JPH0489440A - Chlorination reactor - Google Patents

Abstract

PURPOSE:To obtain a chlorination reactor of wetted wall type efficiently performing chlorinating reaction by using a multi-piped heat exchanger-like wetted wall, comprising many pieces of heat-conduction pipes having small diameter, flowing down a liquid film by uniformly introducing raw material solution into every pipes and uniformly introducing chlorine gas flow in parallel. CONSTITUTION:The objective compact chlorination reactor 1 having a large area forming a wetted wall is composed of a cylindrical body part 2 having an introducing pipe 3 and a discharging pipe 4 of a cooling medium at upper and lower parts on the outer face and having an upper part of an upper pipe board 5 and a lower part of a lower part board 6 connected together through many vertical heat-conduction pipes 7 fitted between the horizontal upper pipe board 5 and the lower pipe board 6, a lower cover 13 covering the lower pipe board 5 and an upper cover 25 covering the upper pipe board 5 having sealed upper part and divided into two parts comprising a lower liquid storing part 22 and an upper gas storing part 23. Dividing pipes 28 are installed at extended positions of the heat-conduction pipes 7 on the upper face of the upper pipe board 5 and liquid holes 32 are pierced in the vicinities of upper face in said upper pipe board 5. Top ends of the dividing pipes are opposed to current board holes 31 having orifice parts 30. Thus, chlorination reaction generating a large amount of heat is efficiently performed at a relatively low temperature.

Description

[Detailed Description of the Invention] [Industrial Application Field] The present invention efficiently performs a chlorination reaction in which, for example, allyl alcohol is reacted with chlorine in an aqueous hydrochloric acid solution to produce 2,3-dichloropropanol. This invention relates to a wet wall type chlorination reactor.

[Prior art] Conventionally, in a chlorination reaction, an organic refrigerant or an aqueous hydrochloric acid solution is placed in a seed reactor equipped with a stirrer and a cooler, the organic substance to be chlorinated is dissolved therein, and chlorine is sucked in while stirring and cooling. I'm making it react. However, although the chlorination reaction is generally a reaction with high reaction heat, it is required that the reaction temperature be relatively low. Therefore, in the above method, a sufficient heat transfer area cannot be obtained, and if the cooling load is to be kept within an industrially practical range, the reaction time will inevitably become longer. As the reaction time becomes longer, the production efficiency decreases, and depending on the type of reaction, there may be other inconveniences such as increased production of by-products.

Therefore, a wet-wall type chlorination reaction is performed in which the raw material liquid is allowed to flow down in a thin film form from the top of a tubular column onto the inner or outer wall, and at the same time chlorine is introduced from the bottom or top of the column to carry out a contact reaction in countercurrent or cocurrent. utensils are now in use.

[Problems to be solved by the invention] However, chlorination is a very fast reaction, and it is necessary to suppress local reactions at the top of the column. Since the thickness must be made thinner, in order to increase the reaction throughput, the diameter of the wetted wall column must be increased to expand the area through which the liquid flows, and - the wetted wall area per column is large. However, this results in the disadvantage that the wetted wall area per installation area becomes smaller.

In order to solve the above problem, the present inventors conducted extensive research and found that by using wet walls in the form of a multi-tubular heat exchanger and cooling the refrigerant by flowing it outside the tubes, the reaction liquid and the inside of the tubes were uniformly distributed. We believed that if chlorine could be introduced in a distributed manner, the chlorination reaction could be carried out efficiently at a low reaction temperature and in an apparatus with high cooling capacity.

The present invention was made based on the above idea, and an object of the present invention is to provide a chlorination reactor that is compact and capable of efficiently producing reaction products.

