Preparation system of high-purity trioctyldecyl tertiary amine

Abstract

The utility model relates to the field of chemical production, and provides a preparation system for high-purity trioctyl decyl tertiary amine. Comprising a reaction kettle and a fractionating tower, a steam outlet is formed in the top of the fractionating tower and connected with a condenser through a pipeline, a non-condensable gas outlet of the condenser is connected with a circulating gas buffer tank through a pipeline, the circulating gas buffer tank is connected with a compressor, and an exhaust port of the compressor is connected with a gas inlet buffer tank; a bypass branch is mounted between an air suction port and an exhaust port of the compressor; non-condensable gas in the reaction process is compressed through a compressor to form gas with certain pressure, and the contact time and the contact range of ammonia gas, the raw materials and the catalyst are increased while the catalyst and the raw materials in the gas inlet buffer tank are fully stirred and mixed, so that the reaction process is accelerated; the pressure of the gas entering the reaction kettle is adjusted, so that the main reaction is promoted, the condensation of byproducts of primary amine, secondary amine and aldol is avoided, and the purity of a finished product is improved.

Description

Technical Field

[0001] The utility model relates to the field of chemical production, in particular to a high-purity trioctyldecyl tertiary amine preparation system. Background Art

[0002] Trioctyldecyl tertiary amine is generally used as an extractant for precious metals and is also an important raw material for organic synthesis. Trioctyldecyl tertiary amine is produced by the catalytic reaction of alcohol and ammonia in a hydrogen atmosphere. The reaction process is the process of ammonia moving from the bottom of the reactor to the upper gas-liquid contact surface of the reactor. Ammonia can react when it encounters alcohol liquid with catalyst. Ammonia plays a churning role in the reactor, which can replace the stirring of conventional reactors, so that the catalyst is fully dispersed in the liquid, which increases the overall reaction area of ​​gas, liquid and solid, and accelerates the reaction process.

[0003] The main reaction in the preparation of trioctyldecyl tertiary amine is to generate trioctyldecyl tertiary amine, and this reaction generates trioctyldecyl primary amine and trioctyldecyl secondary amine. Therefore, the intake speed of ammonia should be effectively controlled. Too short a time will lead to incomplete reaction and violent internal churning. Too long a reaction time will also increase the probability of aldol condensation of fatty alcohols and generate by-products. Therefore, it is necessary to control the residence time of the circulating ammonia in the reactor so that ammonia can participate in the reaction as much as possible, so that the primary amine and secondary amine continue to react with the alcohol to produce tertiary amine products, and promote the main reaction; Summary of the invention

[0004] In order to improve the reaction efficiency in the preparation process of trioctyldecyl tertiary amine, reduce the generation of by-products and improve the purity of the final product, the utility model aims to provide a high-purity trioctyldecyl tertiary amine preparation system.

[0005] The technical solution adopted by the utility model is:

[0006] A high-purity trioctyldecyl tertiary amine preparation system comprises a reactor and a fractionation tower, wherein a heat exchange coil is installed in the reactor, a material feed port, a catalyst inlet, a gas inlet, a gas outlet and a tower reflux port are arranged on the top of the reactor, the material inlet is connected to a raw material preparation reactor through a pipeline and a valve, the catalyst inlet is connected to a catalyst preparation reactor through a pipeline and a valve, the gas inlet is connected to an ammonia generating device, the gas outlet is connected to the fractionation tower through a pipeline and a valve, the bottom of the fractionation tower is connected to the tower reflux port through a pipeline and a valve, a steam outlet is arranged on the top of the fractionation tower, the steam outlet is connected to a condenser through a pipeline, a discharge port is arranged at the bottom of the reactor, and a condensate outlet of the condenser is connected to the condensate outlet of the condenser. The outlet of the condenser is connected to the oil-water separator through a pipeline, the non-condensable gas outlet of the condenser is connected to the circulating gas buffer tank through a pipeline, the circulating gas buffer tank is connected to the compressor, the circulating buffer tank is connected to the air intake of the compressor through a pipeline, the exhaust port of the compressor is connected to the air intake buffer tank through a pipeline and a control valve; a bypass branch is installed between the air intake and exhaust ports of the compressor, and a bypass regulating valve is installed on the bypass branch; the air intake buffer tank is connected to an ammonia generator and a hydrogen pipeline, the air intake buffer tank is connected to the gas inlet of the reactor through a pipeline and a valve, a gas distribution device is installed at the bottom of the reactor, and the gas distribution device is connected to the gas inlet through a pipeline.

