Batch reactor and method for producing aliphatic isocyanates

Abstract

A method for producing an aliphatic isocyanate according to an embodiment of the present invention includes a first step of feeding an aliphatic amine and an organic solvent into a reactor, a second step of supplying gaseous hydrogen chloride into the reactor using a sparger, and a third step of stirring the aliphatic amine, the organic solvent, and the hydrogen chloride using a stirrer installed in the reactor, the third step being performed by stirring the stirrer at a temperature of 500 to 4000 (W / m 3 ) stirring force is controlled.

Description

[Technical field]

[0001] The present invention relates to a batch reactor and a method for producing an aliphatic isocyanate. [Background technology]

[0002] Aliphatic isocyanates are obtained by a first stage of a salt-forming reaction in which an amine is reacted with hydrogen chloride, and a second stage of a phosgenation reaction in which the amine salt produced in the salt-forming reaction is reacted with phosgene.

[0003] The amine salt is produced by reaction of an aliphatic amine with hydrogen chloride provided in an organic solvent, using a conventional batch reactor.

[0004] In this case, the batch reactor generates an amine salt by injecting gaseous hydrogen chloride into the aliphatic amine and organic solvent fed into the reactor and mixing them with an agitator. The gas holdup rate of gaseous hydrogen chloride and the amine conversion rate can be adjusted by controlling the agitation power of the agitator provided in the batch reactor.

[0005] Aliphatic isocyanates are produced by reacting the amine salt produced in the first stage with phosgene, using a conventional batch reactor.

[0006] In this case, the batch reactor produces an aliphatic isocyanate by injecting gaseous phosgene into the amine salt fed into the reactor and mixing with an agitator. The conversion rate of the amine salt can be adjusted by controlling the agitation force of the agitator provided in the batch reactor. Summary of the Invention [Problem to be solved by the invention]

[0007] One aspect of the present invention provides a batch reactor and a method for producing an aliphatic isocyanate, which improves the yield of an isocyanate by adjusting the stirring power to improve the amine conversion rate or the amine salt conversion rate. [Means for solving the problem]

[0008] A batch reactor according to an embodiment of the present invention includes a reactor into which an aliphatic amine and an organic solvent are introduced, a sparger that supplies gaseous hydrogen chloride into the reactor, and an agitator that is installed in the reactor and agitates the aliphatic amine, the organic solvent, and the hydrogen chloride, and the agitator has a stirring power of 500 to 4000 (W / m 3 ).

[0009] The stirring power of the stirrer is 780 to 3570 (W / m 3 ) may also be used.

[0010] The agitator may include a rotating shaft provided in the height direction of the reactor, and an impeller provided on the rotating shaft for agitating the aliphatic amine, the organic solvent, and the hydrogen chloride.

[0011] The agitator may have a radial type impeller or an axial type impeller provided at the lower end of the rotating shaft, and may have one or more impellers of the same type or different types provided on the impeller at the lower end.

[0012] The agitator can be provided with the radial type impeller and the axial type impeller alternately up to the required n stages.

[0013] The sparger may be installed in the lower part of the agitator upward from the bottom of the reactor and may have a plurality of injection ports so that gaseous hydrogen chloride can be injected from the lower part of the agitator.

[0014] The sparger is bent from the bottom of the agitator and has a plurality of nozzles corresponding to the rotation range of the agitator, and the plurality of nozzles can inject gaseous hydrogen chloride into the aliphatic amine and liquid organic solvent.

[0015] A method for producing an aliphatic isocyanate according to an embodiment of the present invention includes a first step of feeding an aliphatic amine and an organic solvent into a reactor, a second step of feeding gaseous hydrogen chloride into the reactor using a sparger, and a third step of stirring the aliphatic amine, the organic solvent, and the hydrogen chloride using a stirrer, the third step being performed by stirring the stirrer at a temperature of 500 to 4000 (W / m 3 ) stirring force is controlled.