[Means for Solving the Problem] In order to achieve the above object, the chlorination reactor of the present invention has the following features:
Refrigerant inlet and outlet pipes are provided above and below the outer surface, a horizontal lower tube plate and a lower tube plate are provided, and a number of vertical heat exchanger tubes are installed between the upper tube plate and the lower tube plate, and the heat exchanger tubes are connected to each other. a cylindrical body part through which the upper part of the upper tube plate and the lower part of the lower tube plate are connected; a lower cover covering the lower tube plate of the body part to which an inlet/outlet pipe is attached; and a horizontal part. an upper cover that covers the upper tube plate, which is divided into two by a rectifying plate into a lower liquid storage part having a liquid introduction pipe and an upper gas storage part having a gas introduction pipe, and the upper part of which is sealed; Distribution pipes located on the extensions of the heat transfer tubes are attached to the upper surface of the upper tube plate, liquid holes are bored in the vicinity of the upper surface of the upper tube plate of these distribution pipes, and the tips of the distribution pipes are close to the current plate and bored in the current plate;
They each face a rectifying plate hole having an orifice portion.

[Function] Since the chlorination reactor of the present invention has the above configuration,
The chlorine gas is held at a constant pressure in the gas reservoir and is supplied to the heat exchanger tubes through orifices provided in the rectifier plate holes, so the amount of chlorine supplied to each heat exchanger tube becomes uniform.

In addition, the reaction liquid is introduced into the distribution pipe from the liquid storage part maintained at a constant liquid depth through the liquid hole, and there is a gap between the tip of the distribution pipe and the lower surface of the rectifying plate, so that the inner and outer heads The difference remains constant and the liquid is uniformly introduced into each distribution pipe. Furthermore, the chlorine blown into the distribution pipe through the orifice has an ejector action, so that almost no chlorine flows into the liquid reservoir from the gap.

[Example] Since highly corrosive raw materials are used in the chlorination reactor of the present invention, corrosion-resistant materials must be used. Therefore, a carbon material (carvate) or a glass lining material, which is widely used as a device material such as synthetic hydrochloric acid, is used in the device.

1 and 2 show an embodiment of a chlorination reactor l according to the present invention, and FIG. 1 is a longitudinal sectional view.

Reference numeral 2 in the figure is a cylindrical body part, and this body part 2 includes a body part 2.
An inlet pipe 3 and an outlet pipe 4 are provided for introducing and leading out the refrigerant inside. Furthermore, a horizontal upper tube plate 5 and a lower tube plate 6 are attached to the upper and lower openings of the body 2. A large number of heat exchanger tubes 7 are installed between the upper tube plate 5 and the lower tube plate 6, as shown in cross section in FIG. The upper tube plate 5 and the lower tube plate 6 are provided with an upper hole 8 and a lower hole, respectively, which communicate the upper part of the upper tube plate 5 and the lower part of the lower tube plate 6 with the heat exchanger tube 7 via the heat exchanger tube 7. 9 is provided.

The heat exchanger tubes 7 are supported by baffle plates 1O or baffle plate stays 11 orthogonal thereto, and are arranged at intervals. Furthermore, support legs 12 are attached to the outer surface of the body 2 to vertically support the reactor.

A lower cover 13 is attached to the lower part of the body 2 so as to cover the lower tube plate 6, and the lower cover 13 is provided with a waste discharge pipe 14, a liquid discharge pipe 15, and a raw material liquid introduction pipe 16.

The upper part of the body part 2 covers the upper tube plate 5 and is divided into two by a horizontal rectifying plate 21 into a lower liquid storage part 22 and an upper gas storage part 23, and this gas storage part 23 is divided into a lid part. 24
An upper cover 25 is attached which is sealed by. A reaction liquid introduction pipe 26 is attached to the liquid storage section 22, and a gas storage section 2 is attached to the lid section 24 of the gas storage section 23.
A gas inlet pipe 27 for introducing chlorine into the interior of the tank 3 is attached.

Further, as shown in FIGS. 3 and 4, which are enlarged views of portions A and B in FIG. The tip thereof is close to the lower surface of the current plate 21, and a gap 29 is provided therebetween. The distal end opening of the distribution pipe 28 faces a rectifying plate hole 31 having an orifice portion 30 formed in the rectifying plate 21 . Further, in the vicinity of the upper surface of the upper tube plate 5 of the distribution pipe 28, as shown in FIG. 5, two or more liquid holes 32 are bored.

In addition, 41 is a drain outlet, 42 is LA and Ll, respectively.
, TA, TI, PIA, etc. detection unit mounting seat.

