Phenolic water recycling device in m-trifluoromethylphenol synthesis process

The phenol water recovery and reuse device recovers the phenol water phase to the reboiler for heating and evaporation and returns it to the hydrolysis kettle to provide heat energy. This solves the problem of resource waste and treatment costs caused by direct discharge of phenol water and achieves efficient temperature control and improved reaction efficiency.

CN223892597UActive Publication Date: 2026-02-10WEIFANG SINO AGRI UNION CHEM CO LTD
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Patent Information

Application Number
CN202520398027.4
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2025-03-07
Publication Date
2026-02-10
Estimated Expiration
2035-03-07

AI Technical Summary

Technical Problem

In the existing technology, the aqueous phenol phase generated in the synthesis process of m-trifluoromethylphenol is directly discharged, resulting in water waste and increased wastewater treatment costs, and it also contains a small amount of phenol that needs to be treated.

Method used

A phenol water recovery and reuse device was designed, including a hydrolysis kettle, an ester water separation tank, a reboiler, and a gas buffer tank. After oil-water separation, the aqueous phase is recovered to the reboiler for heating and evaporation, and the generated phenol water vapor is returned to the hydrolysis kettle to provide heat energy, maintaining a constant temperature and being reused.

Benefits of technology

It reduces environmental pollution and wastewater treatment costs, enables the reuse of phenol water, improves reaction efficiency and temperature control, and reduces the risk of equipment damage.

✦ Generated by Eureka AI based on patent content.

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Abstract

The phenol water recycling and reusing device in the m-trifluoromethylphenol synthesis process comprises a hydrolysis kettle, the upper end of the hydrolysis kettle is provided with a urea solution inlet and a diazonium salt solution inlet, the lower end of the hydrolysis kettle is provided with a solution outlet and a gas inlet, the solution outlet is communicated with an ester water layering tank through a pipeline, and the gas inlet is communicated with the ester water layering tank through a pipeline. The ester water layering tank is communicated with a reboiler, and the reboiler is communicated with the gas inlet. The water phase generated by the ester water layering tank is recycled, so that the problem of environmental pollution caused by direct discharge is reduced, and the wastewater treatment cost is reduced; the recycled water phase is recycled and introduced into the reboiler to be heated and evaporated, the phenol water vapor obtained after evaporation is introduced into the hydrolysis kettle, heat energy is provided for the hydrolysis kettle, the temperature in the hydrolysis kettle is kept constant, and recycling of the water phase is achieved.
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Description

TECHNICAL FIELD

[0001] The utility model relates to a recycling device, specifically, to a phenol water recycling device in m-trifluoromethyl phenol synthesis process. BACKGROUND

[0002] M-trifluoromethyl phenol is a chemical substance, which is generated by a reactor with 53% sulfuric acid as raw material and trifluoromethyl aniline to form aniline sulfate, and the aniline sulfate is reacted with nitrosyl sulfuric acid to form a diazonium salt solution; the diazonium salt solution is continuously sprayed into a hydrolysis kettle, and urea is introduced to carry out hydrolysis reaction, and the mixed solution after reaction is condensed and enters an ester water separation tank, and the organic phase and the aqueous phase of m-trifluoromethyl phenol are obtained by phase separation, then the organic phase of m-trifluoromethyl phenol is continuously treated, and phenol crude product and water are distilled out, and the phenol crude product is taken to negative pressure to obtain phenol.

[0003] And the aqueous phase obtained by the ester water separation tank is often discharged as waste water, which not only causes waste of water resources, but also needs to be treated during the discharge process to reach the discharge standard, thereby increasing the cost of waste water discharge, which is the deficiency of the prior art. UTILITY MODEL CONTENT

[0004] The utility model aims at solving the problems in the background art, and further provides a phenol water recycling device in m-trifluoromethyl phenol synthesis process.

[0005] The utility model solves the technical problems by adopting the technical scheme that a phenol water recycling device in m-trifluoromethyl phenol synthesis process comprises a hydrolysis kettle, a urea solution inlet and a diazonium salt solution inlet are arranged at the upper end of the hydrolysis kettle, a solution outlet and a gas inlet are arranged at the lower end of the hydrolysis kettle, the solution outlet is communicated with an ester water separation tank through a pipeline, the ester water separation tank is communicated with a reboiler, and the reboiler is communicated with the gas inlet.

[0006] Further improvement of the utility model is that the ester water separation tank is provided with an m-trifluoromethyl phenol organic phase outlet and an aqueous phase outlet, and the aqueous phase outlet is communicated with the reboiler.

