Batch type reaction apparatus

Abstract

To provide a batch type reaction apparatus.SOLUTION: A batch reaction apparatus according to an embodiment of the present disclosure includes: a reactor storing a liquid solvent; a sparger configured to supply a gaseous raw material into the reactor; and a stirrer having an impeller on a rotational shaft installed in the reactor in a height direction to stir the solvent and the raw material, where the impeller includes a radial-type impeller and an axial-type impeller.SELECTED DRAWING: Figure 1

Description

[Technical field]

[0001] [CROSS REFERENCE TO RELATED APPLICATIONS] This application claims the benefit of priority to Korean Patent Applications Nos. 10-2020-0178880, 10-2020-0178881, 10-2020-0178882, and 10-2020-0178883, filed December 18, 2020, and all contents disclosed in the documents of these Korean patent applications are incorporated herein by reference.

[0002] The present invention relates to a batch reactor. [Background technology]

[0003] In the manufacturing process of Xylylene Diisocyanate, a batch reactor can be used in which gaseous raw materials are injected into a salt-forming reaction solvent and mixed with an impeller.

[0004] The salt-forming reaction proceeds in the presence of a solvent. The amine salt, which is the product of the salt-forming reaction, is in the form of particles with diameters of several to several tens of microns, so it disperses in the solvent as the reaction proceeds and turns into a slurry.

[0005] In general, in such heterogeneous reactions where different phases exist, mixing of reactants is very important. For example, in order to effectively disperse and quickly dissolve gaseous hydrogen chloride in a liquid solvent, a method has been attempted in which the gas is blown into the liquid in the form of small bubbles to increase the contact area between the gas and the liquid.

[0006] As another example, for the second phosgenation reaction of the two steps in the manufacturing process of xylylene diisocyanate, a batch reactor can be used in which gaseous phosgene is injected into a slurry-like amine salt and mixed with an impeller.

[0007] At this time, the phosgene injected into the reactor must be effectively distributed to the amine salt in a slurry state to ensure gas holdup within a certain time. Summary of the Invention [Problem to be solved by the invention]

[0008] One aspect of the present invention is to provide a batch reaction apparatus that improves reactivity during the reaction of an aliphatic isocyanate using gaseous hydrogen chloride.

[0009] Another object of the present invention is to provide a batch reaction apparatus which improves the mixing performance of reactants during the reaction of an aliphatic isocyanate using gaseous hydrogen chloride.

[0010] Another object of the present invention is to provide a batch reaction apparatus which improves the distribution performance of hydrogen chloride to a solvent during the reaction of an aliphatic isocyanate using gaseous hydrogen chloride.

[0011] Another object of the present invention is to provide a batch reaction apparatus which improves the phosgenation reactivity during the reaction of an aliphatic isocyanate using gaseous phosgene.

[0012] Another object of the present invention is to provide a batch reaction apparatus which improves the mixing performance of phosgene with a slurry-like amine salt during the reaction of an aliphatic isocyanate using gaseous phosgene.

[0013] Another object of the present invention is to provide a batch reaction apparatus which improves the distribution performance of phosgene to a slurry-like amine salt during the reaction of an aliphatic isocyanate using gaseous phosgene. [Means for solving the problem]

[0014] A batch reactor according to an embodiment of the present invention includes a reactor for accommodating a liquid solvent, a sparger for supplying a gaseous raw material into the reactor, and an agitator having an impeller on a rotating shaft installed in the height direction of the reactor to agitate the solvent and the raw material, and the impeller includes a radial type impeller and an axial type impeller.

[0015] The radial type impeller may be provided in one stage at a lower end of the rotating shaft, and the axial type impeller may be provided in one or more stages on the rotating shaft above the radial type impeller.

[0016] The axial type impeller may be provided in one stage at a lower end of the rotating shaft, and the radial type impeller may be provided in one or more stages on the rotating shaft above the axial type impeller.

[0017] The reactor may include a baffle disposed in line with the rotating shaft and installed on an inner surface thereof. The baffle may be in the form of a plate or a rod.

[0018] The feedstock may be hydrogen chloride.

[0019] The batch reactor according to an embodiment of the present invention can produce xylylene diisocyanate by supplying hydrogen chloride as the raw material.

[0020] Meanwhile, a batch reactor according to an embodiment of the present invention includes a reactor for accommodating a liquid solvent, an agitator having an impeller attached to a rotating shaft installed in the height direction within the reactor and rotating, and a sparger for distributing the raw material to the solvent by the operation of the agitator so as to supply hydrogen chloride, which is a gaseous raw material, to the solvent in the reactor to produce xylylene diisocyanate, and the sparger supplies the gaseous raw material in at least one of the axial direction of the agitator and the circumferential direction of the reactor.

[0021] The spargers may be provided in a plurality along the circumferential direction of the agitator and installed on the side wall of the reactor at set intervals.

[0022] The sparger may include a pipe installed in the reactor in a direction whose length intersects with the axial direction of the agitator, and a bubble forming unit provided at an end of the pipe to supply a gaseous raw material in a bubble state toward the impeller.

[0023] The sparger may be provided singly at the lower end of the reactor and installed on the sidewall of the reactor.

[0024] The sparger may include a pipe whose length direction is in the diameter direction of the reactor and is installed in the reactor, and a bubble forming unit provided at an end of the pipe and supplying a gaseous raw material in a bubble state toward below the impeller.

[0025] The sparger may include a circular ring provided below the agitator, and a bubble forming unit provided above the ring to supply a gaseous raw material in a bubble state toward below the impeller.

[0026] The sparger may be installed in the reactor so that its length direction intersects with the axial direction of the agitator, and may be formed of a sintered porous type that supplies gaseous raw material in a bubble state toward the impeller.

[0027] The impeller may be a radial type impeller or an axial type impeller at the lower stage, and one or more impellers of the same or different types may be provided above it.

[0028] Meanwhile, a batch reactor according to an embodiment of the present invention includes a reactor for accommodating a slurry-like amine salt, a sparger for supplying phosgene, which is a gaseous raw material, into the reactor, and an agitator having an impeller on a rotating shaft installed in the height direction of the reactor to agitate the amine salt and phosgene to produce xylylene diisocyanate, and the impellers are arranged in multiple stages on the rotating shaft.

[0029] The impeller may be formed of at least one of a radial type impeller and an axial type impeller.

[0030] The impeller may include a radial type impeller provided in one stage on a lower end of the rotating shaft, and an axial type impeller provided in at least two stages on the rotating shaft above the radial type impeller.

[0031] The impeller may include a radial type impeller provided in one stage on a lower end of the rotating shaft, and an axial type impeller provided in one stage on the rotating shaft above the radial type impeller.

[0032] The sparger may be installed so as to supply the gaseous raw material in the axial direction of the agitator and in the circumferential direction of the reactor.

[0033] The sparger may include a pipe installed on a side wall of the reactor in a direction whose length intersects with the axial direction of the agitator, and a bubble forming unit provided with a plurality of nozzles at an end of the pipe and supplying a gaseous raw material in a bubble state toward the impeller.

[0034] Meanwhile, a batch reactor according to an embodiment of the present invention includes a reactor for accommodating a slurry-type amine salt, an agitator having an impeller attached to a rotating shaft installed in a height direction within the reactor and rotating, and a sparger for supplying a gaseous raw material to the amine salt within the reactor so that the raw material is distributed to the amine salt by the operation of the agitator, and a plurality of spargers are provided along one of an axial direction of the agitator and a circumferential direction of the reactor to supply the gaseous raw material.

[0035] The spargers may be installed on the sidewall of the reactor at set intervals along the axial direction of the agitator.

[0036] The sparger may include a pipe installed in the reactor in a direction whose length intersects with the axial direction of the agitator, and a bubble forming unit provided at an end of the pipe to supply a gaseous raw material in a bubble state toward the impeller.

[0037] The sparger may include an induction path formed through the rotating shaft, and a bubble forming unit that passes through the rotating shaft and is connected to the induction path to supply a gaseous raw material in a bubble state.

[0038] The impeller may be provided in a plurality of stages on the rotating shaft, and the bubble forming portion may be provided below each of the impellers.

[0039] The spargers may be installed on a sidewall of the reactor at set intervals along a circumference of the reactor at a lower end of the reactor.

[0040] The sparger may include a pipe whose length direction is in the diameter direction of the reactor and is installed in the reactor, and a bubble forming unit provided at an end of the pipe and supplying a gaseous raw material in a bubble state toward below the impeller.

[0041] The batch reactor according to an embodiment of the present invention can produce xylylene diisocyanate by supplying phosgene as the raw material.

[0042] The sparger is installed in the reactor so that its length direction intersects with the axial direction of the agitator, and is of a sintered porous type that supplies gaseous raw material in a bubble state toward the impeller. Effect of the Invention

[0043] In one embodiment, the batch reactor is provided with a radial type impeller and an axial type impeller on the rotating shaft of the agitator, so that the mixing performance of the solvent and hydrogen chloride, i.e., the gas holdup, can be improved during the reaction of the aliphatic isocyanate using gaseous hydrogen chloride, and therefore the reactivity of the aliphatic isocyanate using hydrogen chloride can be improved.

