Device for reducing cost for preparing 2-hydroxy-3-naphthoic acid through carboxylation, production process and application

Abstract

The invention provides a device for reducing the cost of preparing 2-hydroxy-3-naphthoic acid through carboxylation, a production process and application, and belongs to the technical field of chemical engineering. According to the device for reducing the cost of preparing 2-hydroxy-3-naphthoic acid through carboxylation, the carboxylation reaction kettle is connected with a set of three-stage pressure equalizing device. The carbon dioxide after the reaction is temporarily stored in the three-stage pressure equalizing device, and is returned to the carboxylation reaction kettle after the next reaction is started, so that the recycling of the carbon dioxide is realized, and the cost is reduced. By using the device disclosed by the invention, the cost for preparing 2-hydroxy-3-naphthoic acid through carboxylation can be reduced, full utilization of resources is realized, the production cost is reduced, and the device has an industrial application prospect.

Description

Technical Field

[0001] The invention belongs to the technical field of chemical industry, relates to a production process of organic chemical products, and specifically relates to a device for reducing the cost of preparing 2-hydroxy-3-naphthoic acid by carboxylation, a production process and an application thereof. Background Art

[0002] 2-Hydroxy-3-naphthoic acid is an important dye, pigment and pharmaceutical intermediate with a wide range of uses. At present, the gas-solid phase method is generally used in the industry to produce 2-hydroxy-3-naphthoic acid, and the process steps are: using carbon dioxide gas to react with 2-naphthol salt for carboxylation, removing the by-products of the reaction, and then undergoing acid precipitation, centrifugation, drying and other steps to obtain the finished 2-hydroxy-3-naphthoic acid.

[0003] In the current process of producing 2-hydroxy-3-naphthoic acid using a gas-solid phase method, carbon dioxide is usually discharged into the exhaust gas during the pressure release process after the carboxylation reaction, which results in a low utilization efficiency of the carbon dioxide used in the production, resulting in a waste of resources. Therefore, it is very important to improve the utilization efficiency of carbon dioxide in the production of 2-hydroxy-3-naphthoic acid.

[0004] Invention patent CN114853591A discloses a process for resource utilization of carbon dioxide in carboxylation reaction. At the end of the preparation process, a gas-liquid separation device is used to cool and condense the gas phase material, and then the carbon dioxide is recovered by gas-liquid separation. Not only are the process equipment and process parameters required to be high, but the energy consumption and process cost caused by cooling and condensation are also high. Invention patent CN112516925A discloses a process for recycling carbon dioxide in carboxylation reaction using a fan. This process is very restrictive and is only applicable to specific fluidized bed reactors. It cannot be used for devices that require high-pressure reactions. Summary of the invention

[0005] In view of the problems existing in the prior art, the present invention provides a device, a production process and an application for reducing the cost of preparing 2-hydroxy-3-naphthoic acid by carboxylation. The device and the production process are simple to operate, the equipment is easily available and the process cost is low.

[0006] To achieve the above purpose, the technical solution adopted by the present invention is as follows:

[0007] In a first aspect, the present invention provides a device for reducing the cost of carboxylation of 2-hydroxy-3-naphthoic acid, wherein the carboxylation reaction kettle is connected to a set of three-stage pressure equalization devices.

[0008] The three-stage pressure equalizing device is composed of three pressure equalizing tanks connected in parallel.

[0009] In a second aspect, the present invention provides an application of the above-mentioned device in improving the carboxylation yield of 2-hydroxy-3-naphthoic acid.

