KR20220088142A - Batch reactor - Google Patents

Abstract

SUMMARY OF THE INVENTION It is an object of the present invention to provide a batch-type reaction apparatus that improves the distribution performance of phosgene to an amine salt in a slurry during the reaction of an aliphatic isocyanate using gaseous phosgene. A batch reaction apparatus according to an embodiment of the present invention includes a reactor for accommodating a slurry-like amine salt, a stirrer rotating with an impeller on a rotating shaft installed in a height direction in the reactor, and a gaseous raw material for the amine salt in the reactor and a sparger for distributing the raw material to the amine salt by the operation of the stirrer by supplying the sparger, wherein the sparger is provided in plurality along one of the axial direction of the stirrer and the circumferential direction of the reactor to supply gaseous raw materials do.

Description

Batch Reactor {BATCH REACTOR}

The present invention relates to a batch-type reactor, and more particularly, to a batch-type reactor for producing aliphatic isocyanate by injecting phosgene, a gaseous raw material, into a slurry-like amine salt and mixing it with a stirrer.

For the second phosgene reaction of the total two steps of the xylylene diisocyanate manufacturing process, gaseous phosgene is injected into the slurry-like amine salt generated in the first step salt formation reaction, and an impeller is used. A batch reactor that produces aliphatic isocyanate by stirring may be used.

At this time, it is necessary to effectively distribute the phosgene injected into the reactor to the amine salt in a slurry state to secure a gas holdup within a certain time.

SUMMARY OF THE INVENTION It is an object of the present invention to provide a batch-type reactor for improving phosgenation reactivity during the reaction of aliphatic isocyanate using gaseous phosgene. SUMMARY OF THE INVENTION It is an object of the present invention to provide a batch-type reaction apparatus that improves the distribution performance of phosgene to an amine salt in a slurry during the reaction of an aliphatic isocyanate using gaseous phosgene.

A batch reaction apparatus according to an embodiment of the present invention includes a reactor for accommodating a slurry-phase amine salt, a stirrer rotating with an impeller on a rotating shaft installed in a height direction in the reactor, and a gaseous raw material for the amine salt in the reactor and a sparger for distributing the raw material to the amine salt by the operation of the stirrer by supplying the sparger, wherein the sparger is provided in plurality along one of the axial direction of the stirrer and the circumferential direction of the reactor to supply gaseous raw materials do.

The sparger may be installed on the side wall of the reactor at set intervals along the axial direction of the agitator.

The sparger includes a pipe installed in the reactor in a direction whose longitudinal direction intersects the axial direction of the stirrer, and a bubble forming part provided at the end of the pipe to supply gaseous raw materials in a bubble state toward the impeller. can

The sparger may include an induction path penetratingly formed in the rotation shaft, and a bubble forming unit connected to the induction path through the rotation shaft to supply gaseous raw materials in a bubble state.

The impeller may be provided in a plurality of stages on the rotation shaft, and the bubble forming unit may be provided under each of the impellers.

The sparger may be installed on the side wall of the reactor at set intervals along the circumferential direction of the reactor from the lower end of the reactor.

The sparger may include a pipe whose longitudinal direction is installed in the reactor in the radial direction of the reactor, and a bubble forming part provided at the end of the pipe to supply gaseous raw materials in a bubble state toward the lower side of the impeller. .

The batch reaction apparatus according to an embodiment of the present invention may supply phosgene as the raw material to prepare xylylene diisocyanate.

The sparger may be installed in the reactor in a direction in which its longitudinal direction intersects the axial direction of the stirrer, and may be of a sintered porous type for supplying gaseous raw materials in a bubble state toward the impeller.

As such, the batch reactor of one embodiment is provided with a plurality of spargers along the axial direction of the stirrer or the circumferential direction of the reactor to supply gaseous raw materials, so that the distribution performance of the raw materials for the amine salt in the slurry, that is, the gas collection rate ( gas holdup) can be improved.

The batch reaction device of one embodiment is provided in plurality along the axial direction of the stirrer or the circumferential direction of the reactor and supplies gaseous phosgene to the impeller side, so the distribution performance of phosgene in the slurry-phase amine salt, that is, gas holdup. can do it Therefore, the reactivity of the aliphatic isocyanate using phosgene can be improved.

1 is a cross-sectional view of a batch-type reactor according to a first embodiment of the present invention.
2 is a cross-sectional view of a batch-type reactor according to a second embodiment of the present invention.
3 is a cross-sectional view of a batch-type reactor according to a third embodiment of the present invention.
4 is a cross-sectional view of a batch-type reactor according to Comparative Example 1.
5 is a cross-sectional view of a batch-type reactor according to a fourth embodiment of the present invention.

