Cyanation reaction system for preparing p-chlorophenylglycine

Abstract

The utility model discloses a cyanidation reaction system for preparing p-chlorophenylglycine, which comprises a vertical sealing tower, a cyanidation reaction cavity, a methanol receiving cavity and a methanol condensing cavity are sequentially arranged in the vertical sealing tower from bottom to top, and a communicating pipe arranged along the vertical direction penetrates through the interiors of the cyanidation reaction cavity, the methanol receiving cavity and the methanol condensing cavity. The bottom end of the communicating pipe is located at the top of the cyanidation reaction cavity, an electromagnetic valve is mounted at the bottom end of the communicating pipe, and the top end of the communicating pipe is located above the methanol condensation cavity; a heat insulation layer is arranged between the cyanidation reaction cavity and the methanol receiving cavity. The cyanidation reaction system for preparing the p-chlorophenylglycine, provided by the utility model, can integrate multiple functions of cyanidation reaction, methanol condensation and methanol receiving, can shorten the length of a production line, reduces the production cost, and is beneficial to the space layout of a site.

Description

Technical Field

[0001] The utility model relates to a cyanidation reaction system for preparing p-chlorophenylglycine, belonging to the technical field of chemical equipment. Background Art

[0002] p-Chlorophenylglycine, also known as DL-p-chlorophenylglycine, is mainly used for the synthesis of bromopyrrole nitrile and chlorfenapyr. p-Chlorobenzaldehyde, ammonium bicarbonate, sodium cyanide, and ammonia water are used as a solvent to undergo cyanation reaction to obtain p-chlorophenyl hydroxylamine. p-Chlorophenyl hydroxylamine undergoes alkaline hydrolysis reaction with liquid alkali to generate p-chlorophenylglycine sodium salt, which is decolorized with activated carbon, neutralized with hydrochloric acid, and centrifuged to obtain the finished p-chlorophenylglycine.

[0003] At present, the cyanidation reaction system required for preparing p-chlorophenylglycine generally includes a cyanidation reactor, a cyanidation condenser and a cyanidation methanol receiving tank arranged in series. The cyanidation condenser and the cyanidation methanol receiving tank are arranged in series with the top of the cyanidation reactor to recover methanol.

[0004] In the prior art, methanol recovery is achieved by connecting multiple devices in series. The production line is relatively long and complicated, the production cost is high, and there is a problem that it is not conducive to the spatial layout of the site.

[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] In view of the deficiencies in the background technology, the utility model provides a cyanidation reaction system for preparing p-chlorophenylglycine, which can integrate cyanidation reaction, methanol condensation and methanol receiving functions, shorten the length of the production line, reduce production costs, and facilitate site space layout.

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

[0008] The invention discloses a cyanidation reaction system for preparing p-chlorophenylglycine, comprising a vertical sealing tower, wherein a cyanidation reaction chamber, a methanol receiving chamber and a methanol condensation chamber are sequentially arranged inside the vertical sealing tower from bottom to top, wherein a connecting pipe arranged in a vertical direction is passed through the inside of the cyanidation reaction chamber, the methanol receiving chamber and the methanol condensation chamber, wherein the bottom end of the connecting pipe is located at the top of the cyanidation reaction chamber, an electromagnetic valve is installed on the bottom end of the connecting pipe, and the top end of the connecting pipe is located above the methanol condensation chamber; and a heat insulating layer is arranged between the cyanidation reaction chamber and the methanol receiving chamber.

[0009] Furthermore, a plurality of fixing seats distributed in a circumference are fixedly connected to the periphery of the vertical sealing tower, and the fixing seats are used to support and fix the vertical sealing tower.

[0010] Furthermore, a stirring paddle is installed at the bottom of the cyanidation reaction chamber, and the stirring paddle is driven by a motor at the bottom of the vertical sealed tower.

[0011] Furthermore, a jacket is provided outside the cyanidation reaction chamber, a circulating water inlet is provided on one side of the bottom of the jacket, and a circulating water outlet is provided on one side of the top of the jacket.

[0012] Furthermore, a material inlet is provided at the top side of the cyanide reaction chamber, and the number of the material inlet is multiple.

[0013] Furthermore, a product outlet is provided on one side of the bottom of the cyanidation reaction chamber.

[0014] Furthermore, a methanol outlet is provided on one side of the bottom of the methanol receiving chamber.

[0015] Furthermore, an upper perforated plate is provided at the top of the methanol condensation chamber, and a lower perforated plate is provided at the bottom, and the upper perforated plate and the lower perforated plate are fixedly connected to the inner wall of the vertical sealing tower.