[0010] In a third aspect, the present invention provides a production process for reducing the cost of carboxylation of 2-hydroxy-3-naphthoic acid, using the above-mentioned device, comprising the following steps:

[0011] S1. After the carboxylation reaction is completed, a first-level pressure equalizing tank is used to perform first-level pressure equalization on the carboxylation reactor;

[0012] S2, after the first-level pressure equalization, using a second-level pressure equalization tank to perform second-level pressure equalization on the carboxylation reactor;

[0013] S3, after the secondary pressure equalization, a third-stage pressure equalization tank is used to perform third-stage pressure equalization on the carboxylation reactor;

[0014] S4, after three-stage equalization, the reaction products are collected and the materials required for the next reaction are introduced;

[0015] S5, according to the order of the three-stage pressure equalizing tank, the second-stage pressure equalizing tank, and the first-stage pressure equalizing tank, the carboxylation reaction kettle is subjected to reverse pressure equalization;

[0016] S6, introducing carbon dioxide into the carboxylation reaction kettle to make up the pressure and continue the reaction.

[0017] Specifically, in the step S1, the endpoint pressure value of the first-stage equalization pressure is 0.35-0.5 MPa.

[0018] Preferably, the endpoint pressure value of the first-stage equalization pressure is 0.4-0.5 MPa.

[0019] Preferably, the endpoint pressure value of the first-stage equalization pressure is 0.4 MPa.

[0020] Specifically, in step S2, the endpoint pressure value of the secondary pressure equalization is 0.15-0.3 MPa.

[0021] Preferably, the endpoint pressure value of the secondary pressure equalization is 0.2-0.3 MPa.

[0022] Preferably, the endpoint pressure value of the secondary pressure equalization is 0.2 MPa.

[0023] Specifically, in step S3, the endpoint pressure value of the three-stage equalization pressure is 0.08-0.12 MPa.

[0024] Preferably, the endpoint pressure value of the three-stage equalization pressure is 0.1-0.12 MPa.

[0025] Preferably, the endpoint pressure value of the three-stage equalization pressure is 0.1 MPa.

[0026] Specifically, in step S6, the replenishing pressure is 0.5-0.6 MPa.

[0027] Preferably, the replenishing pressure is 0.6 MPa.

[0028] The technical effects achieved by the present invention are:

[0029] (1) The present invention recovers unreacted carbon dioxide gas in the production of 2-hydroxy-3-naphthoic acid in situ at the carboxylation reaction kettle, recovers the carbon dioxide and temporarily stores it in a pressure equalizing tank, and then reverses the pressure equalization to achieve carbon dioxide reuse when the next reaction starts, thereby avoiding the cumbersome operation of first discharging carbon dioxide into process waste gas and then condensing and recovering it in the general process.

[0030] (2) The device and production process of the present invention are easy to operate, the equipment is easily available and the process cost is low, and has a good application prospect. DETAILED DESCRIPTION

[0031] The following describes the embodiments of the present invention through specific examples, and those skilled in the art can easily understand other advantages and effects of the present invention from the contents disclosed in this specification. The present invention can also be implemented or applied through other different specific embodiments, and the details in this specification can also be modified or changed in various ways based on different viewpoints and applications without departing from the spirit of the present invention.

[0032] Before further describing the specific embodiments of the present invention, it should be understood that the scope of protection of the present invention is not limited to the specific embodiments described below; it should also be understood that the terms used in the examples of the present invention are for describing specific embodiments rather than for limiting the scope of protection of the present invention.

[0033] Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.

[0034] The present invention does not limit the sources of the raw materials used. Unless otherwise specified, the raw materials used in the present invention are common commercial products in the technical field.

[0035] Example 1

[0036] The volume of carboxylation reactor is 3.5 cubic meters, and wherein material is 2-naphthol salt, and quality is 1700 kilograms, and volume is 1.5 cubic meters, and remaining 2 cubic meters are full of carbon dioxide gas.After carboxylation reaction terminates, the pressure in the reactor is 0.55MPa, and after the first-level is pressed, the pressure is 0.4MPa, and after the second-level is pressed, the pressure is 0.2MPa, and after the three-level is pressed, the pressure in the reactor is reduced to 0.1MPa, and the order of three-level pressure-equalizing tanks, the second-level pressure-equalizing tanks, and the first-level pressure-equalizing tank is reversely pressed to the carboxylation reactor, and the carbon dioxide of 2 cubic meters of 0.45MPa is recovered in the pressure-equalizing tank, and the weight of carbon dioxide is 10 kilograms.