[0016] In the third stage, the agitator is operated at 780 to 3570 (W / m 3 ) stirring force is controlled.

[0017] According to another embodiment of the present invention, a batch reactor includes a reactor containing a slurry of an amine salt, a sparger for supplying gaseous phosgene into the reactor, and an agitator for agitating the amine salt and the phosgene, the agitator having a stirring force of 500 to 10,000 (W / m 3 ).

[0018] The stirring power of the stirrer is 1560 to 3170 (W / m 3 ) may also be used.

[0019] The agitator may include a rotating shaft provided in the height direction of the reactor, and an impeller provided on the rotating shaft for agitating the amine salt and phosgene.

[0020] The agitator may have a radial type impeller or an axial type impeller at the lower end of the rotating shaft, and may have one or more impellers of the same type or different types on the impeller at the lower end.

[0021] The agitator can be provided with the radial type impeller and the axial type impeller alternately up to the required n stages.

[0022] The spargers are provided in a plurality of directions along one of the axial direction of the agitator and the circumferential direction of the reactor, and can supply gaseous phosgene.

[0023] The sparger may include a pipe provided on a side wall of the reactor in a direction intersecting the axial direction of the agitator, and a plurality of nozzles provided at an end of the pipe for supplying gaseous phosgene in a bubble state toward the impeller.

[0024] A method for producing an aliphatic isocyanate according to another embodiment of the present invention includes a first step of preparing a reactor containing a slurry-like amine salt, a second step of supplying gaseous phosgene into the reactor using a sparger, and a third step of stirring the amine salt and the phosgene using an agitator, the third step being performed by stirring the agitator at a temperature of 500 to 10,000 (W / m 3 ) stirring force is controlled.

[0025] In the third stage, the agitator is operated at 1560 to 3170 (W / m 3 ) can be controlled by the stirring force. Effect of the Invention

[0026] In one embodiment, the stirring power of the stirrer is controlled, so that the gas holdup rate of gaseous hydrogen chloride and the surface area per unit volume can be adjusted to control the reactivity, and the particle size of the amine salt particles in the slurry can be adjusted, thereby improving the conversion rate of the amine, and thereby improving the yield of the final product, isocyanate.

[0027] In addition, in one embodiment, the stirring power of the stirrer is controlled to improve the reactivity and reaction rate of the phosgenation reaction, thereby improving the amine salt conversion rate and thereby improving the yield of the final product, isocyanate. [Brief description of the drawings]

[0028] [Figure 1] FIG. 1 is a cross-sectional view of a batch reaction apparatus according to a first embodiment of the present invention. [Diagram 2]1 is a flowchart of a method for producing an aliphatic isocyanate according to a first embodiment of the present invention. [Diagram 3] FIG. 2 is a cross-sectional view of a batch reactor according to a second embodiment of the present invention. [Figure 4] 4 is a flowchart of a method for producing an aliphatic isocyanate according to a second embodiment of the present invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0029] Hereinafter, with reference to the accompanying drawings, an embodiment of the present invention will be described in detail so that a person having ordinary skill in the art to which the present invention pertains can easily carry out the embodiment. However, the present invention can be realized in various different forms and is not limited to the embodiments described herein. In the drawings, parts that are not necessary for the explanation of the present invention are omitted in order to clearly explain the present invention, and the same reference numerals are used throughout the specification to refer to the same or similar components.

[0030] 1 is a cross-sectional view of a batch 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 that contains an aliphatic amine and a liquid organic solvent 101, a sparger 20 that supplies gaseous hydrogen chloride 102 into the reactor 10, and an agitator 30.

[0031] As an example, the reactor 10 includes a cylindrical side wall 11, and a bottom 12 and a cover 13 that respectively form the upper and lower sides of the side wall 11 to form a reaction space. The bottom 12 and the cover 13 are formed into convex curved surfaces on the lower and upper sides, so that the aliphatic amine and liquid organic solvent 101 and gaseous hydrogen chloride (HCl) 102 can flow and be effectively mixed.

