Hydrolysis reaction system for preparing chloromethyl ethyl ether

Abstract

The utility model discloses a hydrolysis reaction system for preparing chloromethyl ether, which comprises a hydrolysis reaction kettle, the top of the hydrolysis reaction kettle is provided with a first port and a second port which are arranged side by side, a dripping kettle is arranged above the first port, an etherification kettle is arranged above the second port, and the first port and the second port are communicated with each other. The dripping kettle and the etherification kettle are respectively connected with the first port and the second port through supporting cylinders; a dripping pipe is arranged in the supporting cylinder above the first port in a penetrating manner, and an air outlet pipe is arranged in the supporting cylinder above the second port in a penetrating manner; the hydrolysis reaction kettle is located in the shell, and a closed clamping cavity is formed between the outer wall of the hydrolysis reaction kettle and the inner wall of the shell. The hydrolysis reaction system provided by the utility model not only can solve the problem that hydrochloric acid mist is generated in the process of conveying phosphorus trichloride to the reaction kettle and dropwise adding the phosphorus trichloride, but also can solve the problems that hydrogen chloride gas is difficult to discharge immediately and the phosphorus trichloride is not completely hydrolyzed.

Description

Technical Field

[0001] The utility model relates to a hydrolysis reaction system for preparing chloromethyl ethyl ether, belonging to the technical field of hydrolysis equipment. Background Art

[0002] Chloromethyl ether, also known as chloromethyl ethyl ether, is a colorless transparent liquid, mainly used for pesticide intermediates, pharmaceutical intermediates, and new material synthesis. The preparation principle of chloromethyl ether: phosphorus trichloride is added dropwise to 31% hydrochloric acid to cause phosphorus trichloride to hydrolyze with water, and the generated hydrogen chloride is sent to the etherification kettle to further react with polyformaldehyde, ethanol, etc. to generate the product chloromethyl ether, while phosphorous acid and hydrochloric acid are produced as by-products.

[0003] The phosphorus trichloride hydrolysis process requires a reactor, such as the phosphorus trichloride hydrolysis reactor disclosed in Patent No. CN201920951847.6, which includes a kettle body having a hydrolysis chamber, a water supply pipe, a feed pipe and a hydrogen chloride discharge pipe connected to the hydrolysis chamber are arranged on the top of the kettle body, and a discharge pipe connected to the hydrolysis chamber is arranged at the bottom of the kettle body.

[0004] Phosphorus trichloride will produce hydrochloric acid mist during the transportation and dripping process to the reactor. If not treated, it will cause damage to the respiratory system of the operator and cause serious pollution to the environment. The hydrogen chloride gas produced by the reaction is difficult to be discharged immediately, which restricts the amount and speed of phosphorus trichloride dripping in the hydrolysis reaction. There is also the problem of incomplete hydrolysis of phosphorus trichloride, and more phosphorus trichloride is brought out by hydrogen chloride gas.

[0005] In summary, the prior art obviously has inconveniences and defects in practical use, so it is necessary to improve it. Utility Model Content

[0006] The utility model aims at the deficiencies in the background technology and provides a hydrolysis reaction system for preparing chloromethyl ether, which can not only solve the problem that hydrochloric acid mist will be generated during the transportation and dropwise addition of phosphorus trichloride to a reactor, but also solve the problem that hydrogen chloride gas is difficult to be discharged immediately and phosphorus trichloride is incompletely hydrolyzed.

[0007] In order to solve the above technical problems, the utility model adopts the following technical solutions:

[0008] A hydrolysis reaction system for preparing chloromethyl ethyl ether comprises a hydrolysis reaction kettle, wherein the top of the hydrolysis reaction kettle is provided with a first port and a second port arranged side by side, a dropping kettle is arranged above the first port, an etherification kettle is arranged above the second port, and the dropping kettle and the etherification kettle are respectively connected to the first port and the second port through a supporting cylinder;

[0009] A dripping tube is inserted into the support tube above the first port, and an air outlet pipe is inserted into the support tube above the second port; the hydrolysis reactor is located inside the shell, and a sealed cavity is provided between the outer wall of the hydrolysis reactor and the inner wall of the shell.

[0010] Furthermore, the top end of the support cylinder is fixedly connected to the bottom of the dropping kettle and the etherification kettle by welding, and the bottom end of the support cylinder is provided with a flange connected to the first port and the second port.

[0011] Furthermore, the dripping pipe and the air outlet pipe are both arranged in a vertical direction.

[0012] Furthermore, the top end of the dripping tube is connected to the bottom of the dripping kettle, the bottom end of the dripping tube is connected to the upper part of the inner cavity of the hydrolysis reactor, and an automatic regulating valve is installed on the dripping tube.