Hereinafter, with reference to the accompanying drawings, the embodiments of the present invention will be described in detail so that those skilled in the art can easily carry out the present invention. However, the present invention may be embodied in several different forms and is not limited to the embodiments described herein. In order to clearly explain the present invention in the drawings, parts irrelevant to the description are omitted, and the same reference numerals are given to the same or similar components throughout the specification.

1 is a cross-sectional view of a batch-type reactor according to a first embodiment of the present invention. Referring to FIG. 1 , the batch reactor 100 of the first embodiment includes a reactor 10 accommodating the amine salt 101 in a slurry form generated in the first-step salt formation reaction, a stirrer 20 and a gas in the reactor 10 . It includes a sparger (30) for supplying the raw material (102) of the phase.

As an example, the reactor 10 includes a cylindrical side wall portion 11 and a bottom portion 12 and a cover portion 13 that form a reaction space by forming the lower and upper sides of the side wall portion 11, respectively. The bottom part 12 and the cover part 13 are formed with convex curved surfaces on the lower side and the upper side, so that the amine salt 101 in the slurry form and the raw material 102 in the gaseous form can flow and be effectively mixed.

The stirrer 20 includes a rotating shaft 21 installed in the height direction of the reactor 10 and an impeller 22 provided on the rotating shaft 21 to stir the amine salt 101 and the raw material 102 . The rotating shaft 21 may be rotatably installed on the cover part 13 of the reactor 10 to face the bottom part 12 at the lower end, and may be driven by a driving motor (not shown) provided outside.

As an example, the impeller 22 includes a radial type impeller 221 and an axial type impeller 222 . The radial type impeller 221 creates a flow in the transverse direction perpendicular to the rotation shaft 21 to crush and disperse the gaseous raw material 102 supplied in the amine salt 101 . The axial type impeller 222 generates a flow in the same axial direction as the rotation shaft 21 to pulverize and disperse the gaseous raw material 102 supplied in the amine salt 101 .

In the first embodiment, the radial type impeller 221 is provided in one stage at the lower end of the rotating shaft 21 , and the axial type impeller 222 is the rotating shaft 21 from the upper side of the radial type impeller 221 . is provided in one stage. Although not shown, the axial type impeller 222 may be installed in more stages depending on the height of the rotation shaft 21 and the reactor 10 .

The sparger 30 is provided in plurality along one of the axial direction of the agitator 20 and the circumferential direction of the reactor 10, and is formed and installed to supply the gaseous raw material 102. According to the first embodiment, a plurality of spargers 30 are installed on the sidewall 11 of the reactor 10 at intervals D set along the axial direction of the agitator 20 .

The sparger 30 includes a pipe 31 and a bubble forming part 32 . The pipe 31 is installed in the side wall portion 11 of the reactor 10 in a direction whose longitudinal direction intersects the axial direction of the agitator 20 . As an example, the pipe 31 is installed at an angle θ set on the side wall portion 11 .

The bubble forming unit 32 is provided with a plurality of injection holes at the end of the pipe 31 to supply the gaseous raw material 102 in a bubble state toward the impeller 22 . A plurality of these spargers 30 are provided in the reactor 10 along the axial direction to uniformly distribute the gaseous raw material 102 in the axial direction.

When the impeller 22 is provided in plurality, the sparger 30 may be installed to correspond to the impeller 22 . Therefore, each impeller 22 uniformly distributes the gaseous raw material 102 supplied from each sparger 30 even within the interval D, and distributes the gaseous raw material 102 with respect to the entire axial direction of the reactor 10 . It can be distributed more evenly.

On the other hand, the radial type impeller 221 is rotationally driven around the gaseous raw material 102 supplied from the bubble forming part 32 of the sparger 30, and the amine salt 101 flows in the transverse direction. Therefore, the gaseous raw material 102 supplied to the bubble forming unit 32 of the sparger 30 is mixed with the amine salt 101 while flowing in the transverse direction by the transverse flow of the amine salt 101 .

The axial type impeller 222 is driven above the radial type impeller 221 to flow the amine salt 101 in the axial direction. Accordingly, the partially mixed gaseous raw material 102 and the gaseous raw material 102 are further mixed with the amine salt 101 while flowing in the axial direction due to the axial flow of the amine salt 101 .

