CN212263211U - Single-tube reaction device for preparing RT base condensation liquid - Google Patents
Single-tube reaction device for preparing RT base condensation liquid Download PDFInfo
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- CN212263211U CN212263211U CN202020500625.5U CN202020500625U CN212263211U CN 212263211 U CN212263211 U CN 212263211U CN 202020500625 U CN202020500625 U CN 202020500625U CN 212263211 U CN212263211 U CN 212263211U
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Abstract
The invention belongs to the field of fine chemical engineering, and relates to a single-tube reaction device for preparing RT base condensation liquid, which is characterized in that: the single-tube reaction device comprises a single-tube reactor, wherein a film falling tube and a preheating tube are arranged in the single-tube reactor, and a heating jacket is arranged outside the single-tube reactor; the single-tube reactor is connected with a water bath system and a vacuum system, the upper part of the single-tube reactor is provided with a gas-liquid separation tube, the lower part of the single-tube reactor is provided with a raw material inlet, a condensation liquid discharge tube and a condensation liquid tank, and the raw material inlet is connected with a preheating tube; the gas-liquid separation pipe is connected with a condensation liquid tank through a pressure balance pipe. Adopt the utility model discloses a device can shorten reaction dwell time to a great extent, has avoided the backmixing of material simultaneously, and this is favorable to reducing the production of condensation reaction accessory substance.
Description
Technical Field
The invention belongs to the field of fine chemical engineering, and relates to preparation of a rubber antioxidant intermediate RT base.
Background
RT base (p-aminodiphenylamine) is widely applied to the fields of rubber auxiliaries, dyes, textile, printing, pharmaceutical industry and the like, and is mainly used for producing rubber antioxidants IPPD, 6PPD and the like.
At present, the yield of domestic RT base production is 200 kt/a. With the development of the rubber industry, the demand of rubber antioxidants is steadily increasing.
RT-sauce is produced mainly by the aniline method, the diphenylamine method, the formanilide method and the nitrobenzene method. The nitrobenzene process is the mainstream process for producing the RT base at present.
The production of RT base by the nitrobenzene method can generate impurities such as 2-aminodiphenylamine, phenazine and the like, and particularly the boiling points of the two substances are close to that of the RT base, so that the rectification of the RT base is difficult, and the quality of the RT base is influenced.
At present, RT base research mainly comprises the steps of optimizing a nitrobenzene method RT base process, improving the recovery efficiency of a phase transfer catalyst, reducing energy consumption and material consumption, inhibiting the generation of byproducts, improving the purity of RT base and the like.
The condensation reaction in the production of RT base is mainly carried out by adopting a kettle type continuous condensation process, but the kettle type process needs to be stirred vigorously, the fluid in the kettle can generate a back mixing phenomenon, the back mixing can cause the selectivity of a target product of the reaction to be reduced, impurities such as azobenzene, phenazine, o (sub) nitrodiphenylamine and the like in a condensation liquid can influence the purity of a finished product of the RT base, and the azobenzene can be reduced into aniline, but the energy consumption and the material consumption of the RT base production can be increased.
Disclosure of Invention
The utility model aims at providing a preparation RT base condensation liquid's single tube reaction unit can shorten reaction dwell time to a great extent, has avoided the backmixing of material simultaneously, reduces the production of condensation reaction accessory substance.
The utility model provides a single tube reaction unit of preparation RT sushi condensation liquid, aniline, nitrobenzene, the mixture of tetramethyl ammonium hydroxide is carried into single tube reaction unit by the raw material pump as reaction raw materials, reaction unit's water bath preheats the material in the material conveying pipe, the raw materials after preheating overflows from material conveying pipe top, the material of overflow is by the effect of gravity, disperse at falling liquid film outer wall uniformly, the raw materials carries and reacts the moisture that produces and gasifies at the outer wall of falling liquid film pipe, take out the reaction unit by vacuum system, the condensation liquid that the reaction generated flows down along falling liquid film outer wall, flow from the condensation liquid outlet pipe.
The technical solution of the utility model is as follows: the single-tube reaction device for preparing the RT base condensation liquid is characterized in that: the single-tube reaction device comprises a single-tube reactor, wherein a film falling tube and a preheating tube are arranged in the single-tube reactor, and a heating jacket is arranged outside the single-tube reactor; the single-tube reactor is connected with a water bath system and a vacuum system, the upper part of the single-tube reactor is provided with a gas-liquid separation tube, the lower part of the single-tube reactor is provided with a raw material inlet, a condensation liquid discharge tube and a condensation liquid tank, and the raw material inlet is connected with a preheating tube; the gas-liquid separation pipe is connected with a condensation liquid tank through a pressure balance pipe.
The falling film tube made of general drop and corrosion-resistant high-strength special alloy steel is resistant to pressure of 15.0MPa at most and resistant to temperature of 100 ℃ at most.
The water bath system comprises a water bath inlet pipe, a water bath overflow pipe, a constant-temperature water bath tank with electric heating and a circulating water bath pump; the water bath inlet pipe is arranged at the lower part of the single-tube reactor, and the water bath overflow pipe extends into the single-tube reactor.