[0013] Furthermore, the top end of the gas outlet pipe is located at the upper part of the inner cavity of the etherification kettle, and the bottom end of the gas outlet pipe is connected to the upper part of the inner cavity of the hydrolysis reactor.

[0014] Furthermore, a stirring paddle is installed inside the hydrolysis reactor, and the stirring paddle is driven by a motor above the hydrolysis reactor.

[0015] Furthermore, the motor is located between the first port and the second port.

[0016] Furthermore, a hydrochloric acid inlet is provided on one side of the top of the hydrolysis reactor, and a phosphorous acid outlet is provided on one side of the bottom of the hydrolysis reactor.

[0017] Furthermore, a circulating water inlet is provided on one side of the bottom of the clamping cavity, a circulating water outlet is provided on one side of the top of the clamping cavity, and a spiral guide blade is provided between the outer wall of the hydrolysis reactor and the inner wall of the shell.

[0018] Compared with the prior art, the utility model has the following advantages after adopting the above technical solution:

[0019] The dripping tube in the utility model is built in the supporting tube between the dripping kettle and the hydrolysis reactor, which can solve the problem that hydrochloric acid mist will be generated during the transportation and dripping of phosphorus trichloride to the reactor;

[0020] The hydrogen chloride outlet pipe in the utility model is built in the support cylinder between the hydrolysis reactor and the etherification reactor, and the hydrogen chloride generated by the hydrolysis reaction is directly introduced into the etherification reactor, which solves the problem that the hydrogen chloride gas is difficult to be discharged immediately;

[0021] The utility model arranges a stirring paddle inside the hydrolysis reaction kettle to make the materials fully contact and realize thorough hydrolysis, thus solving the problem of incomplete hydrolysis of phosphorus trichloride.

[0022] The utility model is described in detail below with reference to the accompanying drawings and embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is a structural schematic diagram of the utility model;

[0024] Figure 2 It is a schematic diagram of the internal structure of the utility model.

[0025] In the figure, 1-hydrolysis reactor, 2-first port, 3-second port, 4-dropping reactor, 5-etherification reactor, 6-support cylinder, 7-dropping tube, 8-automatic regulating valve, 9-air outlet pipe, 10-hydrochloric acid inlet, 11-phosphorous acid outlet, 12-housing, 13-spiral guide blade, 14-circulating water inlet, 15-circulating water outlet, 16-stirring paddle, 17-motor. DETAILED DESCRIPTION

[0026] In order to have a clearer understanding of the technical features, purposes and effects of the utility model, the specific implementation methods of the utility model are now described with reference to the accompanying drawings.

[0027] like Figure 1 and Figure 2 As shown together, the utility model provides a hydrolysis reaction system for preparing chloromethyl ether, comprising a hydrolysis reactor 1, wherein the top of the hydrolysis reactor 1 is provided with a first port 2 and a second port 3 arranged side by side, a dropping reactor 4 is arranged above the first port 2, and an etherification reactor 5 is arranged above the second port 3, and the dropping reactor 4 and the etherification reactor 5 are connected to the first port 2 and the second port 3 through a supporting tube 6, respectively.

[0028] The top end of the support tube 6 is fixedly connected to the bottom of the dropping kettle 4 and the etherification kettle 5 by welding, and the bottom end of the support tube 6 is provided with a flange connected to the first port 2 and the second port 3.

[0029] A dripping tube 7 is inserted into the support tube 6 above the first port 2, and the dripping tube 7 is arranged in the vertical direction. The top end of the dripping tube 7 is connected to the bottom of the dripping kettle 4, and the bottom end of the dripping tube 7 is connected to the upper part of the inner cavity of the hydrolysis reactor 1. An automatic regulating valve 8 is installed on the dripping tube 7.

[0030] An air outlet pipe 9 is provided in the support tube 6 above the second port 3 . The air outlet pipe 9 is arranged in the vertical direction. The top of the air outlet pipe 9 is located at the upper part of the inner cavity of the etherification kettle 5 , and the bottom of the air outlet pipe 9 is connected to the upper part of the inner cavity of the hydrolysis reactor 1 .

[0031] The hydrolysis reactor 1 is provided with a stirring paddle 16 which is driven by a motor 17 above the hydrolysis reactor 1 and located between the first port 2 and the second port 3. The stirring paddle 16 rotates to allow the materials to be fully contacted and achieve thorough hydrolysis.

[0032] A hydrochloric acid inlet 10 is provided on one side of the top of the hydrolysis reactor 1 , and a phosphorous acid outlet 11 is provided on one side of the bottom of the hydrolysis reactor 1 .