As described above, the plurality of spargers 30 arranged in the axial direction uniformly distribute and supply the gaseous raw material 102 to the amine salt 101 to increase the gas holdup within a predetermined time. In conclusion, it is possible to improve the distribution performance of phosgene to the amine salt 101 in the slurry state in the phosgenation reaction proceeds by supplying the raw material 102 phosgene to the amine salt 101 . Accordingly, the reaction rate in the reactor 10 may be increased.

Meanwhile, the reactor 10 further includes a baffle 40 disposed parallel to the rotation shaft 21 and installed on the inner surface of the side wall portion 11 , that is, the inner surface. For example, the baffle 40 may be formed in a plate shape having a set width and height, or may be formed in a rod shape having a set diameter and length.

The baffle 40 generates a vortex in the flowing amine salt 101 when the impeller 22 is driven to mix the amine salt 101 and the raw material 102 more uniformly in the entire height direction of the reactor 10. make it possible

The baffle 40 is provided in plurality in the circumferential direction inside the reactor 10 to repeatedly form a vortex in the circumferential direction to mix the amine salt 101 and the raw material 102 more uniformly in the entire circumferential direction. makes it possible

In addition, the baffle 40 is provided in the vortex region generated by the rotational driving of the radial type impeller 221 and the axial type impeller 222 to directly act on the mixing of the amine salt 101 and the raw material 102 . can

In addition to the sparger 30, the use of the radial type impeller 221 and the axial type impeller 222 and the baffle 40 is when mixing by spraying the gaseous raw material 102 to the amine salt 101, Gas holdup can be further increased. Accordingly, the reaction rate in the reactor 10 may be further increased.

The batch reaction apparatus 100 according to the first embodiment of the present invention is used for a reaction between a gas phase and a slurry phase, and supplies phosgene, which is a gaseous raw material 102 , to an amine salt 101 to produce xylylene diisocyanate. It can be used in the manufacturing process.

Hereinafter, other examples and comparative examples of the present invention will be described. A description of the same configuration as that of the first embodiment will be omitted, and descriptions of different configurations will be described.

2 is a cross-sectional view of a batch-type reactor according to a second embodiment of the present invention. Referring to FIG. 2 , in the batch reactor 200 of the second embodiment, a plurality of spargers 230 include an induction furnace 34 and a bubble forming unit 35 .

The induction furnace 34 is formed through the rotation shaft 21 of the agitator 20 to supply the gaseous raw material 102 . The bubble forming unit 35 passes through the rotation shaft 21 and is connected to the induction furnace 34 to supply the gaseous raw material 102 to the amine salt 101 in a bubble state.

The impeller 22 is provided in a plurality of stages by maintaining the interval D2 set on the rotation shaft 21, and includes a radial type impeller 221 and an axial type impeller 222 which are sequentially provided from the lower side. In this case, the bubble forming portion 35 may be formed in plurality to correspond to the impeller 22 and the gap (D2).

That is, the first bubble forming unit 351 is provided below the radial type impeller 221 to supply gaseous fuel 102 , and the second bubble forming unit 352 is then the axial type impeller 222 . It is provided on the lower side of the gaseous fuel 102 is supplied.

The bubble forming unit 35 is provided with a plurality of injection holes on the rotating shaft 21 to supply the gaseous raw material 102 in a bubble state toward the lower side of the impeller 22 . In the sparger 230, the first and second bubble forming units 351 and 352 are provided in plurality in the reactor 10 along the axial direction, so that the gaseous raw material 102 can be uniformly distributed in the axial direction. let there be

As described above, since the first and second bubble forming parts 351 and 352 of the sparger 230 arranged in the axial direction uniformly distribute and supply the gaseous raw material 102 to the amine salt 101, the gas within a predetermined time Increases gas holdup. In conclusion, it is possible to improve the distribution performance of phosgene to the amine salt in a slurry state in the phosgenation reaction proceeds by supplying phosgene as the raw material 102 to the amine salt 101 . Accordingly, the reaction rate in the reactor 10 may be increased.

3 is a cross-sectional view of a batch-type reactor according to a third embodiment of the present invention. Referring to FIG. 3 , in the batch reactor 300 of the third embodiment, a plurality of spargers 330 are provided at the lower end of the reactor 10 at set intervals along the circumferential direction of the reactor ( It is installed on the side wall part 11 of 10).

The sparger 330 includes a pipe 31 and a bubble forming portion 32 . The pipe 31 is installed in the side wall portion 11 of the reactor 10 in a direction whose longitudinal direction intersects the axial direction of the agitator 20 .