[0032] The sparger 20 is provided below the agitator 30 and faces upward from the bottom 12 of the reactor 10, and is provided with a plurality of injection ports 21 so that gaseous hydrogen chloride can be injected from the bottom of the agitator 30.

[0033] The sparger 20 is bent from the lower part of the agitator 30 and has a plurality of injection ports 21 corresponding to the rotation range of the agitator 30. In the sparger 20, the plurality of injection ports 21 make it possible to uniformly inject gaseous hydrogen chloride 102 into the aliphatic amine and liquid organic solvent 101.

[0034] The agitator 30 includes a rotating shaft 31 provided in the height direction of the reactor 10, an impeller 32 provided on the rotating shaft 31 for stirring the aliphatic amine and organic solvent 101 and the hydrogen chloride 102, and a motor M for driving the rotating shaft 31. When driven by the motor M, the rotating shaft 31 is rotatably provided on the lid 13 of the reactor 10, and faces the bottom 12 at its lower end.

[0035] The impeller 32 includes a radial type impeller 321 and an axial type impeller 322. The radial type impeller 321 generates a flow in a lateral direction perpendicular to the rotation axis 31 to crush and disperse the gaseous hydrogen chloride 102 supplied in the aliphatic amine and the liquid organic solvent 101. The axial type impeller 322 generates a flow in the same axial direction as the rotation axis 31 to crush and disperse the gaseous hydrogen chloride 102 supplied in the aliphatic amine and the liquid organic solvent 101.

[0036] In the first embodiment, the radial type impeller 321 is provided in one stage at the lower end of the rotating shaft 31, and the axial type impeller 322 is provided in one stage on the rotating shaft 31 above the radial type impeller 321. That is, the radial type impeller 321 is provided in the first stage, and the axial type impeller 322 is provided in the second stage.

[0037] In the agitator of the present invention, the impeller may be provided with a radial type impeller or an axial type impeller at the lower end, and one or more impellers of the same or different types may be provided thereon. In addition, in the agitator, the impeller may be provided with radial type impellers and axial type impellers alternately up to the required n stages. Various drawings corresponding to this case will be omitted.

[0038] The radial type impeller 321 is rotationally driven above the gaseous hydrogen chloride 102 injected from the nozzle 21 of the sparger 20, and causes the aliphatic amine and organic solvent 101 to flow laterally. Therefore, the gaseous hydrogen chloride 102 injected from the nozzle 21 of the sparger 20 is mixed with the aliphatic amine and organic solvent 101 while flowing laterally due to the lateral flow of the aliphatic amine and organic solvent 101.

[0039] The axial type impeller 322 is driven above the radial type impeller 321 to axially flow the aliphatic amine and organic solvent 101. Thus, the partially mixed gaseous hydrogen chloride 102 is further mixed with the aliphatic amine and organic solvent 101 while flowing axially due to the axial flow of the aliphatic amine and organic solvent 101.

[0040] The aliphatic amine and organic solvent 101 are mixed with hydrogen chloride 102 to cause a salt-forming reaction to proceed, producing an amine salt. The amine salt, which is the product, is in the form of particles having a diameter of several to several tens of μm, and as the reaction proceeds, it changes into a slurry-like form that disperses in the aliphatic amine and organic solvent 101.

[0041] In this way, the combined use of the radial type impeller 321 and the axial type impeller 322 increases the gas holdup when gaseous hydrogen chloride 102 is injected into and mixed with the aliphatic amine and organic solvent 101. Therefore, the reaction rate in the reactor 10 can be increased. In conclusion, a uniform product can be produced in a shorter time in the reaction of mixing the aliphatic amine and organic solvent 101 with hydrogen chloride 102 to produce a slurry, thereby increasing productivity and improving the stability of the product quality.

[0042] Meanwhile, the reactor 10 further includes a baffle 40 disposed alongside the rotation shaft 31 and provided on the inner surface, i.e., the inner surface, of the side wall 11. For example, the baffle 40 may be formed in a plate shape having a set width and height, or in a rod shape having a set diameter and length.

