports

142 and 152 is equal to or smaller than the height (H1) from the bottom portion 122 to the impeller 131 located at the lowermost end among the one or

more impellers

131, 132, and 133.

Specifically, as shown in fig. 1, a height H2 from the bottom portion 122 to the

injection ports

142 and 152 may be equal to a height H1 from the bottom portion 122 to the impeller 131 located at the lowermost end, and a distance (D2) between the injection port 142 of the first supply nozzle 140 and the injection port 152 of the second supply nozzle 150 may be larger than a rotation diameter D1 of the impeller 131 located at the lowermost end.

Therefore, since the

injection ports

142 and 152 of the

supply nozzles

140 and 150 are located in the region adjacent to the impeller 131 located at the lowermost end, the raw material 160 is injected into the region greatly affected by the rotational flow rotated by the impeller. This results in increased gas hold-up, which can increase the reaction rate in the reactor. In conclusion, it is possible to provide a batch reactor 100 capable of producing a uniform product in a shorter time, improving productivity and improving stability of product quality.

In particular, in order to produce xylene diisocyanate, phosgene must be fed as a raw material into the reactor, and when a gaseous material having a low density, such as phosgene, is fed, it is preferably fed into an area adjacent to the impeller 131 located at the lowermost end among the

impellers

131, 132 and 133. Since a material such as phosgene floats in the liquid solvent 110, it must be supplied from the lower end portion of the cylindrical reactor body 120, and thus, it can be efficiently supplied to the entire batch reactor 100, and the polymerization reaction of the reactants can be uniformly maintained in each region. Therefore, it is preferable that the

injection ports

142 and 152 of the

supply nozzles

140 and 150 are positioned in a region adjacent to the impeller 131 positioned at the lowermost end among the one or

more impellers

131, 132, and 133.

Referring again to fig. 1, the

connection pipes

141 and 151 may have an inclined shape such that the

injection ports

142 and 152 are positioned lower than portions of the

connection pipes

141 and 151 connected to the side wall part 121.

In addition, the

connection pipes

141 and 151 may be inclined to form an angle of 10 to 45 degrees with a width direction (X direction) perpendicular to the rotation shaft 130. The

connection pipes

141 and 151 are generally installed at a fixed height or above the fixed height in the cylindrical reactor body 120. At this time, the

injection ports

142 and 152 may be located at the lower end of the cylindrical reactor body 120 by angling the

connection pipes

141 and 151, and also a distance between the

injection ports

142 and 152 may be closely maintained. This makes it possible to increase the possibility that the gaseous raw material 160 stays at the lower end of the reactor 100 for a long time and comes into contact with the solvent 110, and to prevent the gaseous raw material 160 from floating up or flowing out at the upper end of the reactor 100.

Referring to fig. 2, a batch reactor 200 according to another embodiment of the present disclosure has the same or similar configuration as the batch reactor 100 of fig. 1 except for the injection positions of the

supply nozzles

240 and 250. That is, the batch reactor 200 includes a cylindrical reactor body 220, the cylindrical reactor body 220 including a sidewall portion 221, a bottom portion 222, and a lid portion 223, one or

more impellers

231, 232, and 233, and a rotary shaft 230 connected to the

impellers

231, 232, and 233 and extending in the height direction (Y direction). The solvent 210 is contained inside a cylindrical reactor body 220.

The first and

second supply nozzles

240 and 250, which are positioned apart from each other about the rotational axis 230, further include

connection pipes

241 and 251 and

injection ports

242 and 252, respectively, but the injection positions are different from the

supply nozzles

140 and 150 of fig. 1.

The height H4 from the bottom portion 222 to the injection holes 242 of the first supply nozzle 240 and the injection holes 252 of the second supply nozzle 250 is lower than the height H3 from the bottom portion 222 to the impeller 231 located at the lowermost end.

Further, a distance D4 between the injection holes 242 of the first supply nozzle 240 and the injection holes 252 of the second supply nozzle 250 may be smaller than a rotation diameter D3 of the impeller 231 located at the lowermost end.

That is, the

injection ports

242 and 252 are located lower than the lowest impeller 231, and the distance between the

injection ports

242 and 252 may overlap with the rotational flow area of the impeller, particularly the impeller 231 located at the lowest end, when viewed in plan.

Therefore, the gaseous raw material 260 injected from the

injection ports

242, 252 is immediately supplied to the rotating flow region of the impeller 231 located at the lowermost end, so that gas retention can be further improved, and the reaction rate in the reactor can also be further increased. In addition, it is possible to maintain the gas phase concentration in the lower portion of the reactor 200 and to increase the amount of the raw material 260 (such as phosgene) participating in the reaction. In conclusion, it is possible to provide a batch reactor 200 capable of producing a uniform product in a shorter time, improving productivity and improving stability of product quality.