The bubble forming unit 32 is provided with a plurality of injection holes at the end of the pipe 31 to supply the gaseous raw material to the lower end of the reactor 10 in a bubble state toward the lower side of the impeller. A plurality of these spargers 330 are provided in the reactor 10 along the circumferential direction to uniformly distribute the gaseous raw material in the circumferential direction.

On the other hand, the impeller 22 is rotationally driven from the upper side of the gaseous raw material 102 supplied from the bubble forming part 32 of the sparger 330 to flow the amine salt 101 . Therefore, the gaseous raw material 102 supplied to the bubble forming unit 32 of the sparger 330 is mixed with the amine salt 101 while flowing by the flow of the amine salt 101 .

As described above, since the plurality of spargers 330 arranged in the circumferential direction uniformly distribute and supply the gaseous raw material 102 to the amine salt 101 in the circumferential direction, the gas holdup is increased within a predetermined time. . In conclusion, it is possible to improve the distribution performance of phosgene to the amine salt in a slurry state in the phosgenation reaction proceeds by supplying phosgene as the raw material 102 to the amine salt 101 . Accordingly, the reaction rate in the reactor 10 may be increased.

4 is a cross-sectional view of a batch-type reactor according to Comparative Example 1. Referring to FIG. 4 , in the batch reactor 400 of Comparative Example 1, the sparger 430 is formed in a ring type having an injection hole 431 , and is disposed below the impeller 22 to gaseous raw material 102 . is supplied as an amine salt (101).

The impeller 22 is rotationally driven above the gaseous raw material 102 injected from the sparger 430 to flow the amine salt 101 . Therefore, the gaseous raw material 102 injected into the injection holes 431 of the sparger 430 is mixed with the amine salt 101 while flowing by the flow of the amine salt 101 . Compared with the first, second, and third examples, in Comparative Example 1, the distribution performance of the gaseous raw material 102 with respect to the amine salt 101 is lowered.

5 is a cross-sectional view of a batch-type reactor according to a fourth embodiment of the present invention. Referring to FIG. 5 , in the batch reactor 500 of the fourth embodiment, two spargers 530 are provided, and are installed on the sidewall 11 of the reactor 10 at the lower end of the reactor 10 .

The sparger 530 is formed of a sintered porous type. The sintered porous sparger 530 forms pores in the entire length of the reactor 10 to uniformly distribute the gaseous raw material 102 in the circumferential direction.

In the stirrer of the present invention, the impeller may be provided with one or two or more, that is, a plurality of radial-type impellers or axial-type impellers installed at the bottom, and the same or different types of impellers thereon. In addition, in the agitator, the impeller may be alternately provided up to n stages requiring a radial type impeller and an axial type impeller. Various drawings corresponding to this case are omitted.

Table 1 shows the gas collection rates for Examples 1, 2, 3, 4, and Comparative Examples.

first embodiment second embodiment 3rd embodiment 4th embodiment comparative example type Axially Spaced Pipe Induction furnace in the agitator shaft Circumferentially Spaced Pipe Sintered porous type ring Count revenge revenge revenge revenge - Gas capture rate (%) >10 >15 >10 >15 >5 Reaction time (hr) 13.9 9.5 11.2 10.6 14.3

first embodiment

The amine salt 101 was placed in the batch reactor 100 of FIG. 1 , and phosgene, which is a gaseous raw material 102 , was supplied to the amine salt 101 by a sparger 30 to prepare xylylene diisocyanate. In the first embodiment, two-stage impellers 32 were used, and the pipe-type sparger 30 was used in two stages along the axial direction. The stirrer 20 was rotated at 50 to 500 rpm.

second embodiment

The amine salt 101 was placed in the batch reactor 200 of FIG. 2 , and phosgene as the gaseous raw material 102 was supplied to the amine salt 101 by a sparger 230 to prepare xylylene diisocyanate. In the second embodiment, the two-stage impeller 22 is used, and the bubble forming part 35 is provided in two stages in the induction path 34 formed on the rotating shaft 21 . The stirrer 20 was rotated at 50 to 500 rpm.

The amine salt 101 was placed in the batch reactor 300 of FIG. 3 , and phosgene as the gaseous raw material 102 was supplied to the amine salt 101 by a sparger 330 to prepare xylylene diisocyanate. In the third embodiment, two-stage impellers 22 were used, and two pipe-type spargers 330 were used along the circumferential direction. The stirrer 20 was rotated at 50 to 500 rpm.