[0043] When the impeller 32 is driven, the baffle 40 generates a vortex in the flowing aliphatic amine and organic solvent 101, making it possible to mix the aliphatic amine and organic solvent 101 and the hydrogen chloride 102 more uniformly over the entire heightwise area of ​​the reactor 10.

[0044] A plurality of baffles 40 are provided inside the reactor 10 along the circumferential direction, and repeatedly form vortex flows in the circumferential direction, enabling the aliphatic amine and organic solvent 101 and the hydrogen chloride 102 to be mixed more uniformly over the entire circumferential area.

[0045] In addition, the baffle 40 is provided in the vortex region generated by the rotational drive of the radial type impeller 321 and the axial type impeller 322, and can directly affect the mixing of the aliphatic amine and organic solvent 101 with the hydrogen chloride 102.

[0046] The use of the radial type impeller 321, the axial type impeller 322 and the baffle 40 can further increase the gas holdup when gaseous hydrogen chloride 102 is injected and mixed into the aliphatic amine and the organic solvent 101. Therefore, the reaction rate in the reactor 10 can be further increased.

[0047] The agitator 20 is driven and controlled by a motor M. The agitator 30 can adjust the gas collection rate of the gaseous hydrogen chloride 102 and the surface area per unit volume by controlling the agitation power. Therefore, the reactivity of the aliphatic amine and the organic solvent 101 with the hydrogen chloride 102 is adjusted, and the particle size of the slurry-like amine salt particles is adjusted. This improves the conversion rate of the amine and increases the yield of the final product, the aliphatic isocyanate.

[0048] The batch reactor 100 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 an aliphatic isocyanate by supplying gaseous hydrogen chloride 102 to an aliphatic amine and a liquid organic solvent 101.

[0049] 2 is a flow chart of a method for producing an aliphatic isocyanate according to an embodiment of the present invention. Referring to FIG. 2, the method produces an aliphatic isocyanate using a batch reactor 100 according to the first embodiment.

[0050] The method for producing an aliphatic isocyanate includes a first stage ST1, a second stage ST2, and a third stage ST3. In the first stage ST1, an aliphatic amine and an organic solvent 101 are charged into a reactor 10. In the second stage ST2, gaseous hydrogen chloride 102 is supplied into the reactor 10 by a sparger 20. In the third stage ST3, the aliphatic amine and the organic solvent 101 and the hydrogen chloride 102 are stirred by a stirrer 30.

[0051] In the third stage ST3, the motor M can be controlled to control the stirring force of the stirrer 30. For example, in the third stage ST3, the stirrer 30 is set to a stirring force of 500 to 4000 (W / m 3The stirring power is controlled at 500W / m 3 If the stirring force is less than 4000W / m, the salt formation reaction will be difficult to proceed due to excessively slow stirring. 3 If the stirring speed exceeds this value, the effect of improving the reactivity is very small compared to excessively fast stirring.

[0052] The stirring power of the stirrer 30 is 780 to 3570 (W / m 3 ) This range allows for a high reaction rate for salt formation compared to the stirring force applied.

[0053] Table 1 shows the stirring power and amine conversion rate for Example 1-1, Example 1-2, Example 1-3, and Comparative Example 1. [Table 1]

[0054] Example 1-1 An aliphatic amine and an organic solvent 101 were placed in a batch reactor 100 shown in FIG. 1, and hydrogen chloride 102 was supplied through a sparger 20 to produce an aliphatic isocyanate. In the first embodiment, the stirring power of the stirrer 30 was 9730 W / m 3 It was.

[0055] Example 1-2 An aliphatic amine and an organic solvent 101 were placed in a batch reactor 100 shown in FIG. 1, and hydrogen chloride 102 was supplied through a sparger 20 to produce an aliphatic isocyanate. In the second embodiment, the stirring power of the stirrer 30 was 3570 W / m 3 It was.

