A production apparatus and process for fine chemicals

Abstract

The application is suitable for the field of fine chemical technology, and provides a production device and process of fine chemicals, which comprises a raw material mixing tank, a reaction rectifying tower, a light-removing tower and a heavy-removing tower, the inlet material of the raw material mixing tank is a mixture of phenol, ethylene carbonate and catalyst, the material outlet of the raw material mixing tank is connected with the inlet of the reaction rectifying tower through a reaction preheater, the tower kettle material outlet of the reaction rectifying tower is connected with the material inlet of the light-removing tower, the tower kettle material outlet of the light-removing tower is connected with the material inlet of the heavy-removing tower, and the tower kettle material outlet of the heavy-removing tower is the catalyst concentrate outlet.The process is simple and efficient, the conversion rate of ethylene carbonate is 100%, and the selectivity of phenoxy ethanol is > 95%; the device structure is simple, the operation is convenient, the product quality is stable and reliable, the device investment of phenoxy ethanol can be effectively reduced, and the market competitiveness of the product can be improved.

Description

Technical Field

[0001] The present invention belongs to the technical field of fine chemicals, and in particular relates to a production device and process for fine chemicals. Background Art

[0002] Phenoxyethanol, also known as ethylene glycol phenyl ether (EPH), is a colorless, viscous liquid with a high boiling point and low volatility. EPH has a wide range of applications in the pharmaceutical, daily chemical, coatings, inks, pesticide, and other fields. EPH is also a hypoallergenic, low-toxic, chemically stable, highly effective, broad-spectrum preservative and fungicide, effective against bacteria, molds, and yeasts. EPH is soluble in both water and oil, exhibiting excellent overall properties, leading to its increasing use in the daily chemical industry.

[0003] Currently, methods for synthesizing phenoxyethanol include the chloroethanol method and the ethylene oxide method, with the ethylene oxide method being the predominant industrial production method. The ethylene oxide method uses phenol and ethylene oxide as raw materials. However, ethylene oxide is flammable, explosive, and carcinogenic, placing stringent requirements on both equipment and process.

[0004] Therefore, in view of the above situation, there is an urgent need to develop a simple and efficient production device and process for fine chemicals to overcome the shortcomings in current practical applications. Summary of the Invention

[0005] The purpose of the embodiments of the present invention is to provide a production device and process for fine chemicals, aiming to solve the problems mentioned in the above background technology.

[0006] An embodiment of the present invention is implemented as follows: a production device for fine chemicals includes a raw material mixing tank, a reactive distillation tower, a light-removing tower and a heavy-removing tower, wherein the inlet materials of the raw material mixing tank are phenol, ethylene carbonate and a catalyst mixture, the material outlet of the raw material mixing tank is connected to the inlet of the reactive distillation tower through a reaction preheater, the tower bottom material outlet of the reactive distillation tower is connected to the material inlet of the light-removing tower, the tower bottom material outlet of the light-removing tower is connected to the material inlet of the heavy-removing tower, and the tower bottom material outlet of the heavy-removing tower is an outlet for catalyst concentrate.

[0007] According to a further technical solution, the raw material mixing tank is equipped with a stirrer and has a heating half pipe or a jacket.

[0008] A further technical solution is that the reaction distillation tower is equipped with a reaction condenser, a reaction reflux buffer tank and a reaction reboiler. The top of the reaction distillation tower is connected to the inlet of the reaction reflux buffer tank through the reaction condenser, and the outlet material of the reaction reflux buffer tank is refluxed to the top of the reaction distillation tower. The reaction condenser also has a CO2 outlet; the tower bottom material outlet of the reaction distillation tower is connected to the reaction reboiler, and the outlet material of the reaction reboiler is refluxed to the tower bottom of the reaction distillation tower.

[0009] A further technical solution is that the light removal tower is equipped with a light removal condenser, a light removal reflux buffer tank and a light removal reboiler. The top of the light removal tower is connected to the inlet of the light removal reflux buffer tank through the light removal condenser, and the outlet material of the light removal reflux buffer tank is refluxed to the top of the light removal tower. The outlet of the light removal reflux buffer tank also includes a phenol outlet; the bottom material outlet of the light removal tower is connected to the light removal reboiler, and the outlet material of the light removal reboiler is refluxed to the bottom of the light removal tower.

[0010] A further technical solution is that the deweighting tower is equipped with a deweighting condenser, a deweighting reflux buffer tank and a deweighting reboiler. The top of the deweighting tower is connected to the inlet of the deweighting reflux buffer tank through the deweighting condenser, and the outlet material of the deweighting reflux buffer tank is refluxed to the top of the deweighting tower. The outlet of the deweighting reflux buffer tank also includes a phenoxyethanol outlet; the bottom material outlet of the deweighting tower is connected to the deweighting reboiler, and the outlet material of the deweighting reboiler is refluxed to the bottom of the deweighting tower.

[0011] A further technical solution is that the reaction distillation tower is a packed tower or a plate tower with 20 to 40 plates; the reaction condenser is equipped with a non-condensable gas material outlet; the reaction reflux buffer tank is equipped with an internal heating coil; the light removal tower is a packed tower or a plate tower with 30 to 60 plates; the light removal reflux buffer tank is equipped with an internal heating coil; the heavy removal tower is a packed tower or a plate tower with 30 to 60 plates; the heavy removal reflux buffer tank is equipped with an internal heating coil.

[0012] Another object of an embodiment of the present invention is to provide a production process for fine chemicals, comprising the following steps:

[0013] Step 1: Pretreatment of raw materials

[0014] Phenol, ethylene carbonate and catalyst from the boundary zone are heated and dissolved in a raw material mixing tank at a mass ratio of 1.1-2.0:1:0.005-0.08; the dissolved materials are transported to a reaction preheater for reaction pretreatment;

[0015] Step 2, synthesis of phenoxyethanol

[0016] The mixture of pretreated phenol, ethylene carbonate and catalyst is subjected to a total reflux synthesis reaction of phenoxyethanol in a reactive distillation tower. The main reaction of the synthesis is as follows:

[0017]

[0018] The carbon dioxide gas produced by the reaction is condensed in a reaction condenser and transported from the CO2 outlet to subsequent processing stages for recovery and treatment. The reactant mixture discharged from the reactor of the reaction distillation tower is transported to a lightness removal tower for distillation treatment. The conversion rate of ethylene carbonate after the reaction is 100%, and the selectivity of phenoxyethanol is 95% to 99.5%.

[0019] Step 3: Purification of phenoxyethanol

[0020] The reaction materials from the reactor of the reactive distillation tower are subjected to secondary distillation treatment in a light removal tower and a heavy removal tower to obtain a cosmetic-grade phenoxyethanol product, wherein the obtained phenoxyethanol content is ≥99.5% and the phenol content is <10 mg / kg.

[0021] A further technical solution is that in step 1, the temperature of the material after heating and dissolving in the raw material mixing tank is 50-80°C; the temperature of the material after treatment in the reaction preheater is 80-110°C; the catalyst is a type of ionic liquid, and its structural formula is as follows:

[0022]

[0023] In the formula, R1 is methyl, ethyl or propyl; R2 is butyl, pentyl, hexyl, heptyl or octyl.

[0024] A further technical solution is that in step 2, the top pressure of the reaction distillation tower is 15 to 100 kPa; the temperature of the material after condensation in the reaction condenser is 30 to 50°C; the temperature of the reactor of the reaction distillation tower is 130 to 190°C; the reaction reflux buffer tank is equipped with an internal heating coil, and when the temperature of the material is lower than 20°C, heating is turned on and heating is stopped until the temperature rises to 50°C.

