Production device of dibutyl carbonate
By using continuous reaction and DCS control system, the problem of low efficiency in intermittent operation of dibutyl carbonate production unit has been solved, and high conversion rate and high quality dibutyl carbonate production has been achieved, which is suitable for large-scale production and the application of new catalysts.
Patent Information
- Application Number
- CN202520058197.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-10
- Publication Date
- 2025-12-16
- Estimated Expiration
- 2035-01-10
AI Technical Summary
Existing dibutyl carbonate production facilities are mainly operated intermittently, which is complicated and inefficient, making them unsuitable for large-scale production and difficult to achieve high product quality standards.
Using n-butanol and dimethyl carbonate as raw materials, dibutyl carbonate is produced through continuous reaction. An enhanced reactor and DCS control system are used, combined with packing layer design and automatic control of temperature and flow rate, to achieve material and heat balance, thereby improving conversion rate and product quality.
It enables continuous production of dibutyl carbonate with a conversion rate of up to 99.9%, making it suitable for large-scale production and the production of new catalysts, and simplifying the operation process.
Smart Images
Figure CN223668685U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model belongs to the fine chemical industry field relates to a kind of production device of carbonic acid dibutyl ester, it is suitable for n-butanol and carbonic acid dimethyl ester as raw material, the continuous automation reaction production device of ester exchange method preparation carbonic acid dibutyl ester. BACKGROUND
[0002] Carbonic acid di-n-butyl ester (DBC) is a colorless liquid, with large molecular weight (M=174.24), flash point and other characteristics, and strong oxidation resistance, as non-aqueous electrolyte can fully improve the electrochemical stability of lithium battery and the safety of battery. DBC as a kind of organic symmetrical dialkyl ester containing carbonyl and butyl, also can be used as carbonylation agent or alkylating agent for organic synthesis; DBC is also considered as a substitute for phosgene, used in polycarbonate synthesis field. DBC can also react with organic amine, etc., to prepare N-substituted organic carbamic acid ester, further thermal cracking of organic carbamic acid ester can realize non-phosgene route for preparing organic isocyanate, DBC as carbonyl source and alkylating agent has the characteristics of green and safety in the process. In addition, DBC can also be used as base material for lubricating oil, metal oil removal, leather treatment and other industries, and as a solvent for foaming polystyrene.
[0003] The current domestic carbonic acid dibutyl ester production capacity is not large, and the industrial device is mainly operated intermittently, which is complicated and low in efficiency, and is not conducive to the expansion of the device and the promotion of the product.
[0004] Another patent uses urea and n-butanol to generate n-butyl carbonate. This method has high reaction pressure, long reaction time and is operated intermittently, and the product quality can only reach 99%. SUMMARY
[0005] The utility model aims at providing a kind of production device of carbonic acid dibutyl ester, using n-butanol and carbonic acid dimethyl ester as raw material, continuous reaction generates carbonic acid dibutyl ester, and by-product methanol is generated;The device is controlled by DCS, and the reaction condition is mild, the conversion rate is high, and the product quality can reach more than 99.9%.
[0006] In order to achieve the above object, the technical scheme adopted by the utility model is: a dibutyl carbonate production device: containing a strengthened reactor, a reaction circulating pump, a circulating heater, a reaction feed pump, a reaction rectifying tower, a reaction reboiler, a reaction condenser; wherein the strengthened reactor bottom N1 discharge pipeline is connected with the reaction circulating pump inlet, the reaction circulating pump outlet is connected with the circulating heater inlet, the circulating heater outlet is connected with the strengthened reactor inlet, the strengthened reactor bottom N2 discharge pipeline is connected with the reaction feed pump feed inlet, the reaction feed pump outlet is respectively connected to the reaction rectifying tower feed inlet and the strengthened reactor top circulating port, the reaction rectifying tower top gas phase outlet is connected with the reaction condenser inlet pipeline, the reaction condenser outlet pipeline is respectively connected with the reaction rectifying tower top reflux port and the tower top discharge pipeline, the reaction rectifying tower bottom outlet is respectively connected with the reaction reboiler inlet and the tower kettle discharge pipeline, and the reaction reboiler outlet is connected with the reaction rectifying tower kettle gas phase inlet.