[0033] The hydrolysis reactor 1 is located inside the shell 12, and a sealed cavity is provided between the outer wall of the hydrolysis reactor 1 and the inner wall of the shell 12. A circulating water inlet 14 is provided on one side of the bottom of the cavity, and a circulating water outlet 15 is provided on one side of the top of the cavity. A spiral guide blade 13 is provided between the outer wall of the hydrolysis reactor 1 and the inner wall of the shell 12. The spiral guide blade 13 guides the circulating water in a spiral manner, thereby achieving effective temperature control of the material in the hydrolysis reactor 1 and timely removing the reaction heat.

[0034] The specific working principle of this utility model:

[0035] The motor 17 drives the stirring blade 16 to rotate, 31% hydrochloric acid enters the hydrolysis reactor 1 from the hydrochloric acid inlet 10, and the dropping tube 7 drops the phosphorus trichloride in the dropping reactor 4 into the hydrolysis reactor 1, and a hydrolysis reaction occurs with water. The hydrogen chloride gas generated by the hydrolysis is directly introduced into the etherification reactor 5 from the gas outlet 9 to react with polyformaldehyde, ethanol, etc. to generate the product chloromethyl ether, and the phosphorous acid generated by the hydrolysis is discharged from the phosphorous acid outlet 11. The reaction heat generated in the hydrolysis process is taken away in time by the circulating water to avoid overheating of the reaction.

[0036] The above is an example of the best implementation of the utility model, and the parts not described in detail are common knowledge of ordinary technicians in this field. The protection scope of the utility model is based on the content of the claims, and any equivalent transformation based on the technical inspiration of the utility model is also within the protection scope of the utility model.

Claims

1. A hydrolysis reaction system for preparing chloromethyl ether, characterized in that: The invention comprises a hydrolysis reactor (1), wherein the top of the hydrolysis reactor (1) is provided with a first port (2) and a second port (3) arranged side by side, a dropping reactor (4) is arranged above the first port (2), and an etherification reactor (5) is arranged above the second port (3), and the dropping reactor (4) and the etherification reactor (5) are respectively connected to the first port (2) and the second port (3) via a support tube (6); A dripping tube (7) is inserted into the support tube (6) above the first port (2), and an air outlet pipe (9) is inserted into the support tube (6) above the second port (3); the hydrolysis reactor (1) is located inside the outer shell (12), and a sealed cavity is provided between the outer wall of the hydrolysis reactor (1) and the inner wall of the outer shell (12).

2. The hydrolysis reaction system for preparing chloromethyl ether as claimed in claim 1, characterized in that: The top end of the support cylinder (6) is fixedly connected to the bottom of the dropping kettle (4) and the etherification kettle (5) by welding, and the bottom end of the support cylinder (6) is provided with a flange connected to the first port (2) and the second port (3).

3. The hydrolysis reaction system for preparing chloromethyl ether as claimed in claim 1, characterized in that: The dripping pipe (7) and the air outlet pipe (9) are both arranged in a vertical direction.

4. The hydrolysis reaction system for preparing chloromethyl ether as claimed in claim 3, characterized in that: The top end of the dripping tube (7) is connected to the bottom of the dripping kettle (4), the bottom end of the dripping tube (7) is connected to the upper part of the inner cavity of the hydrolysis reaction kettle (1), and an automatic regulating valve (8) is installed on the dripping tube (7).

5. The hydrolysis reaction system for preparing chloromethyl ether as claimed in claim 3, characterized in that: The top end of the gas outlet pipe (9) is located at the upper part of the inner cavity of the etherification kettle (5), and the bottom end of the gas outlet pipe (9) is connected to the upper part of the inner cavity of the hydrolysis reaction kettle (1).

6. The hydrolysis reaction system for preparing chloromethyl ether according to claim 1, characterized in that: A stirring paddle (16) is installed inside the hydrolysis reactor (1), and the stirring paddle (16) is driven by a motor (17) above the hydrolysis reactor (1).

7. The hydrolysis reaction system for preparing chloromethyl ether as claimed in claim 6, characterized in that: The motor (17) is located between the first port (2) and the second port (3).

8. The hydrolysis reaction system for preparing chloromethyl ether according to claim 1, characterized in that: A hydrochloric acid inlet (10) is provided on one side of the top of the hydrolysis reactor (1), and a phosphorous acid outlet (11) is provided on one side of the bottom of the hydrolysis reactor (1).

9. The hydrolysis reaction system for preparing chloromethyl ether according to claim 1, characterized in that: A circulating water inlet (14) is provided on one side of the bottom of the clamping chamber, a circulating water outlet (15) is provided on one side of the top of the clamping chamber, and a spiral guide blade (13) is provided between the outer wall of the hydrolysis reactor (1) and the inner wall of the outer shell (12).

Images