The water bath inlet pipe and the water bath overflow pipe which are made of the corrosion-resistant high-strength special alloy steel have the maximum pressure resistance of 15.0MPa and the maximum temperature resistance of 100 ℃.
The temperature control range of the water bath system is 60-85 ℃.
The vacuum system comprises a vacuum pump, an aniline water condenser and an aniline water tank, wherein the aniline water tank is connected with a gas-liquid separation pipe at the upper part of the single-tube reactor.
The aniline water condenser made of the stainless steel material can resist temperature of 0-100 ℃.
The vacuum pressure of the vacuum system is less than 0.085 MPa.
The heating jacket is heated by an electric furnace wire, and the heating temperature is 60-85 ℃.
The device of the utility model adds a proper amount of deionized water into the constant temperature water bath before use, opens the heater to heat the temperature of the water bath in the constant temperature water bath to a preset temperature, opens the constant temperature water bath pump, and the water bath is returned to the constant temperature water bath through the overflow pipe after being full of water bath; turning on an external heating jacket power supply; starting a vacuum pump; after the temperature and the pressure of the reaction tube reach the synthesis requirements, a raw material pump is started to carry out condensation reaction.
Adopt the utility model discloses a device can shorten reaction dwell time to a great extent, has avoided the backmixing of material simultaneously, and this is favorable to reducing the production of condensation reaction accessory substance.
The technical advantages of the utility model are that:
the utility model discloses the device can shorten reaction dwell time, avoid the material back mixing among the condensation process to a great extent, reduces the production of condensation reaction accessory substance, improves the product yield, reduces tetramethyl ammonium hydroxide's decomposition.
Adopt the utility model discloses a device carries out condensation reaction, and the conversion rate of nitrobenzene is more than or equal to 99%, and phenazine's selectivity is less than or equal to 0.05%, and the condensation liquid that adopts this device to prepare carries out reduction reaction, and 2-aminodiphenylamine's selectivity is less than or equal to 0.05%.
Drawings
FIG. 1 is a schematic structural diagram of a single-tube reaction device for preparing RT base condensation liquid according to the embodiment of the present invention.
In the figure, 1-a constant temperature water bath; 2-a heater; 3-constant temperature water bath pump; 4-water bath inlet pipe; 5, a water bath overflow pipe; 6-heating jacket; 7-preheating tube; 8, a membrane reduction tube; 9-condensation liquid discharging pipe; 10-condensation liquid tank; 11-a pressure balance tube; 12-a gas-liquid separation tube; 13-a condenser; 14-aniline water tank; 15-vacuum pump.
Detailed Description
The present invention will be further described with reference to the following embodiments and accompanying drawings.
The single-tube reaction device consists of a falling film tube, a water bath system, a vacuum system and an external heating jacket.
Examples
Referring to the attached figure 1, the single-tube reaction device for preparing the RT base condensed liquid mainly comprises a single-tube reactor, wherein a membrane lowering tube 8 and a preheating tube 7 are arranged in the single-tube reactor, and a heating jacket 6 is arranged outside the single-tube reactor; the single-tube reactor is connected with a water bath system and a vacuum system, the upper part of the single-tube reactor is provided with a gas-liquid separation tube 12, the lower part of the single-tube reactor is provided with a raw material inlet, a condensation liquid discharge tube 9 and a condensation liquid tank 10, and the raw material inlet is connected with a preheating tube 7; the gas-liquid separation pipe 12 is connected to the condensation liquid tank 10 through a pressure balance pipe 11.
In the embodiment, the corrosion-resistant high-strength special alloy steel falling film pipe 8 can bear the pressure of 15.0MPa at most and can resist the temperature of 100 ℃ at most.
In the embodiment, the water bath system comprises a water bath inlet pipe 4, a water bath overflow pipe 5, a constant temperature water bath 1 with a heater 2 and a circulating constant temperature water bath pump 3; a water bath inlet pipe 4 is arranged at the lower part of the single-tube reactor, and a water bath overflow pipe 5 extends into the single-tube reactor; a water bath inlet pipe 4 and a water bath overflow pipe 5 which are made of corrosion-resistant high-strength special alloy steel, the maximum pressure resistance is 15.0MPa, and the maximum temperature resistance is 100 ℃; the temperature control range of the water bath system is 60-85 ℃.
In the embodiment, the vacuum system comprises a vacuum pump 15, an aniline water condenser 13 and an aniline water tank 14, wherein the aniline water tank 14 is connected with a gas-liquid separation pipe 12 at the upper part of the single-tube reactor; the aniline water condenser made of stainless steel resists temperature of 0-100 ℃; the vacuum pressure of the vacuum system is less than 0.085 MPa.
In the embodiment, the heating jacket 6 is heated by an electric furnace wire at the temperature of 60-85 ℃.