[0044] In addition, in one embodiment of the batch reactor, the gaseous raw material is supplied to the sparger in the axial direction of the agitator or in the circumferential direction of the reactor, and the raw material is distributed to the solvent by the operation of the agitator, so that the distribution performance of hydrogen chloride to the solvent, i.e., the gas holdup, can be improved during the reaction of aliphatic isocyanate using gaseous hydrogen chloride, and therefore the reactivity of aliphatic isocyanate using hydrogen chloride can be improved.

[0045] In addition, since the batch reactor of the embodiment is provided with a plurality of impellers on the rotating shaft of the agitator, the mixing performance of phosgene with the slurry-like amine salt, i.e., the gas holdup, can be improved during the reaction of the aliphatic isocyanate using gaseous phosgene, and therefore an aliphatic isocyanate with improved phosgenation reactivity can be produced.

[0046] In addition, the batch reactor of the embodiment is provided with a plurality of spargers along the axial direction of the agitator or the circumferential direction of the reactor to supply gaseous raw materials, so that the distribution performance of the raw materials to the slurry-like amine salt, i.e., the gas holdup, can be improved.

[0047] In one embodiment, the batch reactor is provided with a plurality of spargers along the axial direction of the agitator or the circumferential direction of the reactor, and gaseous phosgene is supplied to the impeller side, so that the distribution performance of phosgene in the slurry-like amine salt, i.e., the gas holdup, can be improved, and therefore the reactivity of aliphatic isocyanate using phosgene can be improved. [Brief description of the drawings]

[0048] [Figure 1] FIG. 1 is a cross-sectional view of a batch reaction apparatus according to Example 1-1 of the present invention. [Diagram 2] FIG. 2 is a cross-sectional view of a batch reaction apparatus according to a first and second embodiment of the present invention. [Diagram 3] FIG. 2 is a cross-sectional view of a batch reaction apparatus according to Comparative Example 1-1. [Figure 4] FIG. 2 is a cross-sectional view of a batch reaction apparatus according to Comparative Example 1-2. [Diagram 5] FIG. 2 is a cross-sectional view of a batch reaction apparatus according to the first to third embodiments of the present invention. [Figure 6] FIG. 1 is a cross-sectional view of a batch reaction apparatus according to Examples 1 to 4 of the present invention. [Figure 7] FIG. 1 is a cross-sectional view of a batch reaction apparatus according to Examples 1-5 of the present invention. [Figure 8] FIG. 2 is a cross-sectional view of a batch reaction apparatus according to Example 2-1 of the present invention. [Figure 9] FIG. 2 is a cross-sectional view of a batch reaction apparatus according to Example 2-2 of the present invention. [Figure 10] FIG. 2 is a cross-sectional view of a batch reaction apparatus according to Example 2-3 of the present invention. [Figure 11] FIG. 4 is a cross-sectional view of a batch reaction apparatus according to Comparative Example 2. [Figure 12]FIG. 2 is a cross-sectional view of a batch reaction apparatus according to Example 2-4 of the present invention. [Figure 13] FIG. 3 is a cross-sectional view of a batch reaction apparatus according to Example 3-1 of the present invention. [Figure 14] FIG. 3 is a cross-sectional view of a batch reaction apparatus according to Example 3-2 of the present invention. [Figure 15] FIG. 11 is a cross-sectional view of a batch reaction apparatus according to Comparative Example 3. [Figure 16] FIG. 4 is a cross-sectional view of a batch reaction apparatus according to Example 4-1 of the present invention. [Figure 17] FIG. 4 is a cross-sectional view of a batch reaction apparatus according to Example 4-2 of the present invention. [Figure 18] FIG. 4 is a cross-sectional view of a batch reaction apparatus according to Example 4-3 of the present invention. [Figure 19] FIG. 11 is a cross-sectional view of a batch reaction apparatus according to Comparative Example 4. [Figure 20] FIG. 4 is a cross-sectional view of a batch reaction apparatus according to Example 4-4 of the present invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0049] Hereinafter, the embodiments of the present invention will be described in detail with reference to the accompanying drawings so that those skilled in the art to which the present invention pertains can easily carry out the embodiments. However, the present invention may be embodied in various different forms and is not limited to the embodiments described herein. In order to clearly explain the present invention in the drawings, parts that are not related to the description are omitted, and the same reference numerals are used throughout the specification to refer to the same or similar components.

[0050] A first embodiment of the present invention will now be described.

[0051] Fig. 1 is a cross-sectional view of a batch reactor according to Example 1-1 of the present invention. Referring to Fig. 1, the batch reactor 1100 of Example 1-1 includes a reactor 110 that contains a liquid solvent 1101, a sparger 120 that supplies a gaseous raw material 1102 into the reactor 110, and an agitator 130.

[0052] For example, the reactor 110 includes a cylindrical side wall 111, a bottom 112 and a cover 113 that respectively form the upper and lower sides of the side wall 111 to form a reaction space. The bottom 112 and the cover 113 are formed with curved surfaces that bulge upward and downward, allowing the liquid solvent 1101 and the gaseous raw material 1102 to flow and be effectively mixed.

[0053] The sparger 120 is installed below the agitator 130 at a distance above the bottom 112 of the reactor 110, and has a plurality of injection ports 121 so that gaseous raw materials can be injected from the bottom of the agitator 130.

[0054] The sparger 120 is bent at the bottom of the agitator 130 and has a plurality of nozzles 121 corresponding to the rotation range of the agitator 130. The plurality of nozzles 121 in the sparger 120 enable uniform injection of hydrogen chloride (HCl) of the gaseous raw material 1102 into the liquid solvent 1101.

[0055] The agitator 130 includes a rotating shaft 131 installed in the height direction of the reactor 110, and an impeller 132 attached to the rotating shaft 131 to agitate the solvent 1101 and the raw material 1102. The rotating shaft 131 is rotatably installed on the cover 113 of the reactor 110, with its lower end facing the bottom 112, and can be driven by an external driving motor (not shown).

[0056] The impeller 132 includes a radial type impeller 1321 and an axial type impeller 1322. The radial type impeller 1321 generates a flow in a lateral direction perpendicular to the rotation axis 131 to crush and disperse the gaseous raw material 1102 supplied in the liquid solvent 1101. The axial type impeller 1322 generates a flow in the same axial direction as the rotation axis 131 to crush and disperse the gaseous raw material 1102 supplied in the liquid solvent 1101.

[0057] In the 1-1 embodiment, the radial type impeller 1321 is provided in one stage at the lower end of the rotating shaft 131, and the axial type impeller 1322 may be provided in one stage or more on the rotating shaft 131 above the radial type impeller 1321. That is, the radial type impeller 1321 is installed in the first stage, and the axial type impeller 1322 is installed in the second stage. Although not shown, the axial type impeller 1322 may be installed in one or more stages depending on the height of the rotating shaft 131 and the reactor 110.

[0058] The radial type impeller 1321 is rotated above the gaseous raw material 1102 injected from the injection port 121 of the sparger 120, and causes the solvent 1101 to flow laterally. Therefore, the gaseous raw material 1102 injected from the injection port 121 of the sparger 120 is mixed into the solvent 1101 while flowing laterally due to the lateral flow of the solvent 1101.

[0059] The axial type impeller 1322 is driven above the radial type impeller 1321 to flow the solvent 1101 in the axial direction. Therefore, the partially mixed gaseous raw material 1102 and the gaseous raw material 1102 are further mixed into the solvent 1101 while flowing in the axial direction due to the axial flow of the solvent 1101.

[0060] Amine salt is produced as a salt-forming reaction proceeds by mixing a raw material 1102 with a solvent 1101. The product amine salt is in the form of particles having a diameter of several to several tens of microns, and changes to a slurry form dispersed in the solvent as the reaction proceeds.

[0061] In this way, the combined use of the radial type impeller 1321 and the axial type impeller 1322 increases the gas holdup rate when the gaseous raw material 1102 is injected into and mixed with the solvent 1101. Therefore, the reaction rate in the reactor 110 can be increased. In conclusion, in the reaction in which the raw material 1102 is mixed with the solvent 1101 to generate a slurry, a uniform product can be produced in a shorter time, increasing productivity and improving the stability of the product quality.

[0062] Meanwhile, the reactor 110 further includes a baffle 140 disposed alongside the rotation shaft 131 and installed on the inner surface, i.e., the inner side, of the sidewall 111. For example, the baffle 140 may be formed in a plate shape having a set width and height, or in a rod shape having a set diameter and length.

[0063] The baffle 140 generates a vortex in the flowing solvent 1101 when the impeller 132 is driven, thereby enabling the solvent 1101 and the raw material 1102 to be mixed more uniformly over the entire height direction of the reactor 110 .

[0064] A plurality of baffles 140 are provided inside the reactor 110 along the circumferential direction, and repeatedly form vortexes in the circumferential direction, enabling the solvent 1101 and the raw material 1102 to be mixed more uniformly over the entire circumferential area.