[0007] The raw material feed pipeline is connected on the pipeline of the reaction circulating pump and the circulating heater, enters the device after being heated by the circulating heater; the reaction circulating pump and the circulating thermometer are provided with interlocking, and the circulation amount is controlled by adjusting the frequency of the reaction circulating pump to achieve the purpose of controlling the temperature of the circulating thermometer.
[0008] The strengthened reactor is provided with a filler layer, the number of filler layers is greater than 2, the feed inlet is located at the middle position of the filler layer, and at least one layer of filler is arranged below the feed inlet; the material is partially vaporized after being heated by the circulating heater, the gas-liquid mixture is separated in the strengthened reactor, the liquid phase is distributed through the filler layer and then flows to the bottom of the reactor, and the vapor phase material rises to the top of the reactor and contacts the circulating liquid transported to the top of the reactor by the reaction feed pump through the filler layer and mass transfer and heat transfer, so that the reaction is strengthened, the conversion rate is improved, and the vapor phase material after mass transfer and heat transfer is collected from the top of the reactor and enters the reaction rectifying tower in the form of vapor phase; part of the liquid phase material is transported to the reaction rectifying tower by the reaction feed pump, and part of the liquid phase material is circulated back to the top of the reactor; the reaction feed pump and the feed flowmeter are provided with remote DCS automatic interlocking control, and the feed flowmeter flow is controlled by adjusting the frequency of the reaction feed pump.
[0009] The reaction kettle thermometer is arranged at the kettle of the reaction rectifying tower, the reaction tower middle thermometer is arranged at the feed inlet, the reaction tower top thermometer is arranged at the top of the reaction tower, and remote DCS display is arranged; the reaction reboiler steam adjusting valve group and the reaction tower reflux flowmeter are provided with remote DCS automatic interlocking control, the steam amount is adjusted by the opening degree of the steam adjusting valve group to control the flow of the reaction tower reflux flowmeter; the reaction tower top discharge valve group and the reaction tower top discharge flowmeter are provided with remote DCS automatic interlocking control, and the flow of the reaction tower top discharge flowmeter is controlled by the valve opening degree of the reaction tower top discharge valve group; the material balance and the heat balance of the reaction rectifying tower are adjusted through the three groups of flow control, and the temperatures of the reaction kettle thermometer, the reaction tower middle thermometer and the reaction tower top thermometer are controlled.
[0010] n-butanol, dimethyl carbonate and catalyst enter the circulating heater in a certain proportion, after preheating by the heater, the temperature of the circulating thermometer is controlled by adjusting the frequency of the reaction circulating pump to ensure that the material temperature reaches the reaction temperature, after the material enters the intensified reactor, the liquid phase material flows downward into the bottom of the reactor, and the vapor phase material rises after mass transfer and heat transfer with the circulating liquid and is produced; the reaction is carried out smoothly by circulating heating, and the residence time of the newly added material can be ensured by controlling the liquid level to ensure that the reaction proceeds as much as possible in the positive direction; the liquid phase material is transported to the reaction rectification tower by the reaction feed pump, and the feed amount is controlled by adjusting the frequency of the reaction feed pump; after the material enters the tower, the by-product methanol and dimethyl carbonate form an azeotrope, part of which is refluxed and part of which is produced, the dimethyl carbonate and n-butyl carbonate mixture at the tower bottom is separated into the subsequent process; by controlling the feed and discharge and the reflux ratio, the temperature points in the tower are controlled, the reaction tower bottom thermometer is 110-160 DEG C, the reaction tower middle thermometer is 68-85 DEG C and the reaction tower top thermometer is 62-66 DEG C, and the continuous operation of production is ensured.