[0007] Further improvement of the utility model is that an ester water low-position tank is further arranged between the ester water separation tank and the reboiler, the inlet of the ester water low-position tank is communicated with the aqueous phase outlet of the ester water separation tank, and the outlet of the ester water low-position tank is communicated with the inlet of the reboiler.

[0008] Further improvement of the utility model is that the ester water low-position tank is further communicated with a water pump to supplement tap water into the ester water low-position tank.

[0009] The further improvement of the utility model still has, gas buffer tank is arranged between hydrolysis kettle and reboiler still, the import of gas buffer tank is linked with the export of reboiler, and the export of gas buffer tank is linked with the gas import of hydrolysis kettle.

[0010] The further improvement of the utility model still has, gas buffer tank is arranged between hydrolysis kettle and reboiler still, the import of gas buffer tank is linked with the export of reboiler, and the export of gas buffer tank is linked with the gas import of hydrolysis kettle.

[0011] The further improvement of the utility model still has, gas buffer tank is arranged between hydrolysis kettle and reboiler still, the import of gas buffer tank is linked with the export of reboiler, and the export of gas buffer tank is linked with the gas import of hydrolysis kettle.

[0012] The beneficial effect of the utility model is: the water phase generated by ester water layering tank is recycled, the environmental pollution problem caused by direct discharge is reduced, and the wastewater treatment cost is reduced, the recycled water phase is reused, is passed into reboiler and is heated and evaporated, and the phenol water steam obtained after evaporation is passed into hydrolysis kettle, heat energy is provided for the hydrolysis kettle, the temperature in the hydrolysis kettle is kept constant, and the reuse of water phase is realized. BRIEF DESCRIPTION OF DRAWINGS

[0013] Figure 1 The utility model discloses a specific embodiment structure schematic view.

[0014] In the drawing, 1 is hydrolysis kettle, 11 is diazonium salt solution import, 12 is urea solution import, 13 is solution export, 14 is gas import, 2 is ester water layering tank, 21 is meta-trifluoromethylphenol organic phase export, 22 is water phase export, 3 is gas buffer tank, 31 is export, 32 is import, 4 is reboiler, 5 is water pump, 6 is ester water low-level tank. DETAILED DESCRIPTION

[0015] The technical scheme in the utility model embodiment will be described clearly and completely in combination with the drawings in the utility model embodiment, and obviously, the described embodiment is only a part of the embodiment of the utility model, not all the embodiment. Based on the embodiment in the utility model, all other embodiments obtained by the ordinary skill in the art without making creative labor belong to the range of protection of the utility model. The utility model is further illustrated in combination with the drawings and the embodiment:

[0016] As Figure 1As shown, a kind of phenol water recycling device in m-trifluoromethyl phenol synthesis process, including hydrolysis kettle 1, the upper end of the hydrolysis kettle 1 is provided with urea solution inlet 12 and diazonium salt solution inlet 11, the lower end of the hydrolysis kettle 1 is provided with solution outlet 13 and gas inlet 14, the solution outlet 13 is communicated with ester water layering tank 2 by pipeline, the ester water layering tank 2 is communicated with reboiler 4, and the reboiler 4 is communicated with the gas inlet 14.

[0017] In the application, hydrolysis kettle 1 is as the core place of reaction. Diazonium salt solution is introduced into hydrolysis kettle 1 through diazonium salt solution inlet 11, and 25% urea is introduced into urea solution inlet 12, so that urea and diazonium salt solution are subjected to hydrolysis reaction, the solution after reaction is introduced into ester water layering tank 2 through solution outlet 13, and oil-water separation is carried out in ester water layering tank 2, and the water phase obtained after separation is introduced into reboiler 4, and phenol water steam is generated by heating and evaporation in reboiler 4, and the phenol water steam is introduced into hydrolysis kettle 1 again. These phenol water steams have multiple effects in the hydrolysis reaction. First, the phenol water steam is the energy source required for reaction, and provides heat energy for the hydrolysis reaction. Second, the phenol water steam is mixed uniformly in the hydrolysis kettle 1 reactor, which can help to improve the reaction rate and reaction efficiency. In addition, the phenol water steam can also maintain the temperature of the hydrolysis reaction, so that it is kept at the optimum reaction condition.

[0018] Therefore, the application recycles the water phase generated by ester water layering tank 2, reduces the environmental pollution problem caused by direct discharge, and reduces the wastewater treatment cost. By recycling the water phase and introducing it into reboiler 4 for heating and evaporation, the phenol water steam obtained after evaporation is introduced into hydrolysis kettle 1, which provides heat energy for hydrolysis kettle 1 and keeps the temperature in hydrolysis kettle 1 constant, thereby realizing the recycling of the water phase.