[0025] A further technical solution is that in step 3, the reflux ratio of the top of the light removal tower is 0.5 to 3.0, and the phenol obtained at the top of the light removal tower can be recycled; the top pressure of the light removal tower is 1 to 15 kPa; the temperature of the material after condensation in the light removal condenser is 50 to 70 ° C; the temperature of the tower kettle of the light removal tower is 100 to 140 ° C; the light removal reflux buffer tank is equipped with an internal heating coil, and when the temperature of the material is lower than 50 ° C, the heating is turned on and the heating is stopped until the temperature rises to 60 ° C; the top of the heavy removal tower is The reflux ratio is 0.5 to 3.0, and the phenoxyethanol obtained at the top of the deweighting tower is cosmetic-grade; the catalyst concentrate obtained in the bottom of the deweighting tower is transported to the subsequent process section for recovery and treatment; the top pressure of the deweighting tower is 1 to 15 kPa; the temperature of the material after condensation in the deweighting condenser is 30 to 50°C; the temperature of the bottom of the deweighting tower is 110 to 160°C; the deweighting reflux buffer tank is equipped with an internal heating coil, and when the temperature of the material is lower than 20°C, heating is turned on and the heating is stopped when the temperature rises to 30°C.

[0026] The embodiments of the present invention provide a production device and process for fine chemicals, which have the following beneficial effects:

[0027] 1) The process is simple and efficient, with a conversion rate of ethylene carbonate of 100% and a selectivity of phenoxyethanol greater than 95%;

[0028] 2) The provided ionic liquid catalyst is stable and can be recycled, which is conducive to industrial application;

[0029] 3) The device has a simple structure, is easy to operate, and has stable and reliable product quality, which can effectively reduce the device investment of phenoxyethanol and improve the market competitiveness of the product. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] Figure 1 This is a schematic structural diagram of a fine chemical production device provided by an embodiment of the present invention.

[0031] In the figure: 1-raw material mixing tank, 2-reaction distillation tower, 3-light removal tower, 4-heavy removal tower, 5-reaction preheater, 6-reaction condenser, 7-light removal condenser, 8-heavy removal condenser, 9-reaction reflux buffer tank, 10-light removal reflux buffer tank, 11-heavy removal reflux buffer tank, 12-reaction reboiler, 13-light removal reboiler, 14-heavy removal reboiler, 15-phenol, ethylene carbonate and catalyst mixture, 16-CO2 outlet, 17-phenol outlet, 18-phenoxyethanol outlet, 19-catalyst concentrate outlet. DETAILED DESCRIPTION

[0032] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention.

[0033] The specific implementation of the present invention is described in detail below with reference to specific embodiments.

[0034] like Figure 1 As shown, a production device for fine chemicals provided by an embodiment of the present invention is provided. The raw materials involved are phenol and ethylene carbonate, including a raw material mixing tank 1, a reaction distillation tower 2, a lightness removal tower 3 and a heavy removal tower 4. The inlet materials of the raw material mixing tank 1 are phenol, ethylene carbonate and catalyst mixture 15. The material outlet of the raw material mixing tank 1 is connected to the inlet of the reaction distillation tower 2 through a reaction preheater 5, the tower bottom material outlet of the reaction distillation tower 2 is connected to the material inlet of the lightness removal tower 3, the tower bottom material outlet of the lightness removal tower 3 is connected to the material inlet of the heavy removal tower 4, and the tower bottom material outlet of the heavy removal tower 4 is a catalyst concentrate outlet 19.

[0035] In one embodiment, the raw material mixing tank 1 is equipped with a stirrer and has a heating half pipe or a jacket.

[0036] In one embodiment, the reaction distillation tower 2 is equipped with a reaction condenser 6, a reaction reflux buffer tank 9 and a reaction reboiler 12. The top of the reaction distillation tower 2 is connected to the inlet of the reaction reflux buffer tank 9 through the reaction condenser 6, and the outlet material of the reaction reflux buffer tank 9 is refluxed to the top of the reaction distillation tower 2. The reaction condenser 6 also has a CO2 outlet 16; the bottom material outlet of the reaction distillation tower 2 is connected to the reaction reboiler 12, and the outlet material of the reaction reboiler 12 is refluxed to the bottom of the reaction distillation tower 2.

[0037] Preferably, the reaction distillation tower 2 is a packed tower or a plate tower with 20 to 40 theoretical plates; the reaction condenser 6 is equipped with a non-condensable gas material outlet; and the reaction reflux buffer tank 9 is equipped with an internal heating coil.

[0038] In one embodiment, the de-lightening tower 3 is equipped with a de-lightening condenser 7, a de-lightening reflux buffer tank 10 and a de-lightening reboiler 13. The top of the de-lightening tower 3 is connected to the inlet of the de-lightening reflux buffer tank 10 through the de-lightening condenser 7, and the outlet material of the de-lightening reflux buffer tank 10 is refluxed to the top of the de-lightening tower 3. The outlet of the de-lightening reflux buffer tank 10 also includes a phenol outlet 17, which is used for the discharge of phenol; the bottom material outlet of the de-lightening tower 3 is connected to the de-lightening reboiler 13, and the outlet material of the de-lightening reboiler 13 is refluxed to the bottom of the de-lightening tower 3.

[0039] Preferably, the light-removing column 3 is a packed column or a plate column, and the number of theoretical plates is 30-60; the light-removing reflux buffer tank 10 is provided with an internal heating coil.

[0040] In one embodiment, the heavy-removing column 4 is provided with a heavy-removing condenser 8, a heavy-removing reflux buffer tank 11 and a heavy-removing reboiler 14, the top of the heavy-removing column 4 is connected with the inlet of the heavy-removing reflux buffer tank 11 through the heavy-removing condenser 8, the outlet material of the heavy-removing reflux buffer tank 11 is refluxed to the top of the heavy-removing column 4, and the outlet of the heavy-removing reflux buffer tank 11 further comprises a phenoxyethanol outlet 18, i.e. a discharge for phenoxyethanol; the outlet material of the heavy-removing reboiler 14 is connected with the bottom of the heavy-removing column 4, and the outlet material of the heavy-removing reboiler 14 is refluxed to the bottom of the heavy-removing column 4.

[0041] Preferably, the heavy-removing column 4 is a packed column or a plate column, and the number of theoretical plates is 30-60; the heavy-removing reflux buffer tank 11 is provided with an internal heating coil.

[0042] As shown in FIG. 1, one embodiment of the present application further provides a production process of fine chemicals, which is suitable for synthesizing phenoxyethanol from phenol and ethylene carbonate as raw materials, and comprises the following steps: Figure 1

[0043] Step 1, pretreatment of raw materials

[0044] Phenol, ethylene carbonate and catalyst from the boundary area are heated and dissolved in the raw material mixing tank 1 at a mass ratio of 1.1-2.0:1:0.005-0.08; the dissolved material is delivered to the reaction preheater 5 for reaction pretreatment;

[0045] Step 2, synthesis of phenoxyethanol

[0046] The pretreated mixture of phenol, ethylene carbonate and catalyst is subjected to full reflux synthesis reaction of phenoxyethanol in the reaction rectifying column 2, and the main reaction of the synthesis is as shown below:

[0047]

[0048] The carbon dioxide gas generated in the reaction is condensed by the reaction condenser 6 and then delivered to a subsequent section from the CO2 outlet 16 for recovery treatment; the reaction mixture discharged from the bottom of the reaction rectifying column 2 is delivered to the light-removing column 3 for rectification treatment; the conversion rate of ethylene carbonate after the reaction is 100%, and the selectivity of phenoxyethanol is 95%-99.5%;

[0049] Step 3, purification of phenoxyethanol

[0050] ​The reaction material from the reactor of the reactive distillation tower 2 is subjected to secondary distillation treatment in the light removal tower 3 and the heavy removal tower 4 to obtain a cosmetic-grade phenoxyethanol product, wherein the obtained phenoxyethanol content is ≥99.5% and the phenol content is <10 mg / kg.

[0051] In one embodiment, in step 1, the temperature of the material after heating and dissolving in the raw material mixing tank 1 is 50-80° C.; the temperature of the material after treatment in the reaction preheater 5 is 80-110° C.; the catalyst is a type of ionic liquid, and its structural formula is as follows:

[0052]

[0053] In the formula, R1 is methyl, ethyl or propyl; R2 is butyl, pentyl, hexyl, heptyl or octyl.

[0054] In one embodiment, in step 2, the top pressure of the reaction distillation tower 2 is 15 to 100 kPa; the temperature of the material after condensation in the reaction condenser 6 is 30 to 50°C; the bottom temperature of the reaction distillation tower 2 is 130 to 190°C; the reaction reflux buffer tank 9 is equipped with an internal heating coil, and when the temperature of the material is lower than 20°C, heating is turned on and the heating is stopped until the temperature rises to 50°C.