[0007] Furthermore, the oil-water separator includes a shell, the upper part of the shell is an overflow chamber, the lower part of the shell is a separation chamber, a condensate inlet is provided on one side of the overflow chamber, the condensate inlet is connected to the condensate outlet of the condenser, an overflow port is provided at the top of the overflow chamber, and the overflow port is connected to the reflux port at the top of the distillation tower through a pipeline; a liquid outlet is provided at the bottom of the separation chamber, and the liquid outlet is connected to the recovery tank through a pipeline and a valve.

[0008] Furthermore, a liquid baffle is provided between the overflow chamber and the separation chamber, a gap is left between the liquid baffle and the inner wall of the shell, and the condensate inlet extends to the top of the liquid baffle through a pipeline.

[0009] Furthermore, a distribution pipe is installed in the middle and upper part of the distillation tower, and the distribution pipe is connected to the reflux port.

[0010] Furthermore, the ammonia generating device comprises a liquid ammonia buffer tank and an ammonia evaporator. The liquid ammonia buffer tank is connected to the ammonia evaporator through a pipeline and a valve. The top ammonia outlet of the ammonia evaporator is connected to the air intake buffer tank through a pipeline and a valve.

[0011] Furthermore, the bottom of the raw material preparation kettle is connected to the reaction kettle and the catalyst preparation kettle through pipelines.

[0012] Furthermore, a flow meter is installed on the pipeline between the air intake buffer tank and the reactor.

[0013] Furthermore, the condenser includes two stages of shell and tube heat exchangers arranged in series.

[0014] After adopting the above technical scheme, the beneficial effects of the utility model are as follows: by compressing the non-condensable gases such as hydrogen and ammonia in the reaction process through a compressor to form a gas of a certain pressure, and then mixing it with ammonia in an air intake buffer tank, the gas surges upward from the bottom of the reactor through a distribution pipe at a certain speed, the internal catalyst and raw materials are fully stirred and mixed, while increasing the contact time and contact range of ammonia, raw materials and catalyst, thereby accelerating the reaction process, and adjusting the pressure of the gas entering the reactor through the control of the bypass branch, promoting the main reaction, avoiding the occurrence of by-products of primary amines, secondary amines and aldol condensation, and improving the purity of the finished product. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 It is the reaction principle diagram of the utility model.

[0016] Figure 2 Schematic diagram of the structure of the oil-water separator.

[0017] In the figure: reactor 1, raw material preparation kettle 2, catalyst preparation kettle 3, ammonia generator 4, liquid ammonia buffer tank 41, ammonia evaporator 42, fractionation tower 5, condenser 6, oil-water separator 7, overflow chamber 71, separation chamber 72, liquid baffle 73, circulating gas buffer tank 8, compressor 9, air intake buffer tank 10, hydrogen pipeline 11, bypass branch 12. DETAILED DESCRIPTION

[0018] The specific implementation of the utility model is further described in detail below with reference to the accompanying drawings:

[0019] like Figure 1 As shown, the high-purity trioctyldecyl tertiary amine preparation system consists of a reaction kettle 1, a raw material preparation kettle 2, a catalyst preparation kettle 3, an ammonia generator 4, a fractionating tower 5, a condenser 6, an oil-water separator 7, a circulating gas buffer tank 8, a compressor 9, an air intake buffer tank 10, and pipes and valves connecting the various components. It is used for the synthesis of trioctyldecyl tertiary amine.