[0011] The utility model has the following advantages:
[0012] (1) the reaction device is continuously operated, which is beneficial to production operation and device amplification in large-scale production;
[0013] (2) suitable for the production of new catalysts;
[0014] (3) the device adopts DCS automatic control, which simplifies the production operation. DRAWINGS
[0015] Figure 1 It is the device schematic drawing of the utility model. CONCRETE IMPLEMENTING METHOD
[0016] The utility model further describes in combination with the embodiment, the following embodiment is aimed at explaining the utility model, and is not the limitation of the utility model. The embodiment of the utility model of a kind of dibutyl carbonate production device, its steps are: containing enhanced reactor (R1), reaction circulating pump (P1), circulating heater (E1), reaction feed pump (P2), reaction rectifying column (T1), reaction reboiler (E2), reaction condenser (E3);Wherein enhanced reactor (R1) bottom N1 discharge pipeline is connected with the import of reaction circulating pump (P1), the export of reaction circulating pump (P1) is connected with the import of circulating heater (E1), the export of circulating heater (E1) is connected with the import of enhanced reactor (R1), enhanced reactor (R1) bottom N2 discharge pipeline is connected with the feed inlet of reaction feed pump (P2), the export of reaction feed pump (P2) is connected to reaction rectifying column (T1) feed inlet and enhanced reactor (R1) top circulation port respectively, reaction rectifying column (T1) top gas phase export is connected with the import pipeline of reaction condenser (E3), the export pipeline of reaction condenser (E3) is connected with reaction rectifying column (T1) top backflow port and column top discharge pipeline respectively, the export of reaction rectifying column (T1) bottom is connected with the import of reaction reboiler (E2) and column still discharge pipeline respectively, the export of reaction reboiler (E2) is connected with the column still gas phase import of reaction rectifying column (T1). The packing layer is arranged in the enhanced reactor (R1), and the material feed inlet is in the middle of the packing layer. The outlet of circulating heater (E1) and the import connecting pipe of enhanced reactor (R1) are provided with a circulating thermometer T1, and are provided with remote DCS automatic interlock control by reaction circulating pump (P1), and the temperature of circulating thermometer T1 is controlled by the frequency of reaction circulating pump (P1). Reaction feed pump (P2) and feed flowmeter F1 are provided with remote DCS automatic interlock control, and the flow of feed flowmeter F1 is controlled by the frequency of reaction feed pump (P2). Reaction rectifying column (T1) column still is provided with reaction column still thermometer T2, feed inlet is provided with reaction column thermometer T3, column top is provided with continuous reaction column top thermometer T4, and remote DCS display is set. Steam regulating valve group and reaction column backflow flowmeter F2 are provided with remote DCS automatic interlock control, and the flow of reaction column backflow flowmeter F2 is adjusted by the opening degree of steam regulating valve group to control the amount of steam. Reaction column top discharge valve group and reaction column top discharge flowmeter F3 are provided with remote DCS automatic interlock control, and the flow of reaction column top discharge flowmeter F3 is controlled by the valve opening degree of reaction column top discharge valve group.
[0017] When the process requires the feed to be increased from 2000 kg / h to 2500 kg / h, the reaction feed pump frequency is increased to increase the feed flow meter flow from 2000 kg / h to 2500 kg / h, and the feed of each raw material and catalyst is increased to ensure that the strong reactor liquid level meter liquid level remains unchanged. Due to the increase in raw material feed, the circulating temperature will decrease, the reaction circulating pump frequency is adjusted to increase the circulating amount to keep the circulating temperature unchanged; the reaction rectification column feed is increased, the inlet and outlet materials are unbalanced, which will cause the change of the temperature point in the tower, the reaction tower top discharge valve group valve opening is adjusted to increase the tower top discharge; the steam heating valve group opening is adjusted to increase the heating to ensure the reflux ratio; at the same time, the tower kettle discharge is increased to keep the tower temperature unchanged.