[0055] In one embodiment, in step 3, the reflux ratio of the top of the light removal tower 3 is 0.5 to 3.0, and the phenol obtained at the top of the light removal tower 3 can be recycled; the top pressure of the light removal tower 3 is 1 to 15 kPa; the temperature of the material after condensation in the light removal condenser 7 is 50 to 70°C; the bottom temperature of the light removal tower 3 is 100 to 140°C; the light removal reflux buffer tank 10 is equipped with an internal heating coil, and when the temperature of the material is lower than 50°C, heating is turned on until the temperature rises to 60°C and heating is stopped.

[0056] The reflux ratio at the top of the deweighting tower 4 is 0.5-3.0, and the phenoxyethanol obtained at the top of the deweighting tower 4 is cosmetic-grade; the catalyst concentrate obtained in the bottom of the deweighting tower 4 is transported to the subsequent process section for recovery and treatment; the top pressure of the deweighting tower 4 is 1-15 kPa; the temperature of the material after condensation in the deweighting condenser 8 is 30-50°C; the temperature of the bottom of the deweighting tower 4 is 110-160°C; the deweighting reflux buffer tank 11 is equipped with an internal heating coil, and when the temperature of the material is lower than 20°C, heating is turned on and heating is stopped until the temperature rises to 30°C.

[0057] Example 1

[0058] like Figure 1As shown, a production device for fine chemicals provided by an embodiment of the present invention is provided. The raw materials involved are phenol and ethylene carbonate, including a raw material mixing tank 1, a reaction distillation tower 2, a lightness removal tower 3 and a heavy removal tower 4. The inlet materials of the raw material mixing tank 1 are phenol, ethylene carbonate and catalyst mixture 15. The material outlet of the raw material mixing tank 1 is connected to the inlet of the reaction distillation tower 2 through a reaction preheater 5, the tower bottom material outlet of the reaction distillation tower 2 is connected to the material inlet of the lightness removal tower 3, the tower bottom material outlet of the lightness removal tower 3 is connected to the material inlet of the heavy removal tower 4, and the tower bottom material outlet of the heavy removal tower 4 is a catalyst concentrate outlet 19.

[0059] In one embodiment, the raw material mixing tank 1 is equipped with a stirrer and has a heating half pipe or a jacket.

[0060] In one embodiment, the reaction distillation tower 2 is equipped with a reaction condenser 6, a reaction reflux buffer tank 9 and a reaction reboiler 12. The top of the reaction distillation tower 2 is connected to the inlet of the reaction reflux buffer tank 9 through the reaction condenser 6, and the outlet material of the reaction reflux buffer tank 9 is refluxed to the top of the reaction distillation tower 2. The reaction condenser 6 also has a CO2 outlet 16; the bottom material outlet of the reaction distillation tower 2 is connected to the reaction reboiler 12, and the outlet material of the reaction reboiler 12 is refluxed to the bottom of the reaction distillation tower 2.

[0061] Preferably, the reaction distillation tower 2 is a packed tower or a plate tower with 20 theoretical plates; the reaction condenser 6 is equipped with a non-condensable gas material outlet; and the reaction reflux buffer tank 9 is equipped with an internal heating coil.

[0062] In one embodiment, the de-lightening tower 3 is equipped with a de-lightening condenser 7, a de-lightening reflux buffer tank 10 and a de-lightening reboiler 13. The top of the de-lightening tower 3 is connected to the inlet of the de-lightening reflux buffer tank 10 through the de-lightening condenser 7, and the outlet material of the de-lightening reflux buffer tank 10 is refluxed to the top of the de-lightening tower 3. The outlet of the de-lightening reflux buffer tank 10 also includes a phenol outlet 17, which is used for the discharge of phenol; the bottom material outlet of the de-lightening tower 3 is connected to the de-lightening reboiler 13, and the outlet material of the de-lightening reboiler 13 is refluxed to the bottom of the de-lightening tower 3.

[0063] Preferably, the light removal tower 3 is a packed tower or a plate tower with 30 theoretical plates; the light removal reflux buffer tank 10 is equipped with an internal heating coil.

[0064] In one embodiment, the de-heavy tower 4 is provided with a de-heavy condenser 8, a de-heavy reflux buffer tank 11 and a de-heavy reboiler 14, the top of the de-heavy tower 4 is connected with the de-heavy condenser 8 and the inlet of the de-heavy reflux buffer tank 11, the outlet material of the de-heavy reflux buffer tank 11 is refluxed to the top of the de-heavy tower 4, the outlet of the de-heavy reflux buffer tank 11 further comprises a phenoxy ethanol outlet 18, i.e. a discharge for phenoxy ethanol; the outlet material of the de-heavy reboiler 14 is refluxed to the bottom of the de-heavy tower 4.

[0065] Preferably, the de-heavy tower 4 is a packed tower or a plate tower, and the number of theoretical plates is 30; the de-heavy reflux buffer tank 11 is provided with an internal heating coil.

[0066] As shown in FIG. 1, one embodiment of the present application further provides a production process of fine chemicals, which is suitable for synthesizing phenoxy ethanol from phenol and ethylene carbonate as raw materials, and comprises the following steps: Figure 1

[0067] Step 1, pretreatment of raw materials

[0068] Phenol, ethylene carbonate and catalyst from the boundary region are heated and dissolved in the raw material mixing tank 1 at a mass ratio of 1.1:1:0.005; the dissolved material is delivered to the reaction preheater 5 for reaction pretreatment;

[0069] Step 2, synthesis of phenoxy ethanol

[0070] The pretreated mixture of phenol, ethylene carbonate and catalyst is subjected to a total reflux synthesis reaction of phenoxy ethanol in the reaction distillation column 2, and the main reaction of the synthesis is as shown below:

[0071]

[0072] The carbon dioxide gas generated in the reaction is condensed by the reaction condenser 6 and then delivered to the subsequent section through the CO2 outlet 16 for recovery treatment; the reaction mixture discharged from the bottom of the reaction distillation column 2 is delivered to the de-light tower 3 for distillation treatment; the conversion rate of the reacted ethylene carbonate is 100%, and the selectivity of phenoxy ethanol is 96.5%;

[0073] Step 3, purification of phenoxy ethanol

[0074] The reaction material from the bottom of the reaction distillation column 2 is subjected to two-stage distillation treatment by the de-light tower 3 and the de-heavy tower 4, and the cosmetic-grade phenoxy ethanol product can be obtained, the content of the obtained phenoxy ethanol is 99.65%, and the content of phenol is 4.5 mg / kg.

[0075] ​In one embodiment, in step 1, the temperature of the material after heating and dissolving in the raw material mixing tank 1 is 50° C.; the temperature of the material after treatment in the reaction preheater 5 is 80° C.; the catalyst is a type of ionic liquid, and its structural formula is as follows:

[0076]

[0077] In the formula, R1 is a methyl group; R2 is a butyl group.

[0078] In one embodiment, in step 2, the top pressure of the reaction distillation tower 2 is 15 kPa; the temperature of the material after condensation in the reaction condenser 6 is 30°C; the bottom temperature of the reaction distillation tower 2 is 130°C; the reaction reflux buffer tank 9 is equipped with an internal heating coil, and when the temperature of the material is lower than 20°C, heating is turned on and the heating is stopped until the temperature rises to 50°C.

[0079] In one embodiment, in step 3, the reflux ratio of the top of the light removal tower 3 is 0.5, and the phenol obtained at the top of the light removal tower 3 can be recycled; the top pressure of the light removal tower 3 is 1 kPa; the temperature of the material after condensation in the light removal condenser 7 is 50°C; the bottom temperature of the light removal tower 3 is 100°C; the light removal reflux buffer tank 10 is equipped with an internal heating coil, and when the temperature of the material is lower than 50°C, heating is turned on until the temperature rises to 60°C and heating is stopped.