[0019] Further, the ester water layering tank 2 is provided with m-trifluoromethyl phenol organic phase outlet 21 and water phase outlet 22, and the water phase outlet 22 is communicated with reboiler 4. The m-trifluoromethyl phenol organic phase outlet 21 is used to collect and lead out the organic phase containing the target product, and the water phase outlet 22 is communicated with reboiler 4, thereby realizing the recycling of the water phase.

[0020] Further, the ester water layering tank 2 and reboiler 4 are further provided with ester water low-level tank 6, the inlet of the ester water low-level tank 6 is communicated with the water phase outlet 22 of the ester water layering tank 2, and the outlet of the ester water low-level tank 6 is communicated with the inlet of the reboiler 4. The ester water low-level tank 6 plays a role in temporarily storing the water phase.

[0021] Further, the ester water low-level tank 6 is further communicated with water pump 5, and tap water is supplemented into the low-level tank to adjust the concentration of the water phase, thereby further enhancing the controllability and stability of the system.

[0022] Since the process of the application will produce a large gas pressure change, which will cause the pipe rupture, equipment damage and other problems, in order to avoid the occurrence of such phenomena, the application is also provided with a gas buffer tank 3 between the hydrolysis kettle 1 and the reboiler 4, the inlet 31 of the gas buffer tank 3 is communicated with the outlet of the reboiler 4, and the outlet 32 of the gas buffer tank 3 is communicated with the gas inlet 14 of the hydrolysis kettle 1. The gas buffer tank 3 plays a role of buffering pressure by adjusting the gas pressure in the pipeline, so that the pipeline system is protected, and the safe and stable operation of the equipment is ensured.

[0023] Further, the gas buffer tank 3 is communicated with the hydrolysis kettle 1 through a first pipeline, the first pipeline is provided with a first pressure gauge 7, the gas buffer tank 3 is communicated with the reboiler 4 through a second pipeline, and the second pipeline is provided with a second pressure gauge 8, so that the workers can know the pressure in the pipeline in time.

[0024] The above shows and describes the basic principle, main features and advantages of the utility model. The skilled in the art should understand that the utility model is not limited by the above embodiments, and the above embodiments and the description in the specification are only to illustrate the principle of the utility model, and various changes and improvements of the utility model can be made without departing from the spirit and scope of the utility model, and these changes and improvements all fall within the scope of the utility model. The scope of protection of the utility model is defined by the appended claims and their equivalents.

Claims

1. A device for recovering and reusing phenolic water in the synthesis process of m-trifluoromethylphenol, comprising a hydrolysis reactor, characterized in that, The upper end of the hydrolysis vessel is provided with a urea solution inlet and a diazonium salt solution inlet, and the lower end of the hydrolysis vessel is provided with a solution outlet and a gas inlet. The solution outlet is connected to the ester-water separation tank through a pipe, the ester-water separation tank is connected to the reboiler, and the reboiler is connected to the gas inlet.

2. The phenol water recovery and reuse device in the m-trifluoromethylphenol synthesis process according to claim 1, characterized in that, The ester-water separation tank is equipped with an organic phase outlet of m-trifluoromethylphenol and an aqueous phase outlet, and the aqueous phase outlet is connected to the reboiler.

3. The phenol water recovery and reuse device in the m-trifluoromethylphenol synthesis process according to claim 2, characterized in that, An ester-water low-level tank is also provided between the ester-water stratification tank and the reboiler. The inlet of the ester-water low-level tank is connected to the water phase outlet of the ester-water stratification tank, and the outlet of the ester-water low-level tank is connected to the inlet of the reboiler.

4. The phenol water recovery and reuse device in the m-trifluoromethylphenol synthesis process according to claim 3, characterized in that, The ester water low-level tank is also connected to a water pump to replenish tap water into the ester water low-level tank.

5. The phenol water recovery and reuse device in the m-trifluoromethylphenol synthesis process according to claim 1, characterized in that, A gas buffer tank is also provided between the hydrolysis vessel and the reboiler. The inlet of the gas buffer tank is connected to the outlet of the reboiler, and the outlet of the gas buffer tank is connected to the gas inlet of the hydrolysis vessel.

6. The phenol water recovery and reuse device in the m-trifluoromethylphenol synthesis process according to claim 5, characterized in that, The gas buffer tank and the hydrolysis reactor are connected by a first pipeline, and a first pressure gauge is installed on the first pipeline.

7. The phenol water recovery and reuse device in the m-trifluoromethylphenol synthesis process according to claim 6, characterized in that, The gas buffer tank and the reboiler are connected by a second pipe, and a second pressure gauge is installed on the second pipe.