[0065] In addition, the baffle 140 is provided in the vortex region generated by the rotational drive of the radial type impeller 1321 and the axial type impeller 1322 , and can directly affect the mixing of the solvent 1101 and the raw material 1102 .

[0066] The use of the radial type impeller 1321, the axial type impeller 1322 and the baffle 140 can further increase the gas holdup when the gaseous raw material 1102 is injected and mixed into the solvent 1101. Therefore, the reaction rate in the reactor 110 can be further increased.

[0067] The batch reactor 1100 according to the first embodiment of the present invention is used for a reaction between a gaseous state and a liquid state, and can be used in a process for producing xylylene diisocyanate by supplying hydrogen chloride, which is a gaseous raw material 1102, to a liquid solvent 1101.

[0068] Various modifications and comparative examples of this embodiment will be described below. Explanations of the same configurations as in the 1-1 embodiment will be omitted, and explanations of the different configurations will be given.

[0069] 2 is a cross-sectional view of a batch reactor according to a first embodiment of the present invention. Referring to FIG. 2, in the impeller 152 of the batch reactor 1200 of the first embodiment, the axial type impeller 1522 is provided at the lower end of the rotating shaft 151 in one stage, and the radial type impeller 1521 may be provided at the upper side of the axial type impeller 1522 in one stage or two or more stages on the rotating shaft 151. That is, the axial type impeller 1522 is installed at the first stage, and the radial type impeller 1521 is installed at the second stage. Although not shown, the radial type impeller 1521 may be installed at one or more stages depending on the height of the rotating shaft 151 and the reactor 110.

[0070] The axial type impeller 1522 is rotated above the gaseous raw material 1102 injected from the nozzle 121 of the sparger 120, and causes the solvent 1101 to flow in the axial direction. Therefore, the gaseous raw material 1102 injected from the nozzle 121 of the sparger 120 is mixed into the solvent 1101 while flowing in the axial direction due to the axial flow of the solvent 1101.

[0071] The radial type impeller 1521 is driven above the axial type impeller 1522 to flow the solvent 1101 in a lateral direction. Thus, the partially mixed gaseous raw material 1102 and the gaseous raw material 1102 are further mixed into the solvent 1101 while flowing in a lateral direction due to the lateral flow of the solvent 1101.

[0072] In this way, the combined use of the axial type impeller 1522 and the radial type impeller 1521 increases the gas holdup rate when the gaseous raw material 1102 is injected into and mixed with the solvent 1101. Therefore, the reaction rate in the reactor 110 can be increased. In conclusion, a uniform product can be produced in a shorter time in the reaction of mixing the raw material 1102 with the solvent 1101 to generate a slurry, thereby increasing productivity and improving the stability of the product quality.

[0073] In addition, the baffle 140 is provided in the vortex region generated by the rotational drive of the axial type impeller 1522 and the radial type impeller 1521, and can directly affect the mixing of the solvent 1101 and the raw material 1102.

[0074] The use of the axial type impeller 1522, the radial type impeller 1521 and the baffle 140 can further increase the gas holdup when the gaseous raw material 1102 is injected and mixed into the solvent 1101. Therefore, the reaction rate in the reactor 110 can be further increased.

[0075] 3 is a cross-sectional view of a batch reactor according to Comparative Example 1-1. Referring to FIG. 3, in a batch reactor 1300 of Comparative Example 1-1, an agitator 160 has a plurality of radial type impellers 162 attached to a rotating shaft 161.

[0076] The radial type impeller 162 is rotated above the gaseous raw material 1102 injected from the sparger 120, and causes the solvent 1101 to flow laterally. Therefore, the gaseous raw material 1102 injected from the injection port 121 of the sparger 120 is mixed into the solvent 1101 while flowing laterally due to the lateral flow of the solvent 1101.

[0077] Two or more radial type impellers 162 are driven in the same manner to mix the gaseous raw material 1102 into the solvent 1101 by a flow in the lateral direction of the solvent 1101. Compared with Examples 1-1 and 1-2, it is difficult to form a flow in the axial direction of the solvent 1101 in Comparative Example 1-1.

[0078] 4 is a cross-sectional view of a batch reactor according to Comparative Example 1-2. Referring to FIG. 4, in a batch reactor 1400 of Comparative Example 1-2, an agitator 170 has a plurality of axial type impellers 172 attached to a rotating shaft 171.

[0079] The axial type impeller 172 is rotated above the gaseous raw material 1102 injected from the sparger 120, and causes the solvent 1101 to flow in the axial direction. Therefore, the gaseous raw material 1102 injected from the injection port 121 of the sparger 120 is mixed into the solvent 1101 while flowing in the axial direction due to the axial flow of the solvent 1101.

[0080] The two or more axial type impellers 172 are driven in the same manner to mix the gaseous raw material 1102 into the solvent 1101 by flowing in the axial direction of the solvent 1101. Compared with Examples 1-1 and 1-2, it is difficult to form a flow in a lateral direction relative to the solvent 1101 in Comparative Example 1-2.

[0081] 5 is a cross-sectional view of a batch reactor according to Example 1-3 of the present invention. Referring to FIG. 5, in the impeller 132 of the batch reactor 1500 of Example 1-3, the radial type impeller 1321 is provided at the lower end of the rotating shaft 131 in one stage, and the axial type impeller 1322 is provided at the upper side of the axial type impeller 1322 on the rotating shaft 131 in four stages.

[0082] 6 is a cross-sectional view of a batch reactor according to Example 1-4 of the present invention. Referring to FIG. 6, in the impeller 152 of the batch reactor 1600 of Example 1-4, the axial type impeller 1522 is provided in one stage at the lower end of the rotating shaft 151, and the radial type impeller 1521 is provided in four stages on the rotating shaft 151 above the axial type impeller 1522.

[0083] Fig. 7 is a cross-sectional view of a batch reactor according to Example 1-5 of the present invention. Referring to Fig. 7, in the impeller 152 of the batch reactor 1500 of Example 1-5, the axial type impeller 1522 is provided in three stages at the lower, middle and upper stages of the rotating shaft 151, and the radial type impeller 1521 is provided in two stages between the stages of the axial type impeller 1522.

[0084] Although not shown, the radial type impeller may be provided with three stages at the bottom, middle and top of the rotating shaft, and the axial type impeller may be provided with two stages between the stages of the radial type impeller.

[0085] In conclusion, in the agitator of the present invention, the impeller may be a radial type impeller or an axial type impeller installed in the lower stage, and one or more impellers of the same or different types may be installed above it. Also, in the agitator, the impeller may be installed alternately up to n stages where radial type impellers and axial type impellers are required. Various drawings corresponding to such cases will be omitted.

[0086] Table 1 shows the gas collection efficiencies for Examples 1-1 to 1-5, Comparative Example 1-1, and Comparative Example 1-2.

[0087] [Table 1]

[0088] Example 1-1 Solvent 1101 was placed in batch reactor 1100 in Fig. 1, and hydrogen chloride as raw material 1102 was supplied to solvent 1101 by sparger 120 to produce xylylene diisocyanate. In Example 1-1, a one-stage radial type impeller 1321 and a one-stage axial type impeller 1322 were used. The agitator 130 rotated at 50 to 500 rpm.

[0089] Example 1-2 Solvent 1101 was placed in the batch reactor 1200 of Fig. 2, and hydrogen chloride as raw material 1102 was supplied to the solvent 1101 by a sparger 120 to produce xylylene diisocyanate. In the second example, a one-stage axial type impeller 1522 and a one-stage radial type impeller 1521 were used. The agitator 150 rotated at 50 to 500 rpm.

[0090] Example 1-3 Solvent 1101 was placed in batch reactor 1500 in Fig. 5, and hydrogen chloride as raw material 1102 was supplied to solvent 1101 by sparger 120 to produce xylylene diisocyanate. In Example 1-3, a one-stage radial type impeller 1321 and a four-stage axial type impeller 1322 were used. The agitator 130 rotated at 50 to 500 rpm.

[0091] Examples 1-4 Solvent 1101 was placed in batch reactor 1600 in Fig. 6, and hydrogen chloride as raw material 1102 was supplied to solvent 1101 by sparger 120 to produce xylylene diisocyanate. In Examples 1-4, a one-stage axial type impeller 1522 and a four-stage radial type impeller 1521 were used. The agitator 150 rotated at 50 to 500 rpm.

[0092] Examples 1-5 Solvent 1101 was placed in batch reactor 1700 in Fig. 7, and hydrogen chloride as raw material 1102 was supplied to solvent 1101 by sparger 120 to produce xylylene diisocyanate. In Example 1-5, three-stage axial type impeller 1522 and two-stage radial type impeller 1521 were used, and a total of five stages of impellers were installed alternately. Agitator 150 rotated at 50 to 500 rpm.

[0093] Comparative Example 1-1 Solvent 1101 was placed in a batch reaction apparatus 1300 in Fig. 3, and hydrogen chloride as a raw material 1102 was supplied to the solvent 1101 by a sparger 120 to produce xylylene diisocyanate. In Comparative Example 1-1, a two-stage radial type impeller 162 was used. The agitator 160 rotated at 50 to 500 rpm.