[0080] The reflux ratio at the top of the deweighting tower 4 is 0.5, and the product obtained at the top of the deweighting tower 4 is cosmetic-grade phenoxyethanol; the catalyst concentrate obtained in the bottom of the deweighting tower 4 is transported to the subsequent process section for recovery and treatment; the top pressure of the deweighting tower 4 is 1 kPa; the temperature of the material after condensation in the deweighting condenser 8 is 30°C; the temperature of the bottom of the deweighting tower 4 is 110°C; the deweighting reflux buffer tank 11 is equipped with an internal heating coil, and when the temperature of the material is lower than 20°C, heating is turned on and heating is stopped until the temperature rises to 30°C.

[0081] Example 2

[0082] like Figure 1 As shown, a production device for fine chemicals provided by an embodiment of the present invention is provided. The raw materials involved are phenol and ethylene carbonate, including a raw material mixing tank 1, a reaction distillation tower 2, a lightness removal tower 3 and a heavy removal tower 4. The inlet materials of the raw material mixing tank 1 are phenol, ethylene carbonate and catalyst mixture 15. The material outlet of the raw material mixing tank 1 is connected to the inlet of the reaction distillation tower 2 through a reaction preheater 5, the tower bottom material outlet of the reaction distillation tower 2 is connected to the material inlet of the lightness removal tower 3, the tower bottom material outlet of the lightness removal tower 3 is connected to the material inlet of the heavy removal tower 4, and the tower bottom material outlet of the heavy removal tower 4 is a catalyst concentrate outlet 19.

[0083] In one embodiment, the raw material mixing tank 1 is equipped with a stirrer and has a heating half pipe or a jacket.

[0084] In one embodiment, the reaction distillation tower 2 is equipped with a reaction condenser 6, a reaction reflux buffer tank 9 and a reaction reboiler 12. The top of the reaction distillation tower 2 is connected to the inlet of the reaction reflux buffer tank 9 through the reaction condenser 6, and the outlet material of the reaction reflux buffer tank 9 is refluxed to the top of the reaction distillation tower 2. The reaction condenser 6 also has a CO2 outlet 16; the bottom material outlet of the reaction distillation tower 2 is connected to the reaction reboiler 12, and the outlet material of the reaction reboiler 12 is refluxed to the bottom of the reaction distillation tower 2.

[0085] Preferably, the reaction distillation tower 2 is a packed tower or a plate tower with 30 theoretical plates; the reaction condenser 6 is equipped with a non-condensable gas material outlet; and the reaction reflux buffer tank 9 is equipped with an internal heating coil.

[0086] In one embodiment, the de-lightening tower 3 is equipped with a de-lightening condenser 7, a de-lightening reflux buffer tank 10 and a de-lightening reboiler 13. The top of the de-lightening tower 3 is connected to the inlet of the de-lightening reflux buffer tank 10 through the de-lightening condenser 7, and the outlet material of the de-lightening reflux buffer tank 10 is refluxed to the top of the de-lightening tower 3. The outlet of the de-lightening reflux buffer tank 10 also includes a phenol outlet 17, which is used for the discharge of phenol; the bottom material outlet of the de-lightening tower 3 is connected to the de-lightening reboiler 13, and the outlet material of the de-lightening reboiler 13 is refluxed to the bottom of the de-lightening tower 3.

[0087] Preferably, the light removal tower 3 is a packed tower or a plate tower with 50 theoretical plates; the light removal reflux buffer tank 10 is equipped with an internal heating coil.

[0088] In one embodiment, the deweighting tower 4 is equipped with a deweighting condenser 8, a deweighting reflux buffer tank 11 and a deweighting reboiler 14. The top of the deweighting tower 4 is connected to the inlet of the deweighting reflux buffer tank 11 through the deweighting condenser 8. The outlet material of the deweighting reflux buffer tank 11 is refluxed to the top of the deweighting tower 4. The outlet of the deweighting reflux buffer tank 11 also includes a phenoxyethanol outlet 18, which is used for the discharge of phenoxyethanol; the bottom material outlet of the deweighting tower 4 is connected to the deweighting reboiler 14, and the outlet material of the deweighting reboiler 14 is refluxed to the bottom of the deweighting tower 4.

[0089] Preferably, the deweighting tower 4 is a packed tower or a plate tower with 50 theoretical plates; the deweighting reflux buffer tank 11 is equipped with an internal heating coil.

[0090] like Figure 1 As shown, one embodiment of the present invention further provides a production process for fine chemicals, which is suitable for synthesizing phenol ethanol using phenol and ethylene carbonate as raw materials, comprising the following steps:

[0091] Step 1: Pretreatment of raw materials

[0092] Phenol, ethylene carbonate and catalyst from the boundary zone are heated and dissolved in a raw material mixing tank 1 at a mass ratio of 1.5:1:0.02; the dissolved materials are transported to a reaction preheater 5 for reaction pretreatment;

[0093] Step 2, synthesis of phenoxyethanol

[0094] The pretreated mixture of phenol, ethylene carbonate and catalyst is subjected to a total reflux synthesis reaction of phenoxyethanol in a reactive distillation tower 2. The main reaction of the synthesis is as follows:

[0095]

[0096] The carbon dioxide gas generated by the reaction is condensed in the reaction condenser 6 and transported from the CO2 outlet 16 to the subsequent process for recovery and treatment. The reactant mixture discharged from the bottom of the reaction distillation tower 2 is transported to the lightness removal tower 3 for distillation treatment. The conversion rate of ethylene carbonate after the reaction is 100%, and the selectivity of phenoxyethanol is 99.5%.

[0097] Step 3: Purification of phenoxyethanol

[0098] The reaction material from the reactor of the reactive distillation tower 2 is subjected to secondary distillation treatment in the light removal tower 3 and the heavy removal tower 4 to obtain a cosmetic-grade phenoxyethanol product with a phenoxyethanol content of 99.62% and a phenol content of 2.3 mg / kg.

[0099] In one embodiment, in step 1, the temperature of the material after heating and dissolving in the raw material mixing tank 1 is 70° C.; the temperature of the material after treatment in the reaction preheater 5 is 100° C.; the catalyst is a type of ionic liquid, and its structural formula is as follows:

[0100]

[0101] In the formula, R1 is a methyl group; R2 is a pentyl group.

[0102] In one embodiment, in step 2, the top pressure of the reaction distillation tower 2 is 50 kPa; the temperature of the material after condensation in the reaction condenser 6 is 40°C; the bottom temperature of the reaction distillation tower 2 is 160°C; the reaction reflux buffer tank 9 is equipped with an internal heating coil, and when the temperature of the material is lower than 20°C, heating is turned on and the heating is stopped until the temperature rises to 50°C.

[0103] In one embodiment, in step 3, the reflux ratio of the top of the light removal tower 3 is 1.5, and the phenol obtained at the top of the light removal tower 3 can be recycled; the top pressure of the light removal tower 3 is 8 kPa; the temperature of the material after condensation in the light removal condenser 7 is 60°C; the bottom temperature of the light removal tower 3 is 120°C; the light removal reflux buffer tank 10 is equipped with an internal heating coil, and when the temperature of the material is lower than 50°C, heating is turned on until the temperature rises to 60°C and heating is stopped.

[0104] The reflux ratio at the top of the deweighting tower 4 is 2.0, and the product obtained at the top of the deweighting tower 4 is cosmetic-grade phenoxyethanol; the catalyst concentrate obtained in the bottom of the deweighting tower 4 is transported to the subsequent process section for recovery and treatment; the top pressure of the deweighting tower 4 is 8 kPa; the temperature of the material after condensation in the deweighting condenser 8 is 40°C; the temperature of the bottom of the deweighting tower 4 is 140°C; the deweighting reflux buffer tank 11 is equipped with an internal heating coil, and when the temperature of the material is lower than 20°C, heating is turned on and heating is stopped until the temperature rises to 30°C.

[0105] Example 3

[0106] like Figure 1 As shown, a production device for fine chemicals provided by an embodiment of the present invention is provided. The raw materials involved are phenol and ethylene carbonate, including a raw material mixing tank 1, a reaction distillation tower 2, a lightness removal tower 3 and a heavy removal tower 4. The inlet materials of the raw material mixing tank 1 are phenol, ethylene carbonate and catalyst mixture 15. The material outlet of the raw material mixing tank 1 is connected to the inlet of the reaction distillation tower 2 through a reaction preheater 5, the tower bottom material outlet of the reaction distillation tower 2 is connected to the material inlet of the lightness removal tower 3, the tower bottom material outlet of the lightness removal tower 3 is connected to the material inlet of the heavy removal tower 4, and the tower bottom material outlet of the heavy removal tower 4 is a catalyst concentrate outlet 19.