[0037] Since the carboxylation of 2-hydroxy-3-naphthoic acid is an intermittent reaction and needs to be completed in three times, each batch of materials needs to add carbon dioxide three times and be recycled three times. Each batch of materials can recycle 30 kg of carbon dioxide. 14 tons of carbon dioxide are added every day, and 1,200 kg of carbon dioxide can be recycled.

[0038] Example 2

[0039] The volume of carboxylation reactor is 3.5 cubic meters, and wherein material is 2-naphthol salt, and quality is 1700 kilograms, and volume is 1.5 cubic meters, and remaining 2 cubic meters are full of carbon dioxide gas.After carboxylation reaction terminates, pressure in the reactor is 0.55MPa, and after one-level equalizing pressure, pressure 0.35MPa, pressure 0.15MPa after secondary equalizing pressure, after three-level equalizing pressure, pressure in the reactor is reduced to 0.08MPa, according to the order of three-level equalizing pressure tank, secondary equalizing pressure tank, and one-level equalizing pressure tank, the carboxylation reactor is reversely equalizing pressure, and 2 cubic 0.47MPa carbon dioxide is recovered in the equalizing pressure tank, and the weight of carbon dioxide is 10.45 kilograms.

[0040] Since the carboxylation of 2-hydroxy-3-naphthoic acid is an intermittent reaction and needs to be completed in three times, each batch of materials needs to add carbon dioxide three times and be recycled three times. Each batch of materials can recover 31.35 kg of carbon dioxide. 14 tons of carbon dioxide are added every day, and 1,254 kg of carbon dioxide can be recovered.

[0041] Example 3

[0042] The volume of carboxylation reactor is 3.5 cubic meters, and wherein material is 2-naphthol salt, and quality is 1700 kilograms, and volume is 1.5 cubic meters, and remaining 2 cubic meters are full of carbon dioxide gas.After carboxylation reaction terminates, the pressure in the reactor is 0.55MPa, and after the first-level is pressed, the pressure is 0.5MPa, and after the second-level is pressed, the pressure is 0.3MPa, and after the three-level is pressed, the pressure in the reactor is reduced to 0.12MPa, and the order of three-level pressure-equalizing tanks, the second-level pressure-equalizing tanks, and the first-level pressure-equalizing tank is reversely pressed to the carboxylation reactor, and the carbon dioxide of 2 cubic meters of 0.43MPa is recovered in the pressure-equalizing tank, and the weight of carbon dioxide is 9.55 kilograms.

[0043] Since the carboxylation to produce 2-hydroxy-3-naphthoic acid is an intermittent reaction and needs to be completed in three times, each batch of materials needs to add carbon dioxide three times and be recovered three times. Each batch of materials can recover 28.65 kg of carbon dioxide and obtain 960 kg of 2-hydroxy-3-naphthoic acid. 14 tons of carbon dioxide are added every day, and 1,146 kg of carbon dioxide can be recovered.

[0044] Comparative Example 1

[0045] Compared with Example 1, only one level of pressure equalizing device is used.

[0046] The volume of the carboxylation reactor is 3.5 cubic meters, of which the material is 2-naphthol salt, with a mass of 1700 kg, the material volume is 1.5 cubic meters, and the remaining 2 cubic meters are filled with carbon dioxide gas. After the carboxylation reaction is completed, the pressure in the reactor is 0.55 MPa. After a first-level pressure equalization, the pressure in the reactor drops to 0.35 MPa, and 2 cubic meters of 0.2 MPa carbon dioxide are recovered in the pressure equalization tank, and the weight of carbon dioxide is 4.44 kg.

[0047] Since the carboxylation of 2-hydroxy-3-naphthoic acid is an intermittent reaction and needs to be completed in three times, each batch of materials needs to add carbon dioxide three times and be recycled three times. Each batch of materials can recycle 13.325 kg of carbon dioxide. 14 tons of carbon dioxide are added every day, and 533 kg of carbon dioxide can be recycled every day.