[0056] Example 1-3 An aliphatic amine and an organic solvent 101 were placed in a batch reactor 100 shown in FIG. 1, and hydrogen chloride 102 was supplied through a sparger 20 to produce an aliphatic isocyanate. In the third embodiment, the stirring power of the stirrer 30 was 780 W / m 3 It was.

[0057] Comparative Example 1 An aliphatic amine and an organic solvent 101 were placed in a batch reactor 100 shown in FIG. 1, and hydrogen chloride 102 was supplied through a sparger 20 to produce an aliphatic isocyanate. In the comparative example, the stirring power of the stirrer 30 was 500 W / m 3 It was less than.

[0058] Experimental Example 1 In Example 1-1, Example 1-2, Example 1-3, and Comparative Example 1, the amine conversion rate (%) relative to the stirring power was measured. In Example 1-1, the stirring power of the stirrer 30 was 9730 (W / m 3 ), the amine conversion rate (%) is 99.8% or more, and in the first-2 embodiment, the stirring force of the stirrer 30 is 3570 (W / m 3 ), the amine conversion rate (%) is 99.8%, and in the first to third embodiments, the stirring force of the stirrer 30 is 780 (W / m 3 ), the amine conversion rate (%) was 89.5%, and in Comparative Example 1, the stirring force of the stirrer 30 was 500 (W / m 3 ), the amine conversion rate (%) was 82.2%. Therefore, in comparison with Comparative Example 1, Examples 1-1, 1-2, and 1-3 can improve the amine conversion rate and the yield of the final product, aliphatic isocyanate.

[0059] A second embodiment of the present invention will now be described.

[0060] 3 is a cross-sectional view of a batch reactor according to a second embodiment of the present invention. Referring to FIG 3, the batch reactor 2100 of the second embodiment includes a reactor 210 for accommodating a slurry-like amine salt 2101 produced in a salt-forming reaction, a sparger 230 for supplying gaseous phosgene 2102 into the reactor 210, and an agitator 220.

[0061] As an example, the reactor 210 includes a cylindrical side wall 211, and a bottom 212 and a cover 213 that respectively form the upper and lower sides of the side wall 211 to form a reaction space. The bottom 212 and the cover 213 are formed into convex curved surfaces on the lower and upper sides, so that the amine salt in a slurry state 2101 and the phosgene in a gaseous state 2102 can flow and be effectively mixed.

[0062] The agitator 220 includes a rotating shaft 221 provided in the height direction of the reactor 210, an impeller 222 provided on the rotating shaft 221 and for stirring the amine salt 2101 and the phosgene 2102, and a motor M for driving the rotating shaft 221. By driving the motor M, the rotating shaft 221 is rotatably provided on the lid portion 213 of the reactor 210, and faces the bottom portion 212 at its lower end.

[0063] 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 phosgene 2102 supplied in the amine salt 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 phosgene 2102 supplied in the amine salt 2101.

[0064] In the second 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. That is, the radial type impeller 2221 is provided in the first stage, and the axial type impeller 2222 is provided in the second stage.

[0065] In the agitator of the present invention, the impeller may be provided with a radial type impeller or an axial type impeller at the lower end, and one or more impellers of the same or different types may be provided thereon. In addition, in the agitator, the impeller may be provided with radial type impellers and axial type impellers alternately up to the required n stages. Various drawings corresponding to this case will be omitted.

[0066] A plurality of spargers 230 are provided along one of the axial direction of the agitator 220 and the circumferential direction of the reactor 210, and are formed and provided to supply gaseous phosgene 2102. According to the second embodiment, the plurality of spargers 230 are provided on the side wall portion 211 of the reactor 210 at intervals D set along the axial direction of the agitator 220.

[0067] The sparger 230 includes a pipe 231 and a bubble forming section 232. The pipe 231 is provided on the side wall section 211 of the reactor 210 such that the longitudinal direction of the pipe 231 intersects with the axial direction of the agitator 220. As an example, the pipe 231 is provided on the side wall section 211 at a set angle θ.