4th embodiment

The amine salt 101 was placed in the batch reactor 500 of FIG. 5 , and phosgene as the gaseous raw material 102 was supplied to the amine salt 101 by a sparger 530 to prepare xylylene diisocyanate. In the fourth embodiment, two-stage impellers 22 were used, and two sintered porous spargers 530 were used along the circumferential direction. The stirrer 20 was rotated at 50 to 500 rpm.

Comparative Example 1

The amine salt 101 was placed in the batch reactor 400 of FIG. 4 , and phosgene as the gaseous raw material 102 was supplied to the amine salt 101 by a sparger 430 to prepare xylylene diisocyanate. Comparative Example 1 uses a two-stage impeller 32 , and a single ring-type sparger 430 is used below the impeller 22 . The stirrer 20 was rotated at 50 to 500 rpm.

Experimental Example 1

The gas collection rates of Examples 1, 2, 3, 4 and Comparative Example 1 were measured. In Example 1, for a reaction time of 13.9 hr, the gas collection rate exceeds 10%, in Example 2, for a reaction time of 9.5 hr, the gas collection rate exceeds 15%, and in Example 3, the reaction time 11.2 For hr, the gas capture rate exceeded 10%, and Example 4 had a gas capture rate of more than 15% for a reaction time of 10.6 hr, whereas Comparative Example 1 had a gas capture rate of 5 for a reaction time of 14.3 hr. % was exceeded.

That is, Examples 1, 2, 3, and 4 showed an increased gas capture rate compared to Comparative Example 1 despite a shorter reaction time. Therefore, the first, second, third, and fourth Examples may increase the amount of phosgene, which is the raw material 102 participating in the reaction, as compared to Comparative Example 1, thereby improving the reactivity of the aliphatic isocyanate using phosgene.

Although preferred embodiments of the present invention have been described above, the present invention is not limited thereto, and it is possible to carry out various modifications within the scope of the claims, the description of the invention, and the accompanying drawings, and this also It goes without saying that it falls within the scope of the invention.

10: reactor 11: side wall
12: bottom part 13: cover part
20: agitator 21: rotation shaft
22: impeller 30, 230, 330, 530: sparger
31: pipe 32: bubble forming part
34: induction furnace 35: bubble forming part
40: baffle 100, 200, 300, 500: batch reactor
101: amine salt in slurry form 102: raw material
221: radial type impeller 222: axial type impeller
351: first bubble forming unit 352: second bubble forming unit
D, D2: spacing θ: angle

Claims (9)

a reactor for accommodating the amine salt in the slurry phase;
a stirrer rotating with an impeller on a rotating shaft installed in the height direction in the reactor; and
a sparger that supplies a gaseous raw material to the amine salt in the reactor and distributes the raw material to the amine salt by operation of the stirrer; and
includes,
The sparger
A batch type reactor for supplying a gaseous raw material provided in plurality along one of the axial direction of the stirrer and the circumferential direction of the reactor. According to claim 1,
The sparger
A batch type reactor installed on the side wall of the reactor at set intervals along the axial direction of the agitator. According to claim 1,
The sparger
A pipe installed in the reactor in a direction whose longitudinal direction intersects the axial direction of the agitator, and
A batch type reactor comprising a bubble forming unit provided at the end of the pipe to supply the gaseous raw material in a bubble state toward the impeller. According to claim 1,
The sparger
an induction path formed through the rotation shaft; and
and a bubble forming part connected to the induction furnace through the rotation shaft to supply gaseous raw materials in a bubble state. 5. The method of claim 4,
The impeller is
It is provided in a plurality of stages on the rotating shaft,
The bubble forming part
A batch type reaction device provided under each of the impellers. According to claim 1,
The sparger
A batch type reactor installed on the side wall of the reactor at a set interval along the circumferential direction of the reactor at the lower end of the reactor. 7. The method of claim 6,
The sparger
A pipe whose longitudinal direction is installed in the reactor in the radial direction of the reactor, and
and a bubble forming part provided at the end of the pipe to supply gaseous raw materials in a bubble state toward a downward direction of the impeller. According to claim 1,
A batch type reactor for producing xylylene diisocyanate by supplying the raw material phosgene. 7. The method of claim 6,
The sparger
A batch-type reactor of a sintered porous type that is installed in the reactor in a direction whose longitudinal direction intersects the axial direction of the stirrer to supply gaseous raw materials in a bubble state toward the impeller.

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