[0020] The reactor 1 is equipped with a heat exchange coil, and the top of the reactor is provided with a material feed port, a catalyst inlet, a gas inlet, a gas outlet and a tower reflux port, and the bottom of the reactor 1 is provided with a discharge port. The raw material preparation kettle 2 is filled with raw material alcohol, which enters the reactor 1 from the material inlet through a pipeline and a valve, and the catalyst preparation kettle 32 is filled with a solid granular catalyst. The bottom of the raw material preparation kettle 2 is connected to the catalyst preparation kettle 3 through a pipeline and inputs liquid raw materials and catalysts for mixing, and the catalyst mixture enters the reactor 1 from the catalyst inlet through a pipeline and a valve to participate in the reaction.

[0021] The air inlet buffer tank 10 is connected to the ammonia generator 4 and the hydrogen pipeline 11. The ammonia generator 4 includes a liquid ammonia buffer tank 41 and an ammonia evaporator 42. The liquid ammonia buffer tank 41 is connected to the ammonia evaporator 42 through a pipeline and a valve. The ammonia outlet at the top of the ammonia evaporator 42 is connected to the air inlet buffer tank 10 through a pipeline and a valve. After the ammonia and hydrogen are mixed in the air inlet buffer tank 10, they enter the reactor 1 from the gas inlet through the pipeline to form a hydrogen atmosphere in the reactor. At the same time, the ammonia reacts with the raw material to generate trioctyldecyl tertiary amine. A flow meter is installed on the pipeline between the air inlet buffer tank 10 and the reactor 1.

[0022] A gas distribution device is installed at the bottom of the reactor 1, and the gas distribution device is connected to the gas inlet through a pipeline. After the gas in the air intake buffer tank 10 enters the reactor 1, it surges from bottom to top below the bottom liquid level, and the raw materials and catalyst inside are evenly mixed. During the churning process, the ammonia fully contacts and reacts with the raw materials, which promotes the progress of the reaction and improves the efficiency of the reaction.

[0023] The hydrogen, unreacted ammonia, evaporated water and finished product steam in the reactor 1 enter the fractionation tower 5 from the gas outlet of the reactor through the pipeline and valve. The gas is partially condensed in the fractionation tower 5. The condensed condensate returns to the reactor 1 from the bottom of the fractionation tower 5 through the pipeline and the tower reflux port to continue the reaction. The uncondensed steam enters the condenser 6 from the steam outlet at the top of the fractionation tower 5 to condense. The condenser 6 includes a two-stage shell and tube heat exchanger arranged in series. The water in the steam and part of the finished product and the raw material are liquefied in the condenser 6 and then enter the oil-water separator 7 for collection. The uncondensed gas enters the circulating gas buffer tank 8 through the pipeline. The circulating gas buffer tank 8 is connected to the compressor 9 through the pipeline. The air intake of the compressor 9 sucks out and compresses the gas. The compressed high-pressure gas enters the air intake buffer tank 10 through the pipeline, and after mixing with the ammonia, enters the reactor 1 for circulation reaction.

[0024] In order to prevent the gas from churning or having a short residence time after entering the reactor due to excessive gas pressure after compression, a bypass branch 12 is installed between the air intake and exhaust ports of the compressor 9, and a bypass regulating valve is installed on the bypass branch 12. By adjusting the opening degree of the regulating valve and the power of the compressor 9, the gas pressure can be controlled, thereby controlling the intake of ammonia and avoiding the production of by-products.

[0025] The oil-water separator 7 includes a shell, the upper part of the shell is an overflow chamber 71, the lower part of the shell is a separation chamber 72, a liquid baffle plate 73 is arranged between the overflow chamber 71 and the separation chamber 72, a gap is left between the liquid baffle plate 73 and the inner wall of the shell, a condensate inlet is arranged on one side of the overflow chamber 71, the condensate inlet is connected to the condensate outlet of the condenser 6, and the condensate inlet is extended to the top of the liquid baffle plate 73 through a pipeline. The condensed condensate slowly enters the separation chamber 72 after being blocked by the liquid baffle plate 73, and is layered in the separation chamber, wherein water is located in the lower layer and the finished product is located in the upper layer. An overflow port is arranged at the top of the overflow chamber 71, and the overflow port is connected to the reflux port at the upper part of the fractionation tower 5 through a pipeline, and the oil phase in the upper layer refluxes into the fractionation tower 5 by overflow. A distribution pipe connected to the reflux port is installed in the middle and upper part of the fractionation tower 5, and the refluxed oil phase refluxes downward uniformly. The bottom of the separation chamber 72 is provided with a liquid outlet, which is connected to the recovery tank through a pipeline and a valve, and the lower water phase is discharged through the pipeline in time periods. A liquid level meter and a sight glass are provided on the oil-water separator to facilitate observation of the liquid level of the internal water phase and facilitate timely discharge.