[0068] The bubble forming unit 232 is provided with a plurality of nozzles at the end of the pipe 231, and supplies gaseous phosgene 2102 in a bubble state toward the impeller 222. A plurality of such spargers 230 are provided in the reactor 210 along the axial direction, so that the gaseous phosgene 2102 can be uniformly distributed in the axial direction.

[0069] When a plurality of impellers 222 are provided, the sparger 230 is provided corresponding to the impeller 222. Therefore, each impeller 222 can uniformly distribute the gaseous phosgene 2102 supplied from each sparger 230 even within the interval D, and can further uniformly distribute the gaseous phosgene 2102 over the entire axial direction of the reactor 210.

[0070] On the other hand, the radial type impeller 2221 is rotationally driven around the gaseous phosgene 2102 supplied from the bubble forming section 232 of the sparger 230, and causes the amine salt 2101 to flow laterally. Therefore, the gaseous phosgene 2102 supplied from the bubble forming section 232 of the sparger 230 is mixed with the amine salt 2101 while flowing laterally due to the lateral flow of the amine salt 2101.

[0071] The axial type impeller 2222 is driven above the radial type impeller 2221 to axially flow the amine salt 2101. Thus, the partially mixed gaseous phosgene 2102 and the gaseous phosgene 2102 are further mixed into the amine salt 2101 while flowing axially due to the axial flow of the amine salt 2101.

[0072] In this way, the multiple spargers 230 arranged in the axial direction uniformly distribute and supply gaseous phosgene 2102 to the amine salt 2101, thereby increasing the gas holdup within a certain time. In conclusion, the distribution performance of phosgene to the amine salt 2101 in a slurry state during the phosgenation reaction that proceeds by supplying phosgene 2102 to the amine salt 2101 can be improved. Therefore, the reaction rate in the reactor 210 can be increased.

[0073] Meanwhile, the reactor 210 further includes a baffle 240 disposed alongside the rotation shaft 221 and provided on the inner surface, i.e., the inner surface, 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.

[0074] The baffle 240 generates a vortex in the flowing amine salt 2101 when the impeller 222 is driven, making it possible to mix the amine salt 2101 and the phosgene 2102 more uniformly over the entire area in the height direction of the reactor 210 .

[0075] A plurality of baffles 240 are provided along the circumferential direction inside the reactor 210 to repeatedly form vortex flows in the circumferential direction, thereby enabling the amine salt 2101 and phosgene 2102 to be mixed more uniformly over the entire circumferential area.

[0076] In addition, the baffle 240 is provided in the 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 amine salt 2101 and the phosgene 2102 .

[0077] 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 gaseous phosgene 2102 is injected and mixed into the amine salt 2101. Therefore, the reaction rate in the reactor 210 can be further increased.

[0078] The agitator 220 is driven and controlled by a motor M. The agitator 220 can improve the reactivity and reaction rate of the phosgenation reaction by controlling the agitation force. This improves the conversion rate of the amine salt and the yield of the final product, the aliphatic isocyanate.

[0079] The batch reactor 2100 according to the second embodiment of the present invention can be used for a reaction between a gaseous state and a slurry state, and can be used in a process for producing an aliphatic isocyanate by supplying gaseous phosgene 2102 to an amine salt 2101.

[0080] 4 is a flow chart of a method for producing an aliphatic isocyanate according to a second embodiment of the present invention. Referring to FIG. 4, the method produces an aliphatic isocyanate using a batch reactor 2100 according to the second embodiment.

[0081] The method for producing an aliphatic isocyanate includes a first stage ST21, a second stage ST22, and a third stage ST23. The first stage ST21 provides a reactor 210 containing a slurry of an amine salt. The second stage ST22 supplies gaseous phosgene 2102 into the reactor 210 using a sparger 230. The third stage ST23 stirs the slurry of the amine salt 2101 and the phosgene 2102 using an agitator 220.