[0094] Comparative Example 1-2 Solvent 1101 was placed in a batch reactor 1400 in Fig. 4, and hydrogen chloride as a raw material 1102 was supplied to the solvent 1101 by a sparger 120 to produce xylylene diisocyanate. In Comparative Example 1-2, a two-stage axial type impeller 172 was used. The agitator 170 rotated at 50 to 500 rpm.

[0095] Experimental Example 1 The gas collection rates of Example 1-1 to Example 1-5, Comparative Example 1-1, and Comparative Example 1-2 were measured. Example 1-1 had a gas collection rate of more than 10% during a reaction time of 6.0 hours, Example 1-2 had a gas collection rate of more than 10% during a reaction time of 6.3 hours, Example 1-3 had a gas collection rate of more than 10% during a reaction time of 4.5 hours, Example 1-4 had a gas collection rate of more than 10% during a reaction time of 5.3 hours, and Example 1-5 had a gas collection rate of more than 10% during a reaction time of 5.2 hours, whereas Comparative Example 1-1 had a gas collection rate of 4.7% during a reaction time of 7.8 hours, and Comparative Example 1-2 had a gas collection rate of 8.0% during a reaction time of 6.7 hours.

[0096] That is, Examples 1-1 to 1-5 show increased gas collection efficiency despite the shorter reaction time compared to Comparative Examples 1-1 and 1-2. Therefore, Examples 1-1 to 1-5 can improve the reactivity of aliphatic isocyanate using hydrogen chloride by inducing a change in the form of hydrogen chloride that can efficiently participate in the reaction of hydrogen chloride in the raw material 1102 participating in the reaction, compared to Comparative Examples 1-1 and 1-2.

[0097] A second embodiment of the present invention will now be described.

[0098] 8 is a cross-sectional view of a batch reactor according to Example 2-1 of the present invention. Referring to FIG. 8, the batch reactor 2100 of Example 2-1 includes a reactor 210 that contains a liquid solvent 2101, an agitator 220, and a sparger 230 that supplies a gaseous raw material 2102 into the reactor 210.

[0099] For example, the reactor 210 includes a cylindrical side wall 211, a bottom 212 and a cover 213 that respectively define the upper and lower sides of the side wall 211 to form a reaction space. The bottom 212 and the cover 213 are formed with curved surfaces that bulge at the bottom and top, allowing the liquid solvent 2101 and the gaseous raw material 2102 to flow and be effectively mixed.

[0100] The agitator 220 includes a rotating shaft 221 installed in the height direction of the reactor 210, and an impeller 222 installed on the rotating shaft 221 to agitate the solvent 2101 and the raw material 2102. The rotating shaft 221 is rotatably installed on the cover 213 of the reactor 210, with its lower end facing the bottom 212, and can be driven by an external driving motor (not shown).

[0101] For example, the impeller 222 includes a radial type impeller 2221 and an axial type impeller 2222. The radial type impeller 2221 generates a flow in a lateral direction perpendicular to the rotation axis 221 to crush and disperse the gaseous raw material 2102 supplied in the liquid solvent 2101. The axial type impeller 2222 generates a flow in the same axial direction as the rotation axis 221 to crush and disperse the gaseous raw material 2102 supplied in the liquid solvent 2101.

[0102] In the 2-1 embodiment, the radial type impeller 2221 is provided in one stage at the lower end of the rotating shaft 221, and the axial type impeller 2222 is provided in one stage on the rotating shaft 221 above the radial type impeller 2221. Although not shown, the radial type impeller 2221 and the axial type impeller 2222 may be installed in one or more stages depending on the height of the rotating shaft 221 and the reactor 210.

[0103] In the agitator of the present invention, the impeller may be a radial type impeller or an axial type impeller in the lower stage, and one or more impellers of the same or different types may be provided above it. Also, in the agitator, the impeller may be provided alternately up to n stages where radial type impellers and axial type impellers are required. Various drawings corresponding to such cases are omitted.

[0104] The sparger 230 is formed and installed so as to supply the gaseous raw material 2102 in at least one of the axial direction of the agitator 220 and the circumferential direction of the reactor 210. A plurality of spargers 230 may be provided.

[0105] According to the second embodiment, two spargers 230 are installed on the side wall 211 of the reactor 210 at set intervals along the circumferential direction of the agitator 220 .

[0106] The sparger 230 includes a pipe 231 and a bubble forming section 232. The pipe 231 is installed in the side wall section 211 of the reactor 210 such that the length direction of the pipe 231 intersects with the axial direction of the agitator 220. For example, the pipe 231 is installed at a set angle θ to the side wall section 211.

[0107] The bubble forming unit 232 is provided with a plurality of nozzles at the end of the pipe 231, and supplies the gaseous raw material 2102 in a bubble state toward the impeller 222. A plurality of such spargers 230 are provided in the reactor 210 along the circumferential direction, so that the gaseous raw material 2102 can be uniformly distributed in the circumferential direction.

[0108] The sparger 230 may be installed corresponding to the impeller 222. Thus, the impeller 222 can distribute the gaseous raw material 2102 supplied from the sparger 230 evenly within the interval, and can distribute the hydrogen chloride (HCl) of the gaseous raw material 2102 more evenly over the entire circumferential direction of the reactor 210.

[0109] Meanwhile, the radial type impeller 2221 is rotated around the gaseous raw material 2102 supplied to the bubble forming part 232 of the sparger 230, and causes the solvent 2101 to flow in the lateral direction. Therefore, the gaseous raw material 2102 supplied to the bubble forming part 232 of the sparger 230 is mixed into the solvent 2101 while flowing in the lateral direction due to the lateral flow of the solvent 2101.

[0110] The axial type impeller 2222 is driven above the radial type impeller 2221 to flow the solvent 2101 in the axial direction. Therefore, the partially mixed gaseous raw material 2102 and the gaseous raw material 2102 are further mixed into the solvent 2101 while flowing in the axial direction due to the axial flow of the solvent 2101.

[0111] A raw material 2102 is mixed into a solvent 2101, and an amine salt is produced as a salt-forming reaction proceeds. The amine salt, which is the product, is in the form of particles having a diameter of several to several tens of microns, and changes to a slurry form that disperses in the solvent as the reaction proceeds.

[0112] In this manner, the multiple spargers 230 arranged in the circumferential direction uniformly distribute and supply the gaseous raw material 2102 to the solvent 2101, thereby increasing the gas holdup rate within a certain time period. As a result, the reaction rate in the reactor 210 can be increased. In conclusion, the distribution performance of hydrogen chloride to the solvent can be improved in the reaction of generating a slurry state by supplying hydrogen chloride, which is the raw material 2102, to the solvent 2101. As a result, the reaction rate in the reactor 210 can be increased.

[0113] Meanwhile, the reactor 210 further includes a baffle 240 disposed alongside the rotation shaft 221 and installed on the inner surface, i.e., the inner side, of the sidewall 211. For example, the baffle 240 may be formed in a plate shape having a set width and height, or in a rod shape having a set diameter and length.

[0114] The baffle 240 generates a vortex in the flowing solvent 2101 when the impeller 222 is driven, thereby enabling the solvent 2101 and the raw material 2102 to be mixed more uniformly over the entire height direction of the reactor 210 .

[0115] A plurality of baffles 240 are provided inside the reactor 210 along the circumferential direction, and repeatedly form vortexes in the circumferential direction, enabling the solvent 2101 and the raw material 2102 to be mixed more uniformly over the entire circumferential area.

[0116] In addition, the baffle 240 is provided in a vortex region generated by the rotational drive of the radial type impeller 2221 and the axial type impeller 2222 , and can directly affect the mixing of the solvent 2101 and the raw material 2102 .

[0117] In addition to the sparger 230, the use of the radial type impeller 2221, the axial type impeller 2222, and the baffle 240 can further increase the gas holdup when injecting and mixing the gaseous raw material 2102 into the solvent 2101. Therefore, the reaction rate in the reactor 210 can be further increased.

[0118] The batch reactor 2100 according to the second embodiment of the present invention is used for a reaction between a gaseous state and a liquid state, and can be used in a process for producing xylylene diisocyanate by supplying hydrogen chloride, which is a gaseous raw material 2102, to a liquid solvent 2101.

[0119] Various modifications and comparative examples of this embodiment will be described below. Explanations of the same configurations as in the 2-1 embodiment will be omitted, and only explanations of the different configurations will be given.

[0120] 9 is a cross-sectional view of a batch reactor according to Example 2-2 of the present invention. Referring to FIG. 9, in the batch reactor 2200 of Example 2-2, a single sparger 2230 is provided and is installed on the side wall 211 of the reactor 210 at the lower end of the reactor 210.

[0121] The sparger 2230 includes a pipe 231 and a bubble forming unit 232. The pipe 231 is installed on the side wall 211 of the reactor 210 with its length direction intersecting the axial direction of the agitator 220. The bubble forming unit 232 is provided with a plurality of nozzles at the end of the pipe 231, and supplies the gaseous raw material in a bubble state to the lower end of the reactor 210 below the impeller.