[0016] Furthermore, a condensation tube bundle is provided between the upper orifice plate and the lower orifice plate. The condensation tube bundle includes a plurality of evenly distributed condensation tubes, and both ends of the condensation tubes are fixedly connected to the upper orifice plate and the lower orifice plate.

[0017] Furthermore, a cooling water inlet is provided on one side of the bottom of the methanol condensation chamber, and a cooling water outlet is provided on one side of the top of the methanol condensation chamber.

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

[0019] The vertical sealed tower is provided with a cyanide reaction chamber, a methanol receiving chamber and a methanol condensation chamber from bottom to top. The cyanide reaction chamber, the methanol receiving chamber and the methanol condensation chamber are provided with a connecting pipe. The gaseous methanol can be transported to the methanol condensation chamber through the connecting pipe to achieve condensation. After condensation, the gaseous methanol enters the methanol receiving chamber for storage.

[0020] The utility model integrates the multiple functions of cyanidation reaction, methanol condensation and methanol receiving, shortens the length of the production line, reduces the production cost and is beneficial to the site space layout.

[0021] The utility model is described in detail below with reference to the accompanying drawings and embodiments. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 It is a structural schematic diagram of the utility model;

[0023] Figure 2 It is a schematic diagram of the bottom structure of the utility model;

[0024] Figure 3 It is a schematic diagram of the top structure of the utility model.

[0025] In the figure, 1-vertical sealing tower, 2-fixed seat, 3-cyanide reaction chamber, 4-methanol receiving chamber, 5-methanol condensation chamber, 6-stirring paddle, 7-jacket, 8-circulating water inlet, 9-circulating water outlet, 10-material inlet, 11-product outlet, 12-connecting pipe, 13-solenoid valve, 14-insulation layer, 15-methanol outlet, 16-upper orifice plate, 17-lower orifice plate, 18-cooling water inlet, 19-cooling water outlet, 20-condensation tube bundle. 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-Figure 3 As shown together, the utility model provides a cyanidation reaction system for preparing p-chlorophenylglycine, including a vertical sealing tower 1, a plurality of circumferentially distributed fixing seats 2 are fixedly connected to the periphery of the vertical sealing tower 1, and the fixing seats 2 are used to support and fix the vertical sealing tower 1.

[0028] A cyanide reaction chamber 3, a methanol receiving chamber 4 and a methanol condensation chamber 5 are sequentially arranged inside the vertical sealed tower 1 from bottom to top. A connecting pipe 12 arranged in a vertical direction passes through the cyanide reaction chamber 3, the methanol receiving chamber 4 and the methanol condensation chamber 5. The bottom end of the connecting pipe 12 is located at the top of the cyanide reaction chamber 3. A solenoid valve 13 is installed on the bottom end of the connecting pipe 12. The top end of the connecting pipe 12 is located above the methanol condensation chamber 5.

[0029] A heat insulation layer 14 is provided between the cyanidation reaction chamber 3 and the methanol receiving chamber 4 to prevent the heat in the cyanidation reaction chamber 3 from being transferred to the methanol receiving chamber 4 .

[0030] A stirring paddle 6 is installed at the bottom of the cyanidation reaction chamber 3 , and the stirring paddle 6 is driven by a motor at the bottom of the vertical sealed tower 1 .

[0031] A jacket 7 is provided outside the cyanidation reaction chamber 3 , a circulating water inlet 8 is provided on one side of the bottom of the jacket 7 , and a circulating water outlet 9 is provided on one side of the top of the jacket 7 . The circulating water flows in the jacket 7 to control the temperature of the material in the cyanidation reaction chamber 3 .

[0032] A material inlet 10 is disposed on the top side of the cyanidation reaction chamber 3 , and the number of the material inlet 10 is multiple.

[0033] A product outlet 11 is provided at one side of the bottom of the cyanidation reaction chamber 3 .

[0034] A methanol outlet 15 is provided at one side of the bottom of the methanol receiving chamber 4 .

[0035] An upper perforated plate 16 is disposed on the top of the methanol condensation chamber 5 , and a lower perforated plate 17 is disposed on the bottom. The upper perforated plate 16 and the lower perforated plate 17 are fixedly connected to the inner wall of the vertical sealing tower 1 .

[0036] A condensation tube bundle 20 is provided between the upper orifice plate 16 and the lower orifice plate 17 . The condensation tube bundle 20 includes a plurality of evenly distributed condensation tubes. Both ends of the condensation tubes are fixedly connected to the upper orifice plate 16 and the lower orifice plate 17 .