[0082] The third stage ST23 can control the motor M to control the stirring force of the stirrer 220. For example, the third stage ST23 can control the stirring force of the stirrer 220 to 500 to 10,000 (W / m 3 The stirring power is controlled at 500W / m 3 If the stirring force is less than 10000W / m, the phosgenation reaction is difficult to proceed due to excessively slow stirring. 3 If the stirring speed exceeds this value, the effect of improving the reactivity is very small compared to excessively fast stirring.

[0083] The stirring power of the stirrer 220 is 1560 to 31700 (W / m 3 In this range, a high phosgenation reaction rate can be obtained compared to the stirring power input.

[0084] Table 2 shows the stirring power and the amine salt conversion rate for Example 2-1, Example 2-2, Example 2-3, and Comparative Example 2. [Table 2]

[0085] Example 2-1 An amine salt 2101 was placed in a batch reactor 2100 in FIG. 3, and gaseous phosgene 2102 was supplied to the amine salt 2101 by a sparger 230 to produce an aliphatic isocyanate. In Example 2-1, pipe-type spargers 230 were used in two stages along the axial direction. The stirring power of the stirrer 220 was 14200 (W / m 3 ) was.

[0086] Example 2-2 An amine salt 2101 was placed in a batch reactor 2100 in FIG. 3, and gaseous phosgene 2102 was supplied to the amine salt 2101 by a sparger 230 to produce an aliphatic isocyanate. In Example 2-2, pipe-type spargers 230 were used in two stages along the axial direction. The stirring power of the stirrer 220 was 3170 (W / m 3 ) was.

[0087] Example 2-3 An amine salt 2101 was placed in a batch reactor 2100 in FIG. 3, and gaseous phosgene 2102 was supplied to the amine salt 2101 by a sparger 230 to produce an aliphatic isocyanate. In Example 2-3, pipe-type spargers 230 were used in two stages along the axial direction. The stirring power of the stirrer 220 was 1560 (W / m 3 ) was.

[0088] Experimental Example 2 The amine salt conversion rate (%) relative to the stirring power was measured in Example 2-1, Example 2-2, Example 2-3, and Comparative Example 2. In Example 2-1, the stirring power of the stirrer 220 was 14200 (W / m 3 ), the amine salt conversion rate (%) is 99.3%, and in Example 2-2, the stirring force of the stirrer 220 is 3170 (W / m 3 ), the amine salt conversion rate (%) is 99.2%, and in Example 2-3, the stirring force of the stirrer 220 is 1560 (W / m 3 ), the amine salt conversion rate (%) was 97.8%, and in Comparative Example 2, the stirring force of the stirrer 220 was 500 (W / m 3 ), the amine salt conversion rate (%) was 81.12%.

[0089] Therefore, in comparison with Comparative Example 2, Examples 2-1, 2-2, and 2-3 can improve the reactivity and reaction rate of the phosgenation reaction and can improve the amine salt conversion rate, thereby improving the yield of the final product, that is, isocyanate.

[0090] 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, which of course also fall within the scope of the present invention. [Explanation of symbols]

[0091] 10: reactor, 11: side wall 12: Bottom, 13: Lid 20: sparger, 21: nozzle 30: Agitator, 31: Rotating shaft 32: Impeller, 40: Baffle 100: batch reactor, 101: organic solvent 102: Hydrogen chloride, 321: Radial type impeller 322: Axial type impeller, M: Motor 210: reactor, 211: side wall 212: Bottom, 213: Lid 220: agitator, 221: rotating shaft 222: impeller, 230: sparger 231: pipe, 232: bubble forming section 240: Baffle, 2100: Batch reactor 2101: Amine salt, 2102: Phosgene 2221: Radial type impeller, 2222: Axial type impeller

Claims

1. a reactor into which an aliphatic amine and an organic solvent are introduced; a sparger for supplying gaseous hydrogen chloride into the reactor; a stirrer provided in the reactor for stirring the aliphatic amine, the organic solvent, and the hydrogen chloride; Including, The stirring force of the stirrer is 500 to 4000 (W / m ３ ) a batch reactor.