Referring again to fig. 1 and 2, the one or

more impellers

131, 132, 133, 231, 232, and 233 may include at least one of a radial-type impeller and an axial-type impeller.

Among them, since the

impellers

131 and 231 located at the lowermost ends are adjacent to the

injection ports

142, 152, 242, and 252 for discharging the gaseous

raw materials

160 and 260, it is important to pulverize and disperse the gaseous

raw materials

160 and 260 that flow first. Therefore, it is preferable that the

impellers

131 and 231 located at the lowermost ends be radial type impellers in order to efficiently disperse the gaseous

raw materials

160 and 260 or to pulverize them into a fine gas phase. Since the radial type impeller is an impeller capable of generating a cross flow perpendicular to the rotation axes 130 and 230, the gaseous

raw materials

160 and 260 can be efficiently pulverized and dispersed. In fig. 1 and 2, the

impellers

131 and 231 located at the lowermost ends are shown as radial type impellers in which the plate-shaped agitating

blades

130 and 230 are aligned parallel to the

rotating shafts

130 and 230, but the shape is not limited thereto as long as it can generate a cross flow.

Preferably, the

impellers

132, 133, 232, and 233, which are located higher than the

lowest impellers

131 and 231, are axial type impellers. The axial type impeller is an impeller capable of generating a longitudinal flow parallel to the rotation axes 130 and 230. The gaseous

raw materials

160 and 260 dispersed by the

impellers

131 and 231 located at the lowermost ends and then ascending along the inner walls of the

cylindrical reactor bodies

120 and 220 can be uniformly supplied to the

entire reactors

100 and 200 by the longitudinal flow. That is, an axial type impeller is preferably located in the upper portion of the

reactors

100 and 200 to perform uniform slurry stirring. In fig. 1 and 2, the

impellers

132, 133, 232, and 233, which are located higher than the

lowest impellers

131 and 231, are shown as radial type impellers in which plate-shaped stirring blades are aligned parallel to the

rotation shafts

130 and 230, but the shape is not limited thereto as long as it can generate longitudinal flow.

Further, by configuring one or more of the plurality of

impellers

131, 132, 133, 231, 232, and 233, the reactants in the

batch reactors

100 and 200 can be efficiently stirred, and the flow of the reactants can be uniformly maintained for each region. Therefore, a uniform product can be finally produced, thereby improving productivity and improving stability of product quality.

In addition, although not shown, the

batch reactors

100 and 200 may further include a baffle plate between the

cylindrical reactor bodies

120 and 220 and the one or

more impellers

131, 132, 133, 231, 232, and 233. The baffle (not shown) serves to change the circumferential flow of the reactant in the up and down direction according to the rotation of the

impellers

131, 132, 133, 231, 232, and 233 to improve the mixing of the reactant, and to keep the temperature of the reactant constant by heat exchange between the reactant and the fluid flowing inside the tubes of the baffle (not shown), and may be a plate type, a double tube, or a coil type, and most preferably a plate type, since the shape thereof is not limited.

Meanwhile, as described above, the feeding positions, angles, types of

impellers

131, 132, 133, 231, 232, 233, and the like of the feeding

nozzles

140, 150, 240, and 250 are optimized to increase the reaction rate when the gaseous raw materials 160 and 260 (e.g., phosgene) are supplied to the

liquid solvents

110 and 210. Therefore, the

batch reactors

100 and 200 according to the embodiments of the present disclosure are preferably used for a reaction between a gas phase and a liquid phase. More preferably, phosgene is supplied as a raw material to be used in the process for preparing xylene diisocyanate.

Referring to fig. 3, a batch reactor 300 according to a comparative example has the same or similar configuration as the batch reactor 100 of fig. 1 except for the types of the

supply nozzles

340 and 350 and the

impellers

331, 332, and 333. That is, the batch reactor 300 includes a cylindrical reactor main body 320, the cylindrical reactor main body 320 including a side wall portion 321, a bottom portion 322, and a lid portion 323, and a rotation shaft 330 connected to

impellers

331, 332, and 333 and extending in the height direction (Y direction). The solvent 310 is contained inside the cylindrical reactor body 320.

The

impellers

331, 332, and 333 are curved impellers that rise and curve in the height direction (Y direction) of the rotating shaft 330.

In addition, the

supply nozzles

340 and 350 include

connection pipes

341 and 351 and

injection ports

342 and 352, but the

connection pipes

341 and 351 extend parallel to the height direction (Y direction) in a non-inclined state, and the

injection ports

342 and 352 are spaced apart from the impeller 331 located at the lowermost end by a considerable distance.