[0107] In one embodiment, the raw material mixing tank 1 is equipped with a stirrer and has a heating half pipe or a jacket.

[0108] In one embodiment, the reaction distillation tower 2 is equipped with a reaction condenser 6, a reaction reflux buffer tank 9 and a reaction reboiler 12. The top of the reaction distillation tower 2 is connected to the inlet of the reaction reflux buffer tank 9 through the reaction condenser 6, and the outlet material of the reaction reflux buffer tank 9 is refluxed to the top of the reaction distillation tower 2. The reaction condenser 6 also has a CO2 outlet 16; the bottom material outlet of the reaction distillation tower 2 is connected to the reaction reboiler 12, and the outlet material of the reaction reboiler 12 is refluxed to the bottom of the reaction distillation tower 2.

[0109] Preferably, the reaction distillation tower 2 is a packed tower or a plate tower with 40 theoretical plates; the reaction condenser 6 is equipped with a non-condensable gas material outlet; and the reaction reflux buffer tank 9 is equipped with an internal heating coil.

[0110] In one embodiment, the de-lightening tower 3 is equipped with a de-lightening condenser 7, a de-lightening reflux buffer tank 10 and a de-lightening reboiler 13. The top of the de-lightening tower 3 is connected to the inlet of the de-lightening reflux buffer tank 10 through the de-lightening condenser 7, and the outlet material of the de-lightening reflux buffer tank 10 is refluxed to the top of the de-lightening tower 3. The outlet of the de-lightening reflux buffer tank 10 also includes a phenol outlet 17, which is used for the discharge of phenol; the bottom material outlet of the de-lightening tower 3 is connected to the de-lightening reboiler 13, and the outlet material of the de-lightening reboiler 13 is refluxed to the bottom of the de-lightening tower 3.

[0111] Preferably, the light removal tower 3 is a packed tower or a plate tower with 60 theoretical plates; the light removal reflux buffer tank 10 is equipped with an internal heating coil.

[0112] In one embodiment, the deweighting tower 4 is equipped with a deweighting condenser 8, a deweighting reflux buffer tank 11 and a deweighting reboiler 14. The top of the deweighting tower 4 is connected to the inlet of the deweighting reflux buffer tank 11 through the deweighting condenser 8. The outlet material of the deweighting reflux buffer tank 11 is refluxed to the top of the deweighting tower 4. The outlet of the deweighting reflux buffer tank 11 also includes a phenoxyethanol outlet 18, which is used for the discharge of phenoxyethanol; the bottom material outlet of the deweighting tower 4 is connected to the deweighting reboiler 14, and the outlet material of the deweighting reboiler 14 is refluxed to the bottom of the deweighting tower 4.

[0113] Preferably, the deweighting tower 4 is a packed tower or a plate tower with 60 theoretical plates; the deweighting reflux buffer tank 11 is equipped with an internal heating coil.

[0114] like Figure 1 As shown, one embodiment of the present invention further provides a production process for fine chemicals, which is suitable for synthesizing phenol ethanol using phenol and ethylene carbonate as raw materials, comprising the following steps:

[0115] Step 1: Pretreatment of raw materials

[0116] Phenol, ethylene carbonate and catalyst from the boundary zone are heated and dissolved in a raw material mixing tank 1 at a mass ratio of 2:1:0.08; the dissolved materials are transported to a reaction preheater 5 for reaction pretreatment;

[0117] Step 2, synthesis of phenoxyethanol

[0118] The pretreated mixture of phenol, ethylene carbonate and catalyst is subjected to a total reflux synthesis reaction of phenoxyethanol in a reactive distillation tower 2. The main reaction of the synthesis is as follows:

[0119]

[0120] The carbon dioxide gas generated by the reaction is condensed in the reaction condenser 6 and transported from the CO2 outlet 16 to the subsequent process for recovery and treatment. The reactant mixture discharged from the bottom of the reaction distillation tower 2 is transported to the lightness removal tower 3 for distillation treatment. The conversion rate of ethylene carbonate after the reaction is 100%, and the selectivity of phenoxyethanol is 97.4%.

[0121] Step 3: Purification of phenoxyethanol

[0122] The reaction material from the reactor of the reactive distillation tower 2 is subjected to secondary distillation treatment in the light removal tower 3 and the heavy removal tower 4 to obtain a cosmetic-grade phenoxyethanol product with a phenoxyethanol content of 99.96% and a phenol content of 1.6 mg / kg.

[0123] In one embodiment, in step 1, the temperature of the material after heating and dissolving in the raw material mixing tank 1 is 80° C.; the temperature of the material after treatment in the reaction preheater 5 is 110° C.; the catalyst is a type of ionic liquid, and its structural formula is as follows:

[0124]

[0125] In the formula, R1 is a methyl group; R2 is a hexyl group.

[0126] In one embodiment, in step 2, the top pressure of the reaction distillation tower 2 is 100 kPa; the temperature of the material after condensation in the reaction condenser 6 is 50°C; the bottom temperature of the reaction distillation tower 2 is 190°C; the reaction reflux buffer tank 9 is equipped with an internal heating coil, and when the temperature of the material is lower than 20°C, heating is turned on and the heating is stopped until the temperature rises to 50°C.

[0127] In one embodiment, in step 3, the reflux ratio of the top of the light removal tower 3 is 3.0, and the phenol obtained at the top of the light removal tower 3 can be recycled; the top pressure of the light removal tower 3 is 15 kPa; the temperature of the material after condensation in the light removal condenser 7 is 70°C; the bottom temperature of the light removal tower 3 is 140°C; the light removal reflux buffer tank 10 is equipped with an internal heating coil, and when the temperature of the material is lower than 50°C, heating is turned on until the temperature rises to 60°C and heating is stopped.

[0128] The reflux ratio at the top of the deweighting tower 4 is 3.0, and the product obtained at the top of the deweighting tower 4 is cosmetic-grade phenoxyethanol; the catalyst concentrate obtained in the bottom of the deweighting tower 4 is transported to the subsequent process section for recovery and treatment; the top pressure of the deweighting tower 4 is 15 kPa; the temperature of the material after condensation in the deweighting condenser 8 is 50°C; the temperature of the bottom of the deweighting tower 4 is 160°C; the deweighting reflux buffer tank 11 is equipped with an internal heating coil, and when the temperature of the material is lower than 20°C, heating is turned on and heating is stopped until the temperature rises to 30°C.

[0129] Example 4

[0130] like Figure 1 As shown, a production device for fine chemicals provided by an embodiment of the present invention is provided. The raw materials involved are phenol and ethylene carbonate, including a raw material mixing tank 1, a reaction distillation tower 2, a lightness removal tower 3 and a heavy removal tower 4. The inlet materials of the raw material mixing tank 1 are phenol, ethylene carbonate and catalyst mixture 15. The material outlet of the raw material mixing tank 1 is connected to the inlet of the reaction distillation tower 2 through a reaction preheater 5, the tower bottom material outlet of the reaction distillation tower 2 is connected to the material inlet of the lightness removal tower 3, the tower bottom material outlet of the lightness removal tower 3 is connected to the material inlet of the heavy removal tower 4, and the tower bottom material outlet of the heavy removal tower 4 is a catalyst concentrate outlet 19.

[0131] In one embodiment, the raw material mixing tank 1 is equipped with a stirrer and has a heating half pipe or a jacket.

[0132] In one embodiment, the reaction distillation tower 2 is equipped with a reaction condenser 6, a reaction reflux buffer tank 9 and a reaction reboiler 12. The top of the reaction distillation tower 2 is connected to the inlet of the reaction reflux buffer tank 9 through the reaction condenser 6, and the outlet material of the reaction reflux buffer tank 9 is refluxed to the top of the reaction distillation tower 2. The reaction condenser 6 also has a CO2 outlet 16; the bottom material outlet of the reaction distillation tower 2 is connected to the reaction reboiler 12, and the outlet material of the reaction reboiler 12 is refluxed to the bottom of the reaction distillation tower 2.