2. The stirring force of the stirrer is 780 to 3570 (W / m ３ 2. The batch reactor according to claim 1 ,

3. The agitator is A rotation shaft provided in the height direction of the reactor; 2. The batch reaction apparatus according to claim 1, further comprising: an impeller provided on the rotating shaft for stirring the aliphatic amine, the organic solvent, and the hydrogen chloride.

4. The agitator is A radial type impeller or an axial type impeller is provided at the lower end of the rotating shaft, 4. The batch reactor of claim 3, comprising one or more impellers of the same or different types on the lower end impeller.

5. The agitator is 5. The batch reactor according to claim 4, wherein the radial type impeller and the axial type impeller are alternately provided up to a required number of n stages.

6. The sparger is 2. The batch reaction apparatus according to claim 1, further comprising a plurality of nozzles provided in the lower part of the agitator upward from the bottom of the reactor so that gaseous hydrogen chloride can be injected from the lower part of the agitator.

7. The sparger is A nozzle is bent from the lower part of the stirrer and has a plurality of nozzles corresponding to the rotation range of the stirrer, 7. The batch reactor according to claim 6, wherein the plurality of injection ports inject gaseous hydrogen chloride into the aliphatic amine and the liquid organic solvent.

8. A first stage of charging an aliphatic amine and an organic solvent to a reactor; a second stage of supplying gaseous hydrogen chloride into the reactor via a sparger; a third step of stirring the aliphatic amine, the organic solvent and hydrogen chloride with a stirrer; Including, The third stage is The agitator is set to 500 to 4000 (W / m ３ ) A method for producing aliphatic isocyanates, in which the stirring force is controlled.

9. The third stage is The agitator is set to 780 to 3570 (W / m ３ The method for producing an aliphatic isocyanate according to claim 8, wherein the stirring force is controlled at 0.5 to 1000 rpm.

10. a reactor containing a slurry of the amine salt; a sparger for supplying gaseous phosgene into the reactor; a stirrer provided in the reactor for stirring the amine salt and the phosgene; Including, The stirring force of the stirrer is 500 to 10,000 (W / m ３ ) a batch reactor.

11. The stirring force of the stirrer is 1560 to 3170 (W / m ３ 11. The batch reactor according to claim 10,

12. The agitator is A rotation shaft provided in the height direction of the reactor; 11. The batch reaction apparatus according to claim 10, further comprising: an impeller provided on the rotating shaft for stirring the amine salt and the phosgene.

13. The agitator is A radial type impeller or an axial type impeller is provided at the lower end of the rotating shaft, 13. The batch reactor of claim 12, comprising one or more impellers of the same or different types on the lower end impeller.

14. The agitator is The batch reactor according to claim 13, wherein the radial type impeller and the axial type impeller are alternately provided up to a required number of n stages.

15. The sparger is The batch reaction apparatus according to claim 10, wherein a plurality of the agitators are provided along one of an axial direction of the agitator and a circumferential direction of the reactor, and gaseous phosgene is supplied to the agitator.

16. The sparger is A pipe provided on a side wall of the reactor in a direction intersecting the axial direction of the agitator; and a plurality of nozzles provided at the end of the pipe for supplying gaseous phosgene in a gaseous state toward the impeller.

17. A first step of providing a reactor containing an amine salt in a slurry form; a second stage of supplying gaseous phosgene into the reactor via a sparger; a third step of stirring the amine salt and phosgene with a stirrer; Including, The third stage is The stirrer is set to 500 to 10,000 (W / m ３ ) A method for producing aliphatic isocyanates, in which the stirring force is controlled.

18. The third stage is The agitator is set to 1560 to 3170 (W / m ３ The method for producing an aliphatic isocyanate according to claim 17, wherein the stirring force is controlled at 0.5 to 1.0 MPa.

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