The device of the embodiment is characterized in that a heater 2 on a constant-temperature water bath 1 is started before use, water bath reaching the use temperature enters a reaction device through a water bath inlet pipe 4 by a constant-temperature water bath pump 3, the water bath overflows out of the reaction device through a water bath overflow pipe 5 after being filled with the water bath, an external heating jacket 6 is started to carry out external heating, a vacuum pump 15 is started, after the reaction device reaches the use temperature and pressure, premixed raw materials are conveyed into the reaction device through a preheating pipe 7, the preheated materials overflow from the top of the preheating pipe 7 and are uniformly dispersed on the outer surface of a falling film pipe 8, water and a small amount of aniline in the materials on the outer wall of the falling film pipe 8 are heated and gasified, the materials on the outer wall of the falling film pipe fall to the bottom of the reaction device along the falling film pipe under the action of gravity, flow out of a condensation liquid discharge pipe 9 and are collected into a condensation liquid tank 10, the condensation liquid tank 10 is, aniline water vaporized on the surface of the falling film tube is pumped out of the gas-liquid separator tube 12 by a vacuum pump 15, the pumped gas phase passes through a condenser 13, and the condensed liquid phase is collected into an aniline water tank 14.
The device of the embodiment is adopted for condensation reaction, the conversion rate of nitrobenzene is more than or equal to 99 percent, the selectivity of phenazine is less than or equal to 0.05 percent, and the condensation liquid prepared by the device is adopted for reduction reaction, and the selectivity of 2-aminodiphenylamine is less than or equal to 0.05 percent.
Claims (9)
1. A single-tube reaction device for preparing RT base condensation liquid is characterized in that: the single-tube reaction device comprises a single-tube reactor, wherein a film falling tube and a preheating tube are arranged in the single-tube reactor, and a heating jacket is arranged outside the single-tube reactor; the single-tube reactor is connected with a water bath system and a vacuum system, the upper part of the single-tube reactor is provided with a gas-liquid separation tube, the lower part of the single-tube reactor is provided with a raw material inlet, a condensation liquid discharge tube and a condensation liquid tank, and the raw material inlet is connected with a preheating tube; the gas-liquid separation pipe is connected with a condensation liquid tank through a pressure balance pipe.
2. The single-tube reaction device for preparing RT base condensation solution according to claim 1, wherein: the falling film pipe made of the corrosion-resistant high-strength special alloy steel is resistant to pressure of 15.0MPa at most and resistant to temperature of 100 ℃ at most.
3. The single-tube reaction device for preparing RT base condensation solution according to claim 1, wherein: the water bath system comprises a water bath inlet pipe, a water bath overflow pipe, a constant temperature water bath tank with electric heating and a circulating water bath pump; the water bath inlet pipe is arranged at the lower part of the single-tube reactor, and the water bath overflow pipe extends into the single-tube reactor.
4. The single-tube reaction device for preparing RT base condensation solution according to claim 3, wherein: the water bath inlet pipe and the water bath overflow pipe which are made of corrosion-resistant high-strength special alloy steel have the maximum pressure resistance of 15.0MPa and the maximum temperature resistance of 100 ℃.
5. The single-tube reaction device for preparing RT base condensation solution according to claim 1, wherein: the temperature control range of the water bath system is 60-85 ℃.
6. The single-tube reaction device for preparing RT base condensation solution according to claim 3, wherein: the vacuum system comprises a vacuum pump, an aniline water condenser and an aniline water tank, wherein the aniline water tank is connected with a gas-liquid separation pipe at the upper part of the single-tube reactor.
7. The single-tube reaction device for preparing RT base condensation solution according to claim 6, wherein: the aniline water condenser made of stainless steel can resist temperature of 0-100 ℃.
8. The single-tube reaction device for preparing RT base condensation solution according to claim 1 or 6, characterized in that: the vacuum pressure of the vacuum system is less than 0.085 MPa.
9. The single-tube reaction device for preparing RT base condensation solution according to claim 1, wherein: the heating jacket is heated by an electric furnace wire at the heating temperature of 60-85 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020500625.5U CN212263211U (en) | 2020-04-08 | 2020-04-08 | Single-tube reaction device for preparing RT base condensation liquid |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202020500625.5U CN212263211U (en) | 2020-04-08 | 2020-04-08 | Single-tube reaction device for preparing RT base condensation liquid |
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| CN212263211U true CN212263211U (en) | 2021-01-01 |
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| CN202020500625.5U Active CN212263211U (en) | 2020-04-08 | 2020-04-08 | Single-tube reaction device for preparing RT base condensation liquid |
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Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee after: CHINA PETROLEUM & CHEMICAL Corp. Patentee after: SINOPEC NANJING CHEMICAL RESEARCH INSTITUTE Co.,Ltd. Address before: Liuhe District of Nanjing City, Jiangsu province 210048 geguan Road No. 699 Patentee before: SINOPEC NANJING CHEMICAL RESEARCH INSTITUTE Co.,Ltd. Patentee before: CHINA PETROLEUM & CHEMICAL Corp. |
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