[0133] Preferably, the reaction distillation tower 2 is a packed tower or a plate tower with 30 theoretical plates; the reaction condenser 6 is equipped with a non-condensable gas material outlet; and the reaction reflux buffer tank 9 is equipped with an internal heating coil.

[0134] In one embodiment, the de-lightening tower 3 is equipped with a de-lightening condenser 7, a de-lightening reflux buffer tank 10 and a de-lightening reboiler 13. The top of the de-lightening tower 3 is connected to the inlet of the de-lightening reflux buffer tank 10 through the de-lightening condenser 7, and the outlet material of the de-lightening reflux buffer tank 10 is refluxed to the top of the de-lightening tower 3. The outlet of the de-lightening reflux buffer tank 10 also includes a phenol outlet 17, which is used for the discharge of phenol; the bottom material outlet of the de-lightening tower 3 is connected to the de-lightening reboiler 13, and the outlet material of the de-lightening reboiler 13 is refluxed to the bottom of the de-lightening tower 3.

[0135] Preferably, the light removal tower 3 is a packed tower or a plate tower with 45 theoretical plates; the light removal reflux buffer tank 10 is equipped with an internal heating coil.

[0136] In one embodiment, the deweighting tower 4 is equipped with a deweighting condenser 8, a deweighting reflux buffer tank 11 and a deweighting reboiler 14. The top of the deweighting tower 4 is connected to the inlet of the deweighting reflux buffer tank 11 through the deweighting condenser 8. The outlet material of the deweighting reflux buffer tank 11 is refluxed to the top of the deweighting tower 4. The outlet of the deweighting reflux buffer tank 11 also includes a phenoxyethanol outlet 18, which is used for the discharge of phenoxyethanol; the bottom material outlet of the deweighting tower 4 is connected to the deweighting reboiler 14, and the outlet material of the deweighting reboiler 14 is refluxed to the bottom of the deweighting tower 4.

[0137] Preferably, the deweighting tower 4 is a packed tower or a plate tower with 45 theoretical plates; the deweighting reflux buffer tank 11 is equipped with an internal heating coil.

[0138] like Figure 1 As shown, one embodiment of the present invention further provides a production process for fine chemicals, which is suitable for synthesizing phenol ethanol using phenol and ethylene carbonate as raw materials, comprising the following steps:

[0139] Step 1: Pretreatment of raw materials

[0140] Phenol, ethylene carbonate and catalyst from the boundary zone are heated and dissolved in a raw material mixing tank 1 at a mass ratio of 1.6:1:0.03; the dissolved materials are transported to a reaction preheater 5 for reaction pretreatment;

[0141] Step 2, synthesis of phenoxyethanol

[0142] The pretreated mixture of phenol, ethylene carbonate and catalyst is subjected to a total reflux synthesis reaction of phenoxyethanol in a reactive distillation tower 2. The main reaction of the synthesis is as follows:

[0143]

[0144] The carbon dioxide gas generated by the reaction is condensed in the reaction condenser 6 and transported from the CO2 outlet 16 to the subsequent process for recovery and treatment. The reactant mixture discharged from the bottom of the reaction distillation tower 2 is transported to the lightness removal tower 3 for distillation treatment. The conversion rate of ethylene carbonate after the reaction is 100%, and the selectivity of phenoxyethanol is 99.1%.

[0145] Step 3: Purification of phenoxyethanol

[0146] The reaction material from the reactor of the reactive distillation tower 2 is subjected to secondary distillation treatment in the light removal tower 3 and the heavy removal tower 4 to obtain a cosmetic-grade phenoxyethanol product with a phenoxyethanol content of 99.84% and a phenol content of 1.1 mg / kg.

[0147] In one embodiment, in step 1, the temperature of the material after heating and dissolving in the raw material mixing tank 1 is 70° C.; the temperature of the material after treatment in the reaction preheater 5 is 100° C.; the catalyst is a type of ionic liquid, and its structural formula is as follows:

[0148]

[0149] In the formula, R1 is ethyl; R2 is hexyl.

[0150] In one embodiment, in step 2, the top pressure of the reaction distillation tower 2 is 60 kPa; the temperature of the material after condensation in the reaction condenser 6 is 40°C; the bottom temperature of the reaction distillation tower 2 is 160°C; the reaction reflux buffer tank 9 is equipped with an internal heating coil, and when the temperature of the material is lower than 20°C, heating is turned on and the heating is stopped until the temperature rises to 50°C.

[0151] In one embodiment, in step 3, the reflux ratio of the top of the light removal tower 3 is 2.0, and the phenol obtained at the top of the light removal tower 3 can be recycled; the top pressure of the light removal tower 3 is 9 kPa; the temperature of the material after condensation in the light removal condenser 7 is 60°C; the bottom temperature of the light removal tower 3 is 120°C; the light removal reflux buffer tank 10 is equipped with an internal heating coil, and when the temperature of the material is lower than 50°C, heating is turned on until the temperature rises to 60°C and heating is stopped.

[0152] The reflux ratio at the top of the deweighting tower 4 is 2.0, and the phenoxyethanol obtained at the top of the deweighting tower 4 is cosmetic-grade; the catalyst concentrate obtained in the bottom of the deweighting tower 4 is transported to the subsequent process section for recovery and treatment; the top pressure of the deweighting tower 4 is 9 kPa; the temperature of the material after condensation in the deweighting condenser 8 is 40°C; the temperature of the bottom of the deweighting tower 4 is 140°C; the deweighting reflux buffer tank 11 is equipped with an internal heating coil, and when the temperature of the material is lower than 20°C, heating is turned on and heating is stopped until the temperature rises to 30°C.

[0153] Example 5

[0154] like Figure 1 As shown, a production device for fine chemicals provided by an embodiment of the present invention is provided. The raw materials involved are phenol and ethylene carbonate, including a raw material mixing tank 1, a reaction distillation tower 2, a lightness removal tower 3 and a heavy removal tower 4. The inlet materials of the raw material mixing tank 1 are phenol, ethylene carbonate and catalyst mixture 15. The material outlet of the raw material mixing tank 1 is connected to the inlet of the reaction distillation tower 2 through a reaction preheater 5, the tower bottom material outlet of the reaction distillation tower 2 is connected to the material inlet of the lightness removal tower 3, the tower bottom material outlet of the lightness removal tower 3 is connected to the material inlet of the heavy removal tower 4, and the tower bottom material outlet of the heavy removal tower 4 is a catalyst concentrate outlet 19.

[0155] In one embodiment, the raw material mixing tank 1 is equipped with a stirrer and has a heating half pipe or a jacket.

[0156] In one embodiment, the reaction distillation tower 2 is equipped with a reaction condenser 6, a reaction reflux buffer tank 9 and a reaction reboiler 12. The top of the reaction distillation tower 2 is connected to the inlet of the reaction reflux buffer tank 9 through the reaction condenser 6, and the outlet material of the reaction reflux buffer tank 9 is refluxed to the top of the reaction distillation tower 2. The reaction condenser 6 also has a CO2 outlet 16; the bottom material outlet of the reaction distillation tower 2 is connected to the reaction reboiler 12, and the outlet material of the reaction reboiler 12 is refluxed to the bottom of the reaction distillation tower 2.

[0157] Preferably, the reaction distillation tower 2 is a packed tower or a plate tower with 30 theoretical plates; the reaction condenser 6 is equipped with a non-condensable gas material outlet; and the reaction reflux buffer tank 9 is equipped with an internal heating coil.

[0158] In one embodiment, the de-lightening tower 3 is equipped with a de-lightening condenser 7, a de-lightening reflux buffer tank 10 and a de-lightening reboiler 13. The top of the de-lightening tower 3 is connected to the inlet of the de-lightening reflux buffer tank 10 through the de-lightening condenser 7, and the outlet material of the de-lightening reflux buffer tank 10 is refluxed to the top of the de-lightening tower 3. The outlet of the de-lightening reflux buffer tank 10 also includes a phenol outlet 17, which is used for the discharge of phenol; the bottom material outlet of the de-lightening tower 3 is connected to the de-lightening reboiler 13, and the outlet material of the de-lightening reboiler 13 is refluxed to the bottom of the de-lightening tower 3.