[0122] On the other hand, the impeller 222 is rotated above the gaseous raw material 2102 supplied to the bubble forming part 232 of the sparger 2230, and causes the solvent 2101 to flow. Therefore, the gaseous raw material 2102 supplied to the bubble forming part 232 of the sparger 2230 is mixed into the solvent 2101 while flowing due to the flow of the solvent 2101.

[0123] In this way, one sparger 2230 supplies gaseous raw material 2102 to the solvent 2101, thereby increasing the gas holdup rate within a certain period of time. Therefore, the reaction rate in the reactor 210 can be increased. In conclusion, the distribution performance of hydrogen chloride to the solvent can be improved in the reaction of generating a slurry state by supplying hydrogen chloride of the raw material 2102 to the solvent 2101. Therefore, the reaction rate in the reactor 210 can be increased.

[0124] 10 is a cross-sectional view of a batch reactor according to Example 2-3 of the present invention. Referring to FIG. 10, in the batch reactor 2300 of Example 2-3, a sparger 2330 includes a ring 2331 and a bubble forming unit 2332. The ring 2331 is provided in a circular shape below the agitator 220, and the bubble forming unit 2332 is provided above the ring 2331, and supplies gaseous raw material in a bubble state toward the lower side of the impeller 222. Such a sparger 2330 allows the gaseous raw material to be uniformly distributed in the circumferential direction according to the diameter of the ring 2331.

[0125] On the other hand, the impeller 222 is rotated above the gaseous raw material 2102 supplied to the bubble forming part 2332 of the sparger 2330, and causes the solvent 2101 to flow. Therefore, the gaseous raw material 2102 supplied to the bubble forming part 2332 of the sparger 2330 is mixed into the solvent 2101 while flowing due to the flow of the solvent 2101.

[0126] In this manner, the sparger 2330 arranged in a circular shape below the agitator 220 uniformly distributes and supplies the gaseous raw material 2102 to the solvent 2101 in the circumferential direction, thereby increasing the gas holdup rate within a certain period of time. Therefore, the reaction rate in the reactor 210 can be increased. In conclusion, the distribution performance of hydrogen chloride to the solvent can be improved in the reaction of generating a slurry state by supplying hydrogen chloride, which is the raw material 2102, to the solvent 2101. Therefore, the reaction rate in the reactor 210 can be increased.

[0127] 12 is a cross-sectional view of a batch reactor according to Example 2-4 of the present invention. Referring to FIG. 12, in the batch reactor 2500 of Example 2-4, two spargers 2630 are provided and installed on the side wall 211 of the reactor 210 at the lower end of the reactor 210.

[0128] The sparger 2630 is of a sintered porous type. The sintered porous type sparger 2630 has holes in the entire length of the reactor 210, so that the gaseous raw material 2102 can be uniformly distributed in the circumferential direction.

[0129] 11 is a cross-sectional view of a batch reactor according to Comparative Example 2. Referring to FIG. 11, in the batch reactor 2400 of Comparative Example 2, a sparger 2430 is formed in a spider type and includes a plurality of branches 2431 and a bubble forming portion 2432.

[0130] A plurality of branches 2431 are provided below the agitator 220, and the bubble forming unit 2432 is provided below the branches 2431 and supplies the gaseous raw material in a bubble state toward the bottom 212. Such a sparger 2430 supplies the gaseous raw material far from the agitator 220 in the axial direction according to the length of the branches 2431.

[0131] Meanwhile, the impeller 222 is rotated above the gaseous raw material 2102 supplied to the bubble forming section 2432 of the sparger 2430, and causes the solvent 2101 to flow. Therefore, the gaseous raw material 2102 supplied to the bubble forming section 2432 of the sparger 2430 is mixed into the solvent 2101 while flowing due to the flow of the solvent 2101. Compared with the first, second and third embodiments, it is difficult to improve the distribution performance of hydrogen chloride to the solvent 2101 in the comparative example.

[0132] Table 2 shows the gas collection efficiencies for Example 2-1, Example 2-2, Example 2-3 and Comparative Example 2.

[0133] [Table 2]

[0134] Example 2-1 A solvent 2101 was placed in a batch reaction apparatus 2100 in Fig. 8, and hydrogen chloride as a raw material 2102 was supplied to the solvent 2101 by a sparger 230 to produce xylylene diisocyanate. In Example 2-1, two pipe-shaped spargers 230 were used. The agitator 220 rotated at 50 to 500 rpm.

[0135] Example 2-2 A solvent 2101 was placed in a batch reaction apparatus 2200 in Fig. 9, and hydrogen chloride as a raw material 2102 was supplied to the solvent 2101 by a sparger 2230 to produce xylylene diisocyanate. In Example 2-2, one pipe-shaped sparger 2230 was used. The agitator 220 rotated at 50 to 500 rpm.

[0136] Example 2-3 A solvent 2101 was placed in a batch reaction apparatus 2300 in Fig. 10, and hydrogen chloride as a raw material 2102 was supplied to the solvent 2101 by a sparger 2330 to produce xylylene diisocyanate. In Example 2-3, one ring-shaped sparger 2330 was used. The agitator 220 rotated at 50 to 500 rpm.

[0137] Example 2-4 A solvent 2101 was placed in the batch reaction apparatus 2500 of Fig. 12, and hydrogen chloride as a raw material 2102 was supplied to the solvent 2101 by a sparger 2630 to produce xylylene diisocyanate. In Example 2-4, two sintered porous spargers 2630 were used. The agitator 220 rotated at 50 to 500 rpm.

[0138] Comparative Example 2 11, a solvent 2101 was placed in the batch reaction apparatus 2400, and hydrogen chloride as a raw material 2102 was supplied to the solvent 2101 by a sparger 2430 to produce xylylene diisocyanate. In the comparative example, a spider-shaped sparger 2430 was used. The agitator 220 rotated at 50 to 500 rpm.

[0139] Experimental Example 2 The gas collection rates were measured for Example 2-1, Example 2-2, Example 2-3, and Comparative Example 2. Example 2-1 had a gas collection rate of more than 10% for a reaction time of 4.8 hours, Example 2-2 had a gas collection rate of more than 10% for a reaction time of 5.5 hours, Example 2-3 had a gas collection rate of more than 10% for a reaction time of 4.8 hours, Example 2-4 had a gas collection rate of more than 10% for a reaction time of 4.8 hours, while Comparative Example 2 had a gas collection rate of more than 5% for a reaction time of 7.1 hours.

[0140] That is, Examples 2-1, 2-2, 2-3, and 2-4 show increased gas collection efficiency despite the shorter reaction time compared to Comparative Example 2. Therefore, Examples 2-1, 2-2, 2-3, and 2-4 can increase the amount of hydrogen chloride in the raw material 2102 participating in the reaction compared to Comparative Example 2, thereby improving the reactivity of aliphatic isocyanate using hydrogen chloride.

[0141] A third embodiment of the present invention will now be described.

[0142] Fig. 13 is a cross-sectional view of a batch reactor according to Example 3-1 of the present invention. Referring to Fig. 13, a batch reactor 3100 according to Example 3-1 includes a reactor 310 for accommodating a slurry of an amine salt 3101, a sparger 320 for supplying a gaseous raw material 3102 into the reactor 310, and an agitator 330.

[0143] For example, the reactor 310 includes a cylindrical side wall 311, a bottom 312 and a cover 313 which respectively define the upper and lower sides of the side wall 311 to form a reaction space. The bottom 312 and the cover 313 are formed with curved surfaces which bulge at the bottom and upper sides, so that the amine salt in a slurry state 3101 and the gaseous raw material 3102 can flow and be effectively mixed.

[0144] The sparger 320 is formed and installed so as to supply the gaseous raw material 3102 in the axial direction of the agitator 330 and in the circumferential direction of the reactor 310. The sparger 320 includes a pipe 321 and a bubble forming section 322. The pipe 321 is installed in the side wall section 311 of the reactor 310 such that the length direction of the pipe 321 intersects with the axial direction of the agitator 330. For example, the pipe 321 is installed at a set angle θ to the side wall section 311.

[0145] The bubble forming unit 322 is provided with a plurality of nozzles at the end of the pipe 321, and supplies the gaseous raw material 3102 in a bubble state toward the impeller 332. The plurality of bubble forming units 322 in the sparger 320 enable the phosgene of the gaseous raw material 3102 to be uniformly sprayed into the amine salt slurry 3101.

[0146] The agitator 330 includes a rotating shaft 331 installed in the height direction of the reactor 310, and an impeller 332 installed on the rotating shaft 331 to agitate the amine salt 3101 and the raw material 3102. The impeller 332 is arranged in a plurality of stages on the rotating shaft 331. The rotating shaft 331 is rotatably installed on the cover 313 of the reactor 310, with its lower end facing the bottom 312, and can be driven by an externally installed driving motor (not shown).

[0147] The impeller 332 may be formed of at least one of a radial type impeller and an axial type impeller. In the third embodiment, the impeller 332 includes a radial type impeller 3321 and an axial type impeller 3322.