Example 1

The o-dichlorobenzene solvent was placed in the batch reactor 100 as shown in FIG. 1, and phosgene (COCl) was supplied through the supply nozzles 140 and 150₂) Simultaneously with the raw materials, a phosgenation reaction was carried out to produce xylene diisocyanate. The stirring speed of the

impellers

131, 132 and 133 was maintained at 150 rpm.

Example 2

The o-dichlorobenzene solvent was placed in a batch reactor 200 as shown in FIG. 2, and phosgene (COCl) was supplied thereto through supply nozzles 240 and 250₂) Simultaneously with the raw materials, a phosgenation reaction was carried out to produce xylene diisocyanate. The stirring speed of the

impellers

231, 232 and 233 was kept at 150 rpm.

Comparative example 1

The o-dichlorobenzene solvent was placed in a batch reactor 300 as shown in FIG. 3, and phosgene (COCl) was supplied through supply nozzles 340 and 350₂) Simultaneously with the raw materials, a phosgenation reaction was carried out to produce xylene diisocyanate. The stirring speed of the

impellers

331, 332 and 333 is maintained at 100 rpm.

Experimental example 1

The gas hold-up of example 1, example 2 and comparative example 1 was measured. It can be confirmed that example 1 shows a gas hold up of 9.37%, and example 2 shows a gas hold up of 10.7%, while comparative example 1 shows a value of 6.21% lower than examples 1 and 2. That is, it was confirmed that the reaction rates of example 1 and example 2 were improved as compared with comparative example 1.

Further, it can be confirmed that example 2 in which the supply nozzle is located at the lower end of the lowermost impeller shows higher gas retention than example 1 in which the supply nozzle is located at the side of the lowermost impeller. This is because the supply nozzle is located at the lower end of the lowermost impeller, so that the concentration of the gas phase can be maintained in a lower portion and the amount of the phosgene raw material participating in the reaction is increased.

Although the preferred embodiments of the present disclosure have been described in detail hereinabove, the scope of the present disclosure is not limited thereto, and various modifications and improvements made by those skilled in the art using the basic concept of the present disclosure defined in the appended claims also belong to the scope of the claims.

[ reference numerals ]

100, 200: batch reactor

140. 150, 240, 250: supply nozzle

141. 151, 241, 251: connecting pipe

142. 152, 242, 252: injection port

Claims

1. A batch reactor, comprising:

a cylindrical reactor body including a side wall portion, a bottom portion, and a lid portion;

one or more supply nozzles for supplying the raw material;

one or more impellers; and

a rotating shaft connected to the impeller and extending in a height direction,

wherein the supply nozzle includes a connection pipe extending from a side wall portion toward an inside of the cylindrical reactor main body, and an injection port located at one end of the connection pipe and configured to inject the raw material, and

wherein the height from the bottom portion to the injection port is equal to or less than the height from the bottom portion to the impeller located at the lowermost end among the one or more impellers.

2. A batch reactor according to claim 1,

wherein the connection pipe is inclined such that a position of the injection inlet is lower than a portion of the connection pipe connected to the sidewall part.

3. A batch reactor according to claim 2,

wherein the connection pipe forms an angle of 10 to 45 degrees with a width direction perpendicular to the rotation axis.

4. A batch reactor according to claim 1,

wherein the supply nozzle comprises a first supply nozzle and a second supply nozzle positioned spaced apart from each other about an axis of rotation.

5. A batch reactor according to claim 4,

wherein the height from the bottom portion to the injection port of the first supply nozzle and the injection port of the second supply nozzle is equal to the height from the bottom portion to the impeller located at the lowermost end, and

the distance between the injection port of the first supply nozzle and the injection port of the second supply nozzle is larger than the rotation diameter of the impeller located at the lowermost end.

6. A batch reactor according to claim 4,

wherein a height from the bottom portion to an injection port of the first supply nozzle and an injection port of the second supply nozzle is lower than a height from the bottom portion to the impeller located at the lowermost end, an

The distance between the injection port of the first supply nozzle and the injection port of the second supply nozzle is smaller than the rotation diameter of the impeller located at the lowermost end.

7. A batch reactor according to claim 1,

wherein the connection pipe is a pipe-shaped pipe, and the injection port includes a plurality of holes for injecting the raw material.

8. A batch reactor according to claim 1,

wherein the impeller comprises at least one of a radial type impeller and an axial type impeller.

9. A batch reactor according to claim 8,

wherein the impeller located at the lowermost end is a radial-type impeller.

10. A batch reactor according to claim 1,

wherein a liquid solvent is contained in a cylindrical reactor body, and

the feedstock comprises a gaseous material.

11. A batch reactor according to claim 1,

wherein the raw material comprises phosgene.