To carry out a chlorination reaction using the chlorination reactor configured as described above, as shown in FIG. The liquid is introduced into the liquid reservoir through the liquid introduction pipe 26. The reaction liquid flows down from the liquid hole 32 of the distribution pipe 28 along the inner surface of the heat transfer tube 7, forming a wet wall. At the same time, Cat gas is introduced into gas introduction pipe 2.
Introduced from 7. The C+ gas is uniformly distributed by the orifice section and reacts with the flowing reaction liquid. At this time, since the flowing reaction liquid is a thin film and is cooled from the outside with brine, it is efficiently cooled and maintained at a desired temperature. Further, the chlorination reaction has a fast reaction rate, and the chlorine introduced into each heat exchanger tube 7 reacts and disappears by the time it reaches the lower cover 13. After the reaction reaches a steady state, the liquid reservoir 22
Then, while maintaining the liquid level 43 in the lower cover 13 constant, the raw material liquid is introduced and the generated chloride is extracted.

By this operation, the liquid flowing down the multiple heat transfer tubes 7 is
Temperature rise is prevented and efficient chlorination reaction takes place. HCI produced by the chlorination reaction is extracted and recovered from the gas outlet pipe 14.

In the above reactor, the progress of chlorination can be adjusted by controlling the amount of raw material liquid introduced and the amount of chlorine introduced.

[Effects of the Invention] As explained above, the chlorination reactor of the present invention uses a wet wall shaped like a shell-and-tube heat exchanger in which a large number of small-diameter heat exchanger tubes are grouped together to uniformly distribute the raw material liquid. It is possible to react by introducing chlorine gas uniformly in parallel flow and causing a liquid film to flow down, so it is compact, has a large surface area to form a wet wall, and compares chlorination reactions with a large calorific value. This makes it possible to carry out the process efficiently at a relatively low temperature, resulting in five economic advantages.

[Brief explanation of drawings]

1 and 2 show an embodiment of a chlorination reactor according to the present invention, with FIG. 1 being a longitudinal sectional view and FIG. 2 showing the arrangement of heat exchanger tubes. Fig. 3 is an enlarged view of part A in Fig. 1, Fig. 4 is an enlarged view of part B in Fig. 1, and Fig. 5 is an enlarged view of part B in Fig. 3. A cross-sectional view of the liquid hole, FIG. 6, is an explanatory diagram of the state in which the reactor of FIG. 1 is used. 1. Chlorination reactor, 2. Body, 3 Refrigerant introduction pipe, 4.
...Refrigerant outlet pipe, 5.. Upper tube plate, 6.. Lower tube plate, 7. Heat exchanger tube, 8.. Upper hole, 9. Lower hole, 10. Baffle plate, 11.. Baffle plate stay 12... Support legs, 13...Lower cover 14.
...Gas outlet pipe, 15 Liquid outlet pipe, 16 Raw material introduction pipe, 2
1. Current plate, 22. Liquid storage section, 23. Gas storage section, 2
4...Lid part, 25...Top cover 26...Reaction liquid introduction tube,
27 Distribution piping, 29-・Gap, 30 Rectifier plate hole, 32・Liquid hole, 42・Mounting seat for each detection part, Gas introduction pipe, 28... Orifice section, 31 41... Drain removal, 43 Liquid level, 44.

Claims (1)

[Claims] Refrigerant inlet and outlet pipes are provided above and below the outer surface, horizontal upper and lower tube plates are attached, and a number of vertical heat exchanger tubes are installed between the upper and lower tube plates. a cylindrical body part to which the upper tube plate and the lower part of the lower tube plate are connected through the heat transfer tube; and a lower tube plate of the body to which the inlet/outlet pipe is attached. A lower cover covers the upper tube plate, which is divided into two by a horizontal rectifying plate into a lower liquid storage part having a liquid introduction pipe and an upper gas storage part having a gas introduction pipe, and whose upper part is sealed. an upper cover, distribution pipes located on extensions of the heat transfer tubes are attached to the upper surface of the upper tube plate, and liquid holes are bored in the vicinity of the upper surface of the upper tube plate of these distribution pipes, A chlorination reactor characterized in that the distal end of the distribution pipe is close to the current plate and faces a current plate hole having an orifice portion, which is bored in the current plate.