[0037] A cooling water inlet 18 is provided on one side of the bottom of the methanol condensation chamber 5 , and a cooling water outlet 19 is provided on one side of the top of the methanol condensation chamber 5 .

[0038] The specific working principle of this utility model:

[0039] Methanol is added into the cyanidation reaction chamber 3, and the methanol is cooled to below 35° C. by circulating water in the jacket 7; ammonium bicarbonate is then added in batches, and stirred for a certain period of time by the stirring paddle 6; liquid sodium cyanide, ammonia water, and p-chlorobenzaldehyde are sequentially added into the cyanidation reaction chamber 3, and stirred for a certain period of time; the temperature in the cyanidation reaction chamber 3 is increased, and methanol recovery begins, gaseous methanol enters the upper part of the methanol condensation chamber 5 through the connecting pipe 12, and then enters the condensation tube bundle 20 from top to bottom, condenses inside the condensation tube bundle 20, and enters the methanol receiving chamber 4 after condensation. After the methanol recovery is completed, the temperature in the cyanidation reaction chamber 3 is reduced, and the product after the temperature reduction is discharged from the product outlet 11.

[0040] 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 cyanidation reaction system for preparing p-chlorophenylglycine, characterized in that: The invention comprises a vertical sealed tower (1), wherein a cyanide reaction chamber (3), a methanol receiving chamber (4) and a methanol condensation chamber (5) are arranged in sequence from bottom to top inside the vertical sealed tower (1), wherein a connecting pipe (12) arranged in a vertical direction passes through the inside of the cyanide reaction chamber (3), the methanol receiving chamber (4) and the methanol condensation chamber (5), wherein the bottom end of the connecting pipe (12) is located at the top of the cyanide reaction chamber (3), an electromagnetic valve (13) is installed on the bottom end of the connecting pipe (12), and the top end of the connecting pipe (12) is located above the methanol condensation chamber (5); and a heat insulating layer (14) is provided between the cyanide reaction chamber (3) and the methanol receiving chamber (4).

2. The cyanidation reaction system for preparing p-chlorophenylglycine according to claim 1, characterized in that: A plurality of circumferentially distributed fixing seats (2) are fixedly connected to the periphery of the vertical sealing tower (1), and the fixing seats (2) are used to support and fix the vertical sealing tower (1).

3. The cyanidation reaction system for preparing p-chlorophenylglycine according to claim 1, characterized in that: A stirring paddle (6) is installed at the bottom of the cyanidation reaction chamber (3), and the stirring paddle (6) is driven by a motor at the bottom of the vertical sealing tower (1).

4. The cyanidation reaction system for preparing p-chlorophenylglycine according to claim 1, characterized in that: A jacket (7) is provided outside the cyanidation reaction chamber (3), a circulating water inlet (8) is provided on one side of the bottom of the jacket (7), and a circulating water outlet (9) is provided on one side of the top of the jacket (7).

5. The cyanidation reaction system for preparing p-chlorophenylglycine according to claim 1, characterized in that: A material inlet (10) is provided at the top side of the cyanidation reaction chamber (3), and the number of the material inlet (10) is multiple.

6. The cyanidation reaction system for preparing p-chlorophenylglycine according to claim 1, characterized in that: A product outlet (11) is provided on one side of the bottom of the cyanidation reaction chamber (3).

7. The cyanidation reaction system for preparing p-chlorophenylglycine according to claim 1, characterized in that: A methanol outlet (15) is provided on one side of the bottom of the methanol receiving chamber (4).

8. The cyanidation reaction system for preparing p-chlorophenylglycine according to claim 1, characterized in that: The top of the methanol condensation chamber (5) is provided with an upper perforated plate (16), and the bottom is provided with a lower perforated plate (17), and the upper perforated plate (16) and the lower perforated plate (17) are fixedly connected to the inner wall of the vertical sealing tower (1).

9. The cyanidation reaction system for preparing p-chlorophenylglycine according to claim 8, characterized in that: A condensation tube bundle (20) is provided between the upper orifice plate (16) and the lower orifice plate (17), wherein the condensation tube bundle (20) comprises a plurality of evenly distributed condensation tubes, wherein both ends of the condensation tubes are fixedly connected to the upper orifice plate (16) and the lower orifice plate (17).

10. The cyanidation reaction system for preparing p-chlorophenylglycine according to claim 9, characterized in that: A cooling water inlet (18) is provided on one side of the bottom of the methanol condensation chamber (5), and a cooling water outlet (19) is provided on one side of the top of the methanol condensation chamber (5).

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