[0048] Comparative Example 2

[0049] Compared with Example 1, only two-stage pressure equalizing devices are used.

[0050] The volume of the carboxylation reactor is 3.5 cubic meters, of which the material is 2-naphthol salt, with a mass of 1700 kg, the material volume is 1.5 cubic meters, and the remaining 2 cubic meters are filled with carbon dioxide gas. After the carboxylation reaction is completed, the pressure in the reactor is 0.55 MPa. After the secondary pressure equalization, the pressure in the reactor drops to 0.25 MPa, and 2 cubic meters of 0.3 MPa carbon dioxide are recovered in the pressure equalization tank, and the weight of carbon dioxide is 6.66 kg.

[0051] Since the carboxylation of 2-hydroxy-3-naphthoic acid is an intermittent reaction and needs to be completed in three times, each batch of materials needs to add carbon dioxide three times and be recycled three times. Each batch of materials can recover 19.98 kg of carbon dioxide. 14 tons of carbon dioxide are added every day, and 799.2 kg of carbon dioxide can be recovered every day.

[0052] Example 1 The carboxylation reactor is connected to a set of three-stage pressure equalizing devices, and 30 kg of carbon dioxide can be recovered from each batch of materials. Comparative Example 1 The carboxylation reactor is connected to a set of one-stage pressure equalizing devices, and 13.325 kg of carbon dioxide can be recovered from each batch of materials; Comparative Example 2 The carboxylation reactor is connected to a set of two-stage pressure equalizing devices, and 19.98 kg of carbon dioxide can be recovered from each batch of materials.

[0053] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, rather than to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions of the technical solution of the present invention by ordinary technicians in this field do not deviate from the essence and scope of the technical solution of the present invention.

Claims

1. A device for reducing the cost of carboxylation to produce 2-hydroxy-3-naphthoic acid, characterized in that: The carboxylation reactor is connected to a three-stage pressure equalizing device.

2. The device according to claim 1, characterized in that The three-stage pressure equalizing device is composed of three pressure equalizing tanks connected in parallel.

3. The application of the device as described in any one of claim 1-2 in reducing the cost of carboxylation 2-hydroxy-3-naphthoic acid.

4. A production process for reducing the cost of preparing 2-hydroxy-3-naphthoic acid by carboxylation, characterized in that: Use the device according to any one of claims 1-2.

5. The production process according to claim 4, characterized in that: The following steps are involved: S1. After the carboxylation reaction is completed, a first-level pressure equalizing tank is used to perform first-level pressure equalization on the carboxylation reactor; S2, after the first-level pressure equalization, using a second-level pressure equalization tank to perform second-level pressure equalization on the carboxylation reactor; S3, after the secondary pressure equalization, a third-stage pressure equalization tank is used to perform third-stage pressure equalization on the carboxylation reactor; S4, after three-stage equalization, the reaction products are collected and the materials required for the next reaction are introduced; S5, according to the order of the three-stage pressure equalizing tank, the second-stage pressure equalizing tank, and the first-stage pressure equalizing tank, the carboxylation reaction kettle is subjected to reverse pressure equalization; S6, introducing carbon dioxide into the carboxylation reaction kettle to make up the pressure and continue the reaction.

6. The production process according to claim 5, characterized in that: In the step S1, the endpoint pressure value of the first-stage equalization pressure is 0.35-0.5 MPa, preferably 0.4 MPa.

7. The production process according to claim 5, characterized in that: In the step S2, the endpoint pressure value of the secondary pressure equalization is 0.15-0.3 MPa, preferably 0.2 MPa.

8. The production process according to claim 5, characterized in that: In the step S3, the terminal pressure value of the three-stage equalization pressure is 0.08-0.12 MPa, preferably 0.1 MPa.

9. The production process according to claim 5, characterized in that: In the step S6, the replenishing pressure is 0.5-0.6 MPa.

10. The production process according to claim 9, characterized in that: In the step S6, the replenishing pressure is 0.6 MPa.