[0148] The radial type impeller 3321 generates a flow in a lateral direction perpendicular to the rotation axis 331 to crush and disperse the gaseous raw material 3102 supplied in the slurry-like amine salt 3101. The axial type impeller 3322 generates a flow in the same axial direction as the rotation axis 331 to crush and disperse the gaseous raw material 3102 supplied in the slurry-like amine salt 3101.

[0149] In the 3-1 embodiment, the radial type impeller 3321 is provided in one stage at the lower end of the rotating shaft 331, and the axial type impeller 3322 is provided in four stages on the rotating shaft 331 above the radial type impeller 3321. That is, the radial type impeller 3321 is installed in the first stage, and the axial type impellers 3322 are installed in the second to fifth stages.

[0150] In the agitator of the present invention, the impeller may be a radial type impeller or an axial type impeller in the lower stage, and one or more impellers of the same or different types may be provided above it. Also, the impeller in the agitator may be provided alternately up to n stages where radial type impellers and axial type impellers are required. Various drawings corresponding to such cases are omitted.

[0151] In the 3-1 embodiment, the radial type impeller 3321 is rotated around the gaseous raw material 3102 supplied from the bubble forming section 322 of the sparger 320, and causes the amine salt 3101 to flow laterally. Therefore, the gaseous raw material 3102 injected from the bubble forming section 322 of the sparger 320 is mixed with the amine salt 3101 while flowing laterally due to the lateral flow of the amine salt 3101.

[0152] The four-stage axial type impeller 3322 is driven above the radial type impeller 3321 to cause the amine salt 3101 to flow in the axial direction. Thus, the partially mixed gaseous raw material 3102 and the gaseous raw material 3102 are further mixed with the amine salt 3101 while flowing in the axial direction due to the axial flow of the amine salt 3101.

[0153] In this way, the combined use of one stage radial type impeller 3321 and four stages axial type impeller 3322 increases the gas holdup when the gaseous raw material 3102 is injected and mixed into the amine salt 3101. In conclusion, the distribution performance of phosgene to the reactants in a slurry state can be improved in the phosgenation reaction that is carried out by supplying the raw material 3102 phosgene to the amine salt 3101. Therefore, the reaction rate in the reactor 310 can be increased.

[0154] Meanwhile, the reactor 310 further includes a baffle 340 disposed alongside the rotation shaft 331 and installed on the inner surface, i.e., the inner side, of the sidewall 311. For example, the baffle 340 may be formed in a plate shape having a set width and height, or in a rod shape having a set diameter and length.

[0155] The baffle 340 generates a vortex in the flowing amine salt 3101 when the impeller 332 is driven, thereby enabling the amine salt 3101 and the raw material 3102 to be mixed more uniformly over the entire height direction of the reactor 310 .

[0156] A plurality of baffles 340 are provided inside the reactor 310 along the circumferential direction, and repeatedly form vortexes in the circumferential direction, enabling the amine salt 3101 and the raw material 3102 to be mixed more uniformly over the entire circumferential area.

[0157] In addition, the baffle 340 is provided in the vortex region generated by the rotational drive of the radial type impeller 3321 and the axial type impeller 3322 , and can directly act on the mixing of the amine salt 3101 and the raw material 3102 .

[0158] The use of the radial type impeller 3321, the axial type impeller 3322 and the baffle 340 can further increase the gas holdup when the gaseous raw material 3102 is injected and mixed into the amine salt 3101. Therefore, the reaction rate in the reactor 310 can be further increased.

[0159] The batch reactor 3100 according to the third embodiment of the present invention is used for a reaction between a gaseous state and a slurry state, and can be used in a process for producing xylylene diisocyanate by supplying phosgene, which is a gaseous raw material 3102, to an amine salt in a slurry state 3101.

[0160] Various modifications and comparative examples of this embodiment will be described below. Explanations of the same configurations as in the 3-1 embodiment will be omitted, and only explanations of the different configurations will be given.

[0161] Fig. 14 is a cross-sectional view of a batch reactor according to Example 3-2 of the present invention. Referring to Fig. 14, the impeller 332 of the batch reactor 3200 of Example 3-2 is formed in two stages. The radial type impeller 3321 is provided in one stage at the lower end of the rotating shaft 331, and the axial type impeller 3322 is provided in one stage on the rotating shaft 331 above the radial type impeller 3321. That is, the radial type impeller 3321 is provided in the first stage, and the axial type impeller 3322 is provided in the second stage.

[0162] Although not separately illustrated, an axial type impeller may be provided with one stage at the lower end of the rotating shaft, and a radial type impeller may be provided with one stage on the rotating shaft above the axial type impeller.

[0163] In the 3-2 embodiment, the radial type impeller 3321 is rotated above the gaseous raw material 3102 injected from the injection port 321 of the sparger 320, and causes the amine salt 3101 to flow laterally. Therefore, the gaseous raw material 3102 injected from the injection port 321 of the sparger 320 is mixed with the amine salt 3101 while flowing laterally due to the lateral flow of the amine salt 3101.

[0164] The one-stage axial type impeller 3322 is driven above the radial type impeller 3321 to cause the amine salt 3101 to flow in the axial direction. Thus, the partially mixed gaseous raw material 3102 and the gaseous raw material 3102 are further mixed with the amine salt 3101 while flowing in the axial direction due to the axial flow of the amine salt 3101.

[0165] In this way, the combined use of one stage of radial type impeller 3321 and one stage of axial type impeller 3322 increases the gas holdup when the gaseous raw material 3102 is injected and mixed into the amine salt 3101. In conclusion, the distribution performance of phosgene to the reactants in a slurry state can be improved in the phosgenation reaction that is carried out by supplying the raw material 3102 phosgene to the amine salt 3101. Therefore, the reaction rate in the reactor 310 can be increased.

[0166] Fig. 15 is a cross-sectional view of a batch reactor according to Comparative Example 3. Referring to Fig. 15, in a batch reactor 3300 of Comparative Example 3, an agitator 3330 has one radial type impeller 3323 attached to a rotating shaft 331.

[0167] The radial type impeller 3323 is rotationally driven above the gaseous raw material 3102 injected by the sparger 320, and causes the amine salt 3101 to flow laterally. Therefore, the gaseous raw material 3102 injected from the injection port 321 of the sparger 320 is mixed with the amine salt 3101 while flowing in the circumferential direction due to the circumferential flow of the amine salt 3101.

[0168] In comparison with Examples 3-1 and 3-2, Comparative Example 3 forms only one lateral flow with respect to the amine salt 3101, making it difficult to form an axial flow.

[0169] Table 3 shows the gas collection efficiency (%) for Example 3-1, Example 3-2 and Comparative Example 3.

[0170] [Table 3]

[0171] Example 3-1 13, an amine salt 3101 was placed in the batch reaction apparatus 3100, and phosgene as a raw material 3102 was supplied to the amine salt 3101 by a sparger 320 to produce xylylene diisocyanate. In Example 3-1, a five-stage impeller 332 was used. The agitator 330 rotated at 50 to 500 rpm.

[0172] Example 3-2 14, an amine salt 3101 was placed in the batch reaction apparatus 3200, and phosgene as a raw material 3102 was supplied to the amine salt 3101 by a sparger 320 to produce xylylene diisocyanate. In Example 3-2, a two-stage impeller 332 was used. The agitator 3230 rotated at 50 to 500 rpm.

[0173] Comparative Example 3 15, an amine salt 3101 was placed in a batch reaction apparatus 3300, and phosgene as a raw material 3102 was supplied to the amine salt 3101 by a sparger 320 to produce xylylene diisocyanate. In the comparative example, a single-stage radial type impeller 3323 was used. The agitator 3330 rotated at 50 to 500 rpm.

[0174] Experimental Example 3 The gas collection efficiency was measured for Example 3-1, Example 3-2, and Comparative Example 3. Example 3-1 had a gas collection efficiency of over 10% over a reaction time of 4.5 hours, Example 3-2 had a gas collection efficiency of over 5.2% over a reaction time of 5.2 hours, while Comparative Example 3 had a gas collection efficiency of 4.7% over a reaction time of 7.8 hours.

[0175] That is, Examples 3-1 and 3-2 show an increased gas collection rate despite the shorter reaction time compared to Comparative Example 3. Therefore, Examples 3-1 and 3-2 increase the amount of phosgene in the raw material 3102 participating in the reaction compared to Comparative Example 3, thereby improving the reactivity of aliphatic isocyanate using phosgene.

[0176] A fourth embodiment of the present invention will now be described.

[0177] Fig. 16 is a cross-sectional view of a batch reactor according to Example 4-1 of the present invention. Referring to Fig. 16, the batch reactor 4100 of Example 4-1 includes a reactor 410 for accommodating a slurry-like amine salt 4101 produced in a one-stage salt-forming reaction, an agitator 420, and a sparger 430 for supplying a gaseous raw material 4102 into the reactor 410.