[0159] Preferably, the light removal tower 3 is a packed tower or a plate tower with 50 theoretical plates; the light removal reflux buffer tank 10 is equipped with an internal heating coil.

[0160] In one embodiment, the deweighting tower 4 is equipped with a deweighting condenser 8, a deweighting reflux buffer tank 11 and a deweighting reboiler 14. The top of the deweighting tower 4 is connected to the inlet of the deweighting reflux buffer tank 11 through the deweighting condenser 8. The outlet material of the deweighting reflux buffer tank 11 is refluxed to the top of the deweighting tower 4. The outlet of the deweighting reflux buffer tank 11 also includes a phenoxyethanol outlet 18, which is used for the discharge of phenoxyethanol; the bottom material outlet of the deweighting tower 4 is connected to the deweighting reboiler 14, and the outlet material of the deweighting reboiler 14 is refluxed to the bottom of the deweighting tower 4.

[0161] Preferably, the deweighting tower 4 is a packed tower or a plate tower with 50 theoretical plates; the deweighting reflux buffer tank 11 is equipped with an internal heating coil.

[0162] like Figure 1 As shown, one embodiment of the present invention further provides a production process for fine chemicals, which is suitable for synthesizing phenol ethanol using phenol and ethylene carbonate as raw materials, comprising the following steps:

[0163] Step 1: Pretreatment of raw materials

[0164] Phenol, ethylene carbonate and catalyst from the boundary zone are heated and dissolved in a raw material mixing tank 1 at a mass ratio of 1.7:1:0.05; the dissolved materials are transported to a reaction preheater 5 for reaction pretreatment;

[0165] Step 2, synthesis of phenoxyethanol

[0166] The pretreated mixture of phenol, ethylene carbonate and catalyst is subjected to a total reflux synthesis reaction of phenoxyethanol in a reactive distillation tower 2. The main reaction of the synthesis is as follows:

[0167]

[0168] The carbon dioxide gas generated by the reaction is condensed in the reaction condenser 6 and transported from the CO2 outlet 16 to the subsequent process for recovery and treatment. The reactant mixture discharged from the bottom of the reaction distillation tower 2 is transported to the lightness removal tower 3 for distillation treatment. The conversion rate of ethylene carbonate after the reaction is 100%, and the selectivity of phenoxyethanol is 98.3%.

[0169] Step 3: Purification of phenoxyethanol

[0170] The reaction material from the reactor of the reactive distillation tower 2 is subjected to secondary distillation treatment in the light removal tower 3 and the heavy removal tower 4 to obtain a cosmetic-grade phenoxyethanol product with a phenoxyethanol content of 99.59% and a phenol content of 0.9 mg / kg.

[0171] In one embodiment, in step 1, the temperature of the material after heating and dissolving in the raw material mixing tank 1 is 70° C.; the temperature of the material after treatment in the reaction preheater 5 is 100° C.; the catalyst is a type of ionic liquid, and its structural formula is as follows:

[0172]

[0173] In the formula, R1 is ethyl; R2 is heptyl.

[0174] In one embodiment, in step 2, the top pressure of the reaction distillation tower 2 is 60 kPa; the temperature of the material after condensation in the reaction condenser 6 is 40°C; the bottom temperature of the reaction distillation tower 2 is 160°C; the reaction reflux buffer tank 9 is equipped with an internal heating coil, and when the temperature of the material is lower than 20°C, heating is turned on and the heating is stopped until the temperature rises to 50°C.

[0175] In one embodiment, in step 3, the reflux ratio of the top of the light removal tower 3 is 2.0, and the phenol obtained at the top of the light removal tower 3 can be recycled; the top pressure of the light removal tower 3 is 8 kPa; the temperature of the material after condensation in the light removal condenser 7 is 60°C; the bottom temperature of the light removal tower 3 is 120°C; the light removal reflux buffer tank 10 is equipped with an internal heating coil, and when the temperature of the material is lower than 50°C, heating is turned on until the temperature rises to 60°C and heating is stopped.

[0176] The reflux ratio at the top of the deweighting tower 4 is 2.0, and the product obtained at the top of the deweighting tower 4 is cosmetic-grade phenoxyethanol; the catalyst concentrate obtained in the bottom of the deweighting tower 4 is transported to the subsequent process section for recovery and treatment; the top pressure of the deweighting tower 4 is 8 kPa; the temperature of the material after condensation in the deweighting condenser 8 is 40°C; the temperature of the bottom of the deweighting tower 4 is 140°C; the deweighting reflux buffer tank 11 is equipped with an internal heating coil, and when the temperature of the material is lower than 20°C, heating is turned on and heating is stopped until the temperature rises to 30°C.

[0177] Example 6

[0178] like Figure 1 As shown, a production device for fine chemicals provided by an embodiment of the present invention is provided. The raw materials involved are phenol and ethylene carbonate, including a raw material mixing tank 1, a reaction distillation tower 2, a lightness removal tower 3 and a heavy removal tower 4. The inlet materials of the raw material mixing tank 1 are phenol, ethylene carbonate and catalyst mixture 15. The material outlet of the raw material mixing tank 1 is connected to the inlet of the reaction distillation tower 2 through a reaction preheater 5, the tower bottom material outlet of the reaction distillation tower 2 is connected to the material inlet of the lightness removal tower 3, the tower bottom material outlet of the lightness removal tower 3 is connected to the material inlet of the heavy removal tower 4, and the tower bottom material outlet of the heavy removal tower 4 is a catalyst concentrate outlet 19.

[0179] In one embodiment, the raw material mixing tank 1 is equipped with a stirrer and has a heating half pipe or a jacket.

[0180] In one embodiment, the reaction distillation tower 2 is equipped with a reaction condenser 6, a reaction reflux buffer tank 9 and a reaction reboiler 12. The top of the reaction distillation tower 2 is connected to the inlet of the reaction reflux buffer tank 9 through the reaction condenser 6, and the outlet material of the reaction reflux buffer tank 9 is refluxed to the top of the reaction distillation tower 2. The reaction condenser 6 also has a CO2 outlet 16; the bottom material outlet of the reaction distillation tower 2 is connected to the reaction reboiler 12, and the outlet material of the reaction reboiler 12 is refluxed to the bottom of the reaction distillation tower 2.

[0181] Preferably, the reaction distillation tower 2 is a packed tower or a plate tower with 30 theoretical plates; the reaction condenser 6 is equipped with a non-condensable gas material outlet; and the reaction reflux buffer tank 9 is equipped with an internal heating coil.

[0182] In one embodiment, the de-lightening tower 3 is equipped with a de-lightening condenser 7, a de-lightening reflux buffer tank 10 and a de-lightening reboiler 13. The top of the de-lightening tower 3 is connected to the inlet of the de-lightening reflux buffer tank 10 through the de-lightening condenser 7, and the outlet material of the de-lightening reflux buffer tank 10 is refluxed to the top of the de-lightening tower 3. The outlet of the de-lightening reflux buffer tank 10 also includes a phenol outlet 17, which is used for the discharge of phenol; the bottom material outlet of the de-lightening tower 3 is connected to the de-lightening reboiler 13, and the outlet material of the de-lightening reboiler 13 is refluxed to the bottom of the de-lightening tower 3.

[0183] Preferably, the light removal tower 3 is a packed tower or a plate tower with 50 theoretical plates; the light removal reflux buffer tank 10 is equipped with an internal heating coil.

[0184] In one embodiment, the deweighting tower 4 is equipped with a deweighting condenser 8, a deweighting reflux buffer tank 11 and a deweighting reboiler 14. The top of the deweighting tower 4 is connected to the inlet of the deweighting reflux buffer tank 11 through the deweighting condenser 8. The outlet material of the deweighting reflux buffer tank 11 is refluxed to the top of the deweighting tower 4. The outlet of the deweighting reflux buffer tank 11 also includes a phenoxyethanol outlet 18, which is used for the discharge of phenoxyethanol; the bottom material outlet of the deweighting tower 4 is connected to the deweighting reboiler 14, and the outlet material of the deweighting reboiler 14 is refluxed to the bottom of the deweighting tower 4.