Claims

1. A high-purity trioctyldecyl tertiary amine preparation system, comprising a reactor and a fractionation tower, wherein a heat exchange coil is installed in the reactor, a material feed port, a catalyst inlet, a gas inlet, a gas outlet and a tower reflux port are arranged on the top of the reactor, the material inlet is connected to a raw material preparation reactor through a pipeline and a valve, the catalyst inlet is connected to a catalyst preparation reactor through a pipeline and a valve, the gas inlet is connected to an ammonia generator, the gas outlet is connected to the fractionation tower through a pipeline and a valve, the bottom of the fractionation tower is connected to the tower reflux port through a pipeline and a valve, a steam outlet is arranged on the top of the fractionation tower, the steam outlet is connected to a condenser through a pipeline, and a discharge port is arranged at the bottom of the reactor, characterized in that: The condensate outlet of the condenser is connected to the oil-water separator through a pipeline, and the non-condensable gas outlet of the condenser is connected to a circulating gas buffer tank through a pipeline, and the circulating gas buffer tank is connected to a compressor, and the circulating buffer tank is connected to the air intake of the compressor through a pipeline, and the exhaust port of the compressor is connected to an intake buffer tank through a pipeline and a control valve; a bypass branch is installed between the air intake and exhaust ports of the compressor, and a bypass regulating valve is installed on the bypass branch; the intake buffer tank is connected to an ammonia generator and a hydrogen pipeline, and the intake buffer tank is connected to the gas inlet of the reactor through a pipeline and a valve, and a gas distribution device is installed at the bottom of the reactor, and the gas distribution device is connected to the gas inlet through a pipeline.

2. The high-purity trioctyldecyl tertiary amine preparation system according to claim 1, characterized in that: The oil-water separator includes a shell, the upper part of the shell is an overflow chamber, the lower part of the shell is a separation chamber, a condensate inlet is provided on one side of the overflow chamber, the condensate inlet is connected to the condensate outlet of the condenser, an overflow port is provided on the top of the overflow chamber, and the overflow port is connected to the reflux port on the upper part of the distillation tower through a pipeline; a liquid outlet is provided at the bottom of the separation chamber, and the liquid outlet is connected to a recovery tank through a pipeline and a valve.

3. The high-purity trioctyldecyl tertiary amine preparation system according to claim 2, characterized in that: A liquid baffle is arranged between the overflow chamber and the separation chamber, a gap is left between the liquid baffle and the inner wall of the shell, and the condensate inlet extends to the top of the liquid baffle through a pipeline.

4. The high-purity trioctyldecyl tertiary amine preparation system according to claim 2, characterized in that: A distribution pipe is installed in the middle and upper part of the distillation tower, and the distribution pipe is connected to the reflux port.

5. The high-purity trioctyldecyl tertiary amine preparation system according to claim 1, characterized in that: The ammonia generating device comprises a liquid ammonia buffer tank and an ammonia evaporator. The liquid ammonia buffer tank is connected to the ammonia evaporator through a pipeline and a valve. The top ammonia outlet of the ammonia evaporator is connected to the air intake buffer tank through a pipeline and a valve.

6. The high-purity trioctyldecyl tertiary amine preparation system according to claim 1, characterized in that: The bottom of the raw material preparation kettle is connected to the reaction kettle and the catalyst preparation kettle through pipelines.

7. The high-purity trioctyldecyl tertiary amine preparation system according to claim 1, characterized in that: A flow meter is installed on the pipeline between the air intake buffer tank and the reactor.

8. The high-purity trioctyldecyl tertiary amine preparation system according to claim 1, characterized in that: The condenser comprises two stages of shell and tube heat exchangers arranged in series.

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