[0178] For example, the reactor 410 includes a cylindrical side wall 411, a bottom 412 and a cover 413 which respectively define the upper and lower sides of the side wall 411 to form a reaction space. The bottom 412 and the cover 413 are formed with curved surfaces which bulge at the bottom and top, allowing the slurry amine salt 4101 and the gaseous raw material 4102 to flow and be effectively mixed.

[0179] The agitator 420 includes a rotating shaft 421 installed in the height direction of the reactor 410, and an impeller 422 installed on the rotating shaft 421 to agitate the amine salt 4101 and the raw material 4102. The rotating shaft 421 is rotatably installed on the cover 413 of the reactor 410, with its lower end facing the bottom 412, and can be driven by an external driving motor (not shown).

[0180] For example, the impeller 422 includes a radial type impeller 4221 and an axial type impeller 4222. The radial type impeller 4221 generates a flow in a lateral direction perpendicular to the rotation axis 421 to crush and disperse the gaseous raw material 4102 supplied in the amine salt 4101. The axial type impeller 4222 generates a flow in the same axial direction as the rotation axis 421 to crush and disperse the gaseous raw material 4102 supplied in the amine salt 4101.

[0181] In the 4-1 embodiment, the radial type impeller 4221 is provided in one stage at the lower end of the rotating shaft 421, and the axial type impeller 4222 is provided in one stage on the rotating shaft 421 above the radial type impeller 4221. Although not shown, the axial type impeller 4222 may be installed in more stages depending on the height of the rotating shaft 421 and the reactor 410.

[0182] The sparger 430 is provided in a plurality along one of the axial direction of the agitator 420 and the circumferential direction of the reactor 410, and is formed and installed to supply the gaseous raw material 4102. According to the 4-1 embodiment, the plurality of spargers 430 are installed on the side wall 411 of the reactor 410 at intervals (D) set along the axial direction of the agitator 420.

[0183] The sparger 430 includes a pipe 431 and a bubble forming section 432. The pipe 431 is installed in the side wall section 411 of the reactor 410 such that the length direction of the pipe 431 intersects with the axial direction of the agitator 420. For example, the pipe 431 is installed in the side wall section 411 at a set angle θ.

[0184] The bubble forming unit 432 is provided with a plurality of nozzles at the end of the pipe 431, and supplies the gaseous raw material 4102 in a bubble state toward the impeller 422. A plurality of such spargers 430 are provided in the reactor 10 along the axial direction, so that the gaseous raw material 4102 can be uniformly distributed in the axial direction.

[0185] When a plurality of impellers 422 are provided, the sparger 430 may be installed corresponding to the impeller 422. Therefore, each impeller 422 can uniformly distribute the gaseous raw material 4102 supplied by each sparger 430 even within the interval (D), and can further uniformly distribute the gaseous raw material 4102 over the entire axial direction of the reactor 410.

[0186] Meanwhile, the radial type impeller 4221 is rotated around the gaseous raw material 4102 supplied to the bubble forming section 432 of the sparger 430, and causes the amine salt 4101 to flow laterally. Therefore, the gaseous raw material 4102 supplied to the bubble forming section 432 of the sparger 430 is mixed with the amine salt 4101 while flowing laterally due to the lateral flow of the amine salt 4101.

[0187] Axial type impeller 4222 is driven above radial type impeller 4221 to flow amine salt 4101 in the axial direction. Thus, partially mixed gaseous raw material 4102 and gaseous raw material 4102 are further mixed with amine salt 4101 while flowing in the axial direction due to the axial flow of amine salt 4101.

[0188] In this manner, the multiple spargers 430 arranged in the axial direction uniformly distribute and supply the gaseous raw material 4102 to the amine salt 4101, thereby increasing the gas holdup within a certain time. In conclusion, in the phosgenation reaction that is carried out by supplying the raw material 4102, phosgene, to the amine salt 4101, the distribution performance of phosgene to the amine salt 101 in a slurry state can be improved. Therefore, the reaction rate in the reactor 410 can be increased.

[0189] Meanwhile, the reactor 410 further includes a baffle 440 disposed alongside the rotation shaft 421 and installed on the inner surface, i.e., the inner side, of the side wall 411. For example, the baffle 440 may be formed in a plate shape having a set width and height, or in a rod shape having a set diameter and length.

[0190] The baffle 440 generates a vortex in the flowing amine salt 4101 when the impeller 422 is driven, thereby enabling the amine salt 4101 and the raw material 4102 to be mixed more uniformly over the entire height direction of the reactor 410 .

[0191] A plurality of baffles 440 are provided inside the reactor 410 along the circumferential direction, and repeatedly form vortexes in the circumferential direction, enabling the amine salt 4101 and the raw material 4102 to be mixed more uniformly over the entire circumferential area.

[0192] In addition, the baffle 440 is provided in the vortex region generated by the rotational drive of the radial type impeller 4221 and the axial type impeller 4222 , and can directly act on the mixing of the amine salt 4101 and the raw material 4102 .

[0193] In addition to the sparger 430, the use of the radial type impeller 4221, the axial type impeller 4222, and the baffle 440 can further increase the gas holdup when the gaseous raw material 4102 is injected and mixed into the amine salt 4101. Therefore, the reaction rate in the reactor 410 can be further increased.

[0194] The batch reactor 4100 according to the fourth embodiment of the present invention is used for a reaction between a gaseous state and a slurry state, and can be used in a process for producing xylylene diisocyanate by supplying phosgene, which is a gaseous raw material 4102, to an amine salt 4101.

[0195] Various modifications and comparative examples of this embodiment will be described below. Explanations of the same configurations as in the 4-1 embodiment will be omitted, and explanations of the different configurations will be given.

[0196] 17 is a cross-sectional view of a batch reactor according to Example 4-2 of the present invention. Referring to FIG. 17, in the batch reactor 4200 of Example 4-2, a plurality of spargers 4230 are provided, each of which includes an induction passage 434 and a bubble forming section 435.

[0197] The induction path 434 is formed penetrating within the rotating shaft 421 of the agitator 420 to supply the gaseous raw material 4102. The bubble forming unit 435 passes through the rotating shaft 421 and is connected to the induction path 434 to supply the gaseous raw material 4102 to the amine salt 4101 in the form of bubbles.

[0198] The impeller 422 is provided in a plurality of stages at a set interval (D2) on the rotating shaft 421, and includes a radial type impeller 4221 and an axial type impeller 4222 provided in sequence from the bottom. In this case, the bubble forming portion 435 may be formed in a plurality of stages corresponding to the impeller 422 and the interval (D2).

[0199] That is, the first bubble forming portion 4351 is provided below the radial type impeller 4221 and supplies the gaseous fuel 4102 , and the second bubble forming portion 4352 is provided below the next axial type impeller 4222 and supplies the gaseous fuel 4102 .

[0200] The bubble forming unit 435 is provided with a plurality of nozzles on the rotating shaft 421, and supplies the gaseous raw material 4102 in a bubble state toward the lower side of the impeller 422. In the sparger 4230, the first and second bubble forming units 4351 and 4352 are provided in the reactor 410 along the axial direction, and allow the gaseous raw material 4102 to be uniformly distributed in the axial direction.

[0201] As described above, the first and second bubble forming parts 4351 and 4352 of the sparger 4230 arranged in the axial direction uniformly distribute and supply the gaseous raw material 4102 to the amine salt 4101, thereby increasing the gas holdup within a certain time. In conclusion, the distribution performance of phosgene to the amine salt in a slurry state can be improved in the phosgenation reaction that is carried out by supplying the raw material 4102, phosgene, to the amine salt 4101. Therefore, the reaction rate in the reactor 410 can be increased.

[0202] 18 is a cross-sectional view of a batch reactor according to Example 4-3 of the present invention. Referring to FIG. 18, in the batch reactor 4300 of Example 4-3, a plurality of spargers 4330 are provided and installed on the side wall 411 of the reactor 410 at intervals along the circumferential direction of the reactor 410 at the lower end of the reactor 410.

[0203] The sparger 4330 includes a pipe 431 and a bubble forming section 432. The pipe 431 is installed in the side wall section 411 of the reactor 410 such that the length direction of the pipe 431 intersects with the axial direction of the agitator 420.

[0204] The bubble forming unit 432 is provided with a plurality of nozzles at the end of the pipe 431, and supplies the gaseous raw material in a gaseous state to the lower end of the reactor 410 below the impeller. A plurality of such spargers 4330 are provided in the reactor 410 along the circumferential direction, so that the gaseous raw material can be uniformly distributed in the circumferential direction.

[0205] On the other hand, the impeller 422 is rotated above the gaseous raw material 4102 supplied to the bubble forming section 432 of the sparger 4330, and causes the amine salt 4101 to flow. Therefore, the gaseous raw material 4102 supplied to the bubble forming section 432 of the sparger 4330 is mixed with the amine salt 4101 while flowing due to the flow of the amine salt 4101.

[0206] In this way, the multiple spargers 4330 arranged in the circumferential direction uniformly distribute and supply the gaseous raw material 4102 to the amine salt 4101 in the circumferential direction, thereby increasing the gas holdup within a certain time. In conclusion, in the phosgenation reaction that is carried out by supplying the raw material 4102 phosgene to the amine salt 4101, the distribution performance of phosgene to the amine salt in a slurry state can be improved. Therefore, the reaction rate in the reactor 410 can be increased.