[0018] When the process requires the feed to be decreased from 2000 kg / h to 1500 kg / h, the reaction feed pump frequency is reduced to reduce the feed flow meter flow from 2000 kg / h to 1500 kg / h, and the feed of each raw material and catalyst is reduced to ensure that the strong reactor liquid level meter liquid level remains unchanged. Due to the decrease in raw material feed, the circulating temperature will increase, the reaction circulating pump frequency is reduced to reduce the circulating amount to keep the circulating temperature unchanged; the reaction rectification column feed is reduced, the inlet and outlet materials are unbalanced, which will cause the change of the temperature point in the tower, the reaction tower top discharge valve group valve opening is adjusted to reduce the tower top discharge; the steam heating valve group opening is adjusted to reduce the heating to ensure the reflux ratio; at the same time, the tower kettle discharge is reduced to keep the tower temperature unchanged.
[0019] The above embodiment is only one implementation form of the carbon dioxide butyl ester production device, and other deformations of the scheme provided by the present application, increase or decrease the components or steps therein, or apply the present application to the technical field similar to the present application, all belong to the protection scope of the present application.
Claims
1. A production apparatus for dibutyl carbonate, characterized in that: The reaction system comprises a reinforced reactor (R1), a reaction circulating pump (P1), a circulating heater (E1), a reaction feed pump (P2), a reaction rectifying tower (T1), a reaction reboiler (E2), and a reaction condenser (E3). The reinforced reactor (R1) is connected with the reaction circulating pump (P1) through a pipeline at the bottom N1, the outlet of the reaction circulating pump (P1) is connected with the inlet of the circulating heater (E1), the outlet of the circulating heater (E1) is connected with the inlet of the reinforced reactor (R1), the reinforced reactor (R1) is connected with the reaction feed pump (P2) through a pipeline at the bottom N2, the outlet of the reaction feed pump (P2) is connected with the inlet of the reaction rectifying tower (T1) and the top of the reinforced reactor (R1), the top gas phase outlet of the reaction rectifying tower (T1) is connected with the inlet pipeline of the reaction condenser (E3), the outlet pipeline of the reaction condenser (E3) is connected with the top reflux inlet of the reaction rectifying tower (T1) and the tower top outlet pipeline, the bottom outlet of the reaction rectifying tower (T1) is connected with the inlet of the reaction reboiler (E2) and the tower kettle outlet pipeline, and the outlet of the reaction reboiler (E2) is connected with the tower kettle gas phase inlet of the reaction rectifying tower (T1).
2. The dibutyl carbonate production apparatus according to claim 1, characterized by: The reinforced reactor (R1) is provided with a filler layer, and the material feed inlet is in the middle of the filler layer.
3. The apparatus for producing dibutyl carbonate according to claim 1, wherein: the distillation column is a packed column. The pipeline connecting the outlet of the circulating heater (E1) with the inlet of the reinforced reactor (R1) is provided with a circulating thermometer T1, and the reaction circulating pump (P1) is provided with a remote DCS automatic interlock control, and the circulating thermometer T1 temperature is controlled by the frequency of the reaction circulating pump (P1).
4. The apparatus for producing dibutyl carbonate according to claim 1, wherein: the distillation column is a packed column. The reaction feed pump (P2) is provided with a remote DCS automatic interlock control with the feed flowmeter F1, and the feed flowmeter (F1) flow is controlled by the frequency of the reaction feed pump (P2).
5. The apparatus for producing dibutyl carbonate according to claim 1, wherein: the distillation column is a packed column. The reaction rectifying tower (T1) is provided with a reaction tower kettle thermometer T2, a reaction tower middle thermometer T3, and a continuous reaction tower top thermometer T4, and a remote DCS display is arranged.
6. The apparatus for producing dibutyl carbonate according to claim 1, wherein: the distillation column is a packed column. The steam adjusting valve group and the reaction column reflux flowmeter F2 are provided with a remote DCS automatic interlock control, and the reaction column reflux flowmeter F2 flow is controlled by the opening degree of the steam adjusting valve group.
7. The apparatus for producing dibutyl carbonate according to claim 1, wherein: the distillation column is a packed column. The reaction tower top outlet valve group and the reaction tower top outlet flowmeter F3 are provided with a remote DCS automatic interlock control, and the reaction tower top outlet flowmeter F3 flow is controlled by the valve opening degree of the reaction tower top outlet valve group.