[0185] Preferably, the deweighting tower 4 is a packed tower or a plate tower with 50 theoretical plates; the deweighting reflux buffer tank 11 is equipped with an internal heating coil.

[0186] like Figure 1 As shown, one embodiment of the present invention further provides a production process for fine chemicals, which is suitable for synthesizing phenol ethanol using phenol and ethylene carbonate as raw materials, comprising the following steps:

[0187] Step 1: Pretreatment of raw materials

[0188] Phenol, ethylene carbonate and catalyst from the boundary zone are heated and dissolved in a raw material mixing tank 1 at a mass ratio of 1.4:1:0.03; the dissolved materials are transported to a reaction preheater 5 for reaction pretreatment;

[0189] Step 2, synthesis of phenoxyethanol

[0190] The pretreated mixture of phenol, ethylene carbonate and catalyst is subjected to a total reflux synthesis reaction of phenoxyethanol in a reactive distillation tower 2. The main reaction of the synthesis is as follows:

[0191]

[0192] The carbon dioxide gas generated by the reaction is condensed in the reaction condenser 6 and transported from the CO2 outlet 16 to the subsequent process for recovery and treatment. The reactant mixture discharged from the bottom of the reaction distillation tower 2 is transported to the lightness removal tower 3 for distillation treatment. The conversion rate of ethylene carbonate after the reaction is 100%, and the selectivity of phenoxyethanol is 95.2%.

[0193] Step 3: Purification of phenoxyethanol

[0194] The reaction material from the reactor of the reactive distillation tower 2 is subjected to secondary distillation treatment in the light removal tower 3 and the heavy removal tower 4 to obtain a cosmetic-grade phenoxyethanol product with a phenoxyethanol content of 99.72% and a phenol content of 1.2 mg / kg.

[0195] In one embodiment, in step 1, the temperature of the material after heating and dissolving in the raw material mixing tank 1 is 60° C.; the temperature of the material after treatment in the reaction preheater 5 is 90° C.; the catalyst is a type of ionic liquid, and its structural formula is as follows:

[0196]

[0197] In the formula, R1 is propyl; R2 is octyl.

[0198] In one embodiment, in step 2, the top pressure of the reaction distillation tower 2 is 70 kPa; the temperature of the material after condensation in the reaction condenser 6 is 40°C; the bottom temperature of the reaction distillation tower 2 is 160°C; the reaction reflux buffer tank 9 is equipped with an internal heating coil, and when the temperature of the material is lower than 20°C, heating is turned on and the heating is stopped until the temperature rises to 50°C.

[0199] In one embodiment, in step 3, the reflux ratio of the top of the light removal tower 3 is 2.0, and the phenol obtained at the top of the light removal tower 3 can be recycled; the top pressure of the light removal tower 3 is 8 kPa; the temperature of the material after condensation in the light removal condenser 7 is 60°C; the bottom temperature of the light removal tower 3 is 120°C; the light removal reflux buffer tank 10 is equipped with an internal heating coil, and when the temperature of the material is lower than 50°C, heating is turned on until the temperature rises to 60°C and heating is stopped.

[0200] The reflux ratio at the top of the deweighting tower 4 is 2.0, and the product obtained at the top of the deweighting tower 4 is cosmetic-grade phenoxyethanol; the catalyst concentrate obtained in the bottom of the deweighting tower 4 is transported to the subsequent process section for recovery and treatment; the top pressure of the deweighting tower 4 is 8 kPa; the temperature of the material after condensation in the deweighting condenser 8 is 40°C; the temperature of the bottom of the deweighting tower 4 is 140°C; the deweighting reflux buffer tank 11 is equipped with an internal heating coil, and when the temperature of the material is lower than 20°C, heating is turned on and heating is stopped until the temperature rises to 30°C.

[0201] The above embodiments of the present invention provide a production device and process for fine chemicals, the main advantages of which are as follows:

[0202] 1) The process is simple and efficient, with a conversion rate of ethylene carbonate of 100% and a selectivity of phenoxyethanol greater than 95%;

[0203] 2) The provided ionic liquid catalyst is stable and can be recycled, which is conducive to industrial application;

[0204] 3) The device has a simple structure, is easy to operate, and has stable and reliable product quality, which can effectively reduce the device investment of phenoxyethanol and improve the market competitiveness of the product.

[0205] The technical features of the above-mentioned embodiments can be combined arbitrarily. In order to make the description concise, not all possible combinations of the technical features in the above-mentioned embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0206] The above-described embodiments merely illustrate several implementations of the present invention, and while their descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that a person skilled in the art would be able to make numerous variations and improvements without departing from the spirit of the present invention, all of which fall within the scope of protection of the present invention. Therefore, the scope of protection of the present invention shall be determined by the appended claims.

Claims

1. A production process for fine chemicals, comprising a reaction reflux buffer tank, a light removal condenser, a light removal reflux buffer tank, a heavy removal condenser and a heavy removal reflux buffer tank, characterized in that: The process includes the following steps: Step 1: Pretreatment of raw materials Phenol, ethylene carbonate and catalyst from the boundary zone are heated and dissolved in a raw material mixing tank at a mass ratio of 1.1-2.0:1:0.005-0.08; the dissolved materials are transported to a reaction preheater for reaction pretreatment; Step 2, synthesis of phenoxyethanol The mixture of pretreated phenol, ethylene carbonate and catalyst is subjected to a total reflux synthesis reaction of phenoxyethanol in a reactive distillation tower. The main reaction of the synthesis is as follows: The carbon dioxide gas produced by the reaction is condensed in a reaction condenser and transported from the CO2 outlet to subsequent processing stages for recovery and treatment. The reactant mixture discharged from the reactor of the reaction distillation tower is transported to a lightness removal tower for distillation treatment. The conversion rate of ethylene carbonate after the reaction is 100%, and the selectivity of phenoxyethanol is 95% to 99.5%. Step 3: Purification of phenoxyethanol The reaction material from the reactor of the reactive distillation tower is subjected to secondary distillation treatment in a light removal tower and a heavy removal tower to obtain a cosmetic-grade phenoxyethanol product with a phenoxyethanol content of ≥99.5% and a phenol content of <10 mg / kg. Among them, the cosmetic-grade phenoxyethanol obtained from the top of the deweighting tower is the catalyst concentrate obtained from the bottom of the deweighting tower, which is transported to the subsequent process section for recovery and treatment.

2. The production process of fine chemicals according to claim 1, characterized in that: In step 1, the temperature of the material after heating and dissolving in the raw material mixing tank is 50-80°C; The temperature of the material after being treated in the reaction preheater is 80-110°C; The catalyst is a type of ionic liquid, and its structural formula is shown below: In the formula, R1 is methyl, ethyl or propyl; R2 is butyl, pentyl, hexyl, heptyl or octyl.

3. The production process of fine chemicals according to claim 2, characterized in that: In step 2, the top pressure of the reactive distillation tower is 15-100 kPa; The temperature of the material after condensation in the reaction condenser is 30-50°C; The reactor temperature of the reactive distillation tower is 130-190°C; The reaction reflux buffer tank is equipped with an internal heating coil. When the temperature of the material is lower than 20°C, heating is turned on and the heating is stopped until the temperature rises to 50°C.

4. The production process of fine chemicals according to claim 3, characterized in that: In step 3, the reflux ratio of the light removal tower top is 0.5-3.0, the phenol obtained at the light removal tower top can be recycled, the top pressure of the light removal tower is 1-15 kPa, and the temperature of the light removal tower kettle is 100-140°C; The temperature of the material after condensation in the light removal condenser is 50-70°C; The de-light reflux buffer tank is equipped with an internal heating coil. When the temperature of the material is lower than 50°C, heating is turned on and the heating is stopped when the temperature rises to 60°C. The reflux ratio of the weight removal tower top is 0.5-3.0, the top pressure of the weight removal tower is 1-15 kPa, and the kettle temperature of the weight removal tower is 110-160°C; The temperature of the material after condensation in the de-weighting condenser is 30-50°C; The de-weighting reflux buffer tank is equipped with an internal heating coil. When the temperature of the material is lower than 20°C, heating is turned on and the heating is stopped when the temperature rises to 30°C.

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