[0207] Fig. 19 is a cross-sectional view of a batch reactor according to Comparative Example 4. Referring to Fig. 19, in the batch reactor 4400 of Comparative Example 4, a sparger 4430 is formed in a ring type having an injection port 4431, and is disposed below the impeller 422 to supply a gaseous raw material 4102 to an amine salt 4101.

[0208] The impeller 422 is rotated above the gaseous raw material 4102 injected from the sparger 4430, and causes the amine salt 4101 to flow. Therefore, the gaseous raw material 4102 injected from the injection port 4431 of the sparger 4430 is mixed with the amine salt 4101 while flowing due to the flow of the amine salt 4101. Compared with Examples 4-1, 4-2, and 4-3, Comparative Example 4 has a lower distribution performance of the gaseous raw material 4102 relative to the amine salt 4101.

[0209] 20 is a cross-sectional view of a batch reactor according to Example 4-4 of the present invention. Referring to FIG. 20, in the batch reactor 4500 of Example 4-4, two spargers 4530 are provided and installed on the side wall 411 of the reactor 410 at the lower end of the reactor 410.

[0210] The sparger 4530 is of a sintered porous type. The sintered porous type sparger 4530 forms holes in the entire length range within the reactor 410, so that the gaseous raw material 4102 can be uniformly distributed in the circumferential direction.

[0211] In the agitator of the present invention, the impeller may be a radial type impeller or an axial type impeller installed in the lower stage, and one or more impellers of the same or different types may be installed above it. Also, the impeller in the agitator may be installed alternately up to n stages where radial type impellers and axial type impellers are required. Various drawings corresponding to such cases are omitted.

[0212] Table 4 shows the gas collection efficiencies for Example 4-1, Example 4-2, Example 4-3, Example 4-4 and Comparative Example 4.

[0213] [Table 4]

[0214] Example 4-1 Amine salt 4101 was placed in a batch reactor 4100 in Fig. 16, and phosgene, a gaseous raw material 4102, was supplied to the amine salt 4101 by a sparger 430 to produce xylylene diisocyanate. In Example 4-1, a two-stage impeller 432 was used, and a pipe-shaped sparger 430 was used in two stages along the axial direction. The agitator 420 rotated at 50 to 500 rpm.

[0215] Example 4-2 17, an amine salt 4101 was placed in the batch reaction apparatus 4200, and phosgene, which was a gaseous raw material 4102, was supplied to the amine salt 4101 by a sparger 4230 to produce xylylene diisocyanate. In Example 4-2, a two-stage impeller 422 was used, and a guide path 434 formed in a rotating shaft 421 was provided with two stages of bubble forming parts 435. The agitator 420 rotated at 50 to 500 rpm.

[0216] Example 4-3 Amine salt 4101 was placed in a batch reaction apparatus 4300 shown in Fig. 18, and phosgene in the gaseous raw material 4102 was supplied to the amine salt 4101 by a sparger 4330 to produce xylylene diisocyanate. In Example 4-3, a two-stage impeller 422 was used, and two pipe-shaped spargers 4330 were used along the circumferential direction. The agitator 420 rotated at 50 to 500 rpm.

[0217] Example 4-4 Amine salt 4101 was placed in a batch reactor 4500 in Fig. 20, and phosgene, a gaseous raw material 4102, was supplied to the amine salt 4101 by a sparger 4530 to produce xylylene diisocyanate. In Example 4-4, a two-stage impeller 422 was used, and two sintered porous sparger 4530 were used along the circumferential direction. The agitator 420 rotated at 50 to 500 rpm.

[0218] Comparative Example 4 19, an amine salt 4101 was placed in the batch reaction apparatus 4400, and phosgene in the gaseous raw material 4102 was supplied to the amine salt 4101 by a sparger 4430 to produce xylylene diisocyanate. In Comparative Example 4, a two-stage impeller 432 was used, and one ring-shaped sparger 4430 was used below the impeller 422. The agitator 420 rotated at 50 to 500 rpm.

[0219] Experimental Example 4 The gas collection efficiencies were measured for Example 4-1, Example 4-2, Example 4-3, Example 4-4, and Comparative Example 4. Example 4-1 had a gas collection rate of more than 10% for a reaction time of 13.9 hours, Example 4-2 had a gas collection rate of more than 15% for a reaction time of 9.5 hours, Example 4-3 had a gas collection rate of more than 10% for a reaction time of 11.2 hours, Example 4-4 had a gas collection rate of more than 15% for a reaction time of 10.6 hours, while Comparative Example 4 had a gas collection rate of more than 5% for a reaction time of 14.3 hours.

[0220] That is, Examples 4-1, 4-2, 4-3, and 4-4 show increased gas collection efficiency despite the shorter reaction time compared to Comparative Example 4. Therefore, Examples 4-1, 4-2, 4-3, and 4-4 can increase the amount of phosgene in the raw material 4102 participating in the reaction compared to Comparative Example 4, thereby improving the reactivity of aliphatic isocyanate using phosgene.

[0221] Although the preferred embodiments of the present invention have been described above, the present invention is not limited to these, and various modifications and variations can be made within the scope of the claims, the description of the invention, and the accompanying drawings, and it is to be understood that these also fall within the scope of the present invention. [Explanation of symbols]

[0222] 110 Reactor 111 Side wall 112 Bottom 113 Lid 1100 Batch Reactor 1101 Liquid solvents 1102 Gaseous materials 120 Sparger 121 Nozzle 130 Stirrer 131 Rotational axis 132 Impeller 1321 Radial type impeller 1322 Axial type impeller

Claims

1. a reactor containing the amine salt in slurry form; A sparger for supplying a gaseous raw material, phosgene, into the reactor; and An agitator having an impeller on a rotating shaft installed in the height direction of the reactor to agitate the amine salt and phosgene to produce xylylene diisocyanate. Including, The impeller is A batch reactor arranged in a plurality of stages on the rotating shaft.

2. The impeller is 2. The batch reactor of claim 1, which is formed with at least one of a radial type impeller and an axial type impeller.

3. The impeller is a radial type impeller provided in one stage at the lower end of the rotating shaft; and 2. The batch reactor of claim 1, further comprising an axial type impeller provided in at least two stages on the rotating shaft above the radial type impeller.

4. The impeller is a radial type impeller provided in one stage at the lower end of the rotating shaft; and 2. The batch reactor of claim 1, further comprising an axial type impeller provided in one stage on the rotating shaft above the radial type impeller.

5. The sparger is 2. The batch reaction apparatus according to claim 1, wherein the batch reaction apparatus is installed so as to supply a gaseous raw material in an axial direction of the agitator and in a circumferential direction of the reactor.

6. The sparger is A pipe installed on the side wall of the reactor in a direction perpendicular to the axial direction of the agitator; and 6. The batch reactor according to claim 5, further comprising a bubble forming section provided with a plurality of nozzles at an end of the pipe and supplying a gaseous raw material in a bubble state toward the impeller.

7. a reactor containing the amine salt in slurry form; A stirrer having an impeller on a rotating shaft installed in the height direction within the reactor; and A sparger for supplying a gaseous raw material to the amine salt in the reactor so that the raw material is distributed to the amine salt by the operation of the agitator. Including, The sparger is A batch reaction apparatus including a plurality of batch reaction apparatuses provided along one of the axial direction of the agitator and the circumferential direction of the reactor, and supplying a gaseous raw material.

8. The sparger is 8. The batch reactor according to claim 7, wherein the agitator is installed on the side wall of the reactor at set intervals along the axial direction of the agitator.

9. The sparger is A pipe installed in the reactor, the length of which intersects with the axial direction of the agitator; and 8. The batch reactor according to claim 7, further comprising a bubble forming section provided at an end of the pipe for supplying a gaseous raw material in a bubble state toward the impeller.

10. The sparger is A guideway formed through the rotating shaft; and 8. The batch reactor according to claim 7, further comprising a bubble forming section that passes through the rotating shaft and is connected to the guide path to supply the gaseous raw material in a bubble state.

11. The impeller is The rotary shaft is provided with a plurality of stages, The bubble forming section includes:

11. The batch reactor of claim 10, wherein the impeller is disposed below each of the impellers.

12. The sparger is 8. The batch reactor according to claim 7, wherein the reactor is provided on a side wall of the reactor at set intervals along a circumferential direction of the reactor at a lower end of the reactor.

13. The sparger is a pipe disposed in the reactor with its length oriented in the direction of the diameter of the reactor; and The batch reactor according to claim 12, further comprising a bubble forming section provided at an end of the pipe for supplying a gaseous raw material in a bubble state downward to the impeller.

14. The batch reactor according to claim 7, wherein the raw material phosgene is supplied to produce xylylene diisocyanate.

15. The sparger is 13. The batch reaction apparatus according to claim 12, which is a sintered porous type that is installed in the reactor such that its length direction intersects with the axial direction of the agitator and supplies the gaseous raw material in a bubble state toward the impeller.

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