Production device of bis (octyl / decyl) methyl tertiary amine

Abstract

The utility model belongs to the technical field of production of fine chemicals, and particularly relates to a production device of bis (octyl / decyl) methyl tertiary amine. Comprising a packed tower, at least two groups of reaction kettles, at least two groups of rectifying towers, a first gas-liquid separator, a second gas-liquid separator, a first air heater and a second air heater, the packed tower is filled with a ceramic filler and a composite solid metal catalyst, and a bottom discharge port of the packed tower is connected with liquid inlets of the reaction kettles; the top of the packed tower is provided with a packed tower feed port and a packed tower gas outlet, one side of the lower part is provided with a packed tower gas inlet, and the outer wall is provided with a constant-temperature heat exchanger. According to the production device of the bis (octyl / decyl) methyl tertiary amine, provided by the utility model, the bis (octyl / decyl) methyl tertiary amine can be produced in a continuous feeding and discharging manner; the method effectively inhibits the generation of aldol condensation compounds of caprylic / capric acid caprylic / capric ester and caprylic / capric aldehyde, improves the utilization rate of raw materials, and reduces by-products.

Description

Technical Field

[0001] The utility model belongs to the technical field of fine chemical production, and particularly relates to a production device for di(octyl / decyl)methyl tertiary amine. Background Art

[0002] Dialkylmethyl tertiary amine is an important intermediate for the preparation of cationic and zwitterionic surfactants. It can be used in preservatives, fungicides, pigment dispersants, mineral flotation agents, cosmetics and other fields, and has high market value. Among them, di(octyl / decyl)methyl tertiary amine is prepared into quaternary ammonium salt surfactant due to its carbon chain length adaptation, showing better dispersing and bactericidal effects, and is a third-generation bactericide with excellent performance.

[0003] There are two main methods for preparing alkyl tertiary amines: the halogenation method and the fatty alcohol one-step method. The halogenation method requires multiple steps to react to obtain alkyl tertiary amines. Currently, alkyl tertiary amines are generally prepared by the fatty alcohol one-step method. Fatty alcohols react with ammonia in the presence of a catalyst and hydrogen to obtain a mixture of alkyl tertiary amines and water. For the preparation of disilyl alkyl tertiary amines, if the control is not appropriate, a large amount of long-chain alkyl alcohols will not react normally, resulting in the generation of long-chain aldol condensation products and long-chain alkyl ester impurities, which will affect product quality and increase production costs. Summary of the invention

[0004] In order to solve the above problems, the present invention provides a production device for di(octyl / decyl)methyl tertiary amine, which uses n-octyl / decyl alcohol and methylamine as raw materials, and produces di(octyl / decyl)methyl tertiary amine by continuous feeding and discharging under the action of metal catalyst and hydrogen reduction.

[0005] The technical solution of the utility model is: a production device for di(octyl / decyl)methyl tertiary amine,

[0006] The invention comprises a packed tower, at least two groups of reaction kettles, at least two groups of distillation towers, a first gas-liquid separator, a second gas-liquid separator, a first air heater and a second air heater.

[0007] The packed tower is filled with ceramic fillers and composite solid metal catalysts, the bottom discharge port of the packed tower is connected to the liquid inlet of the reactor, the top of the packed tower is provided with a packed tower feed port and a packed tower gas outlet, the lower side is provided with a packed tower gas inlet, the outer wall is provided with a constant temperature heat exchanger, the packed tower feed port is connected to the alcohol delivery pipeline through a pipeline, and the alcohol delivery pipeline is connected in series with a valve, a flow meter and a transmission pump;

[0008] The first gas-liquid separator and the first gas heater are connected in series to the pipeline connected to the gas outlet of the packing tower, and the pipeline between the first gas-liquid separator and the first gas heater is connected to the gas inlet pipe through a tee;

[0009] The reactor is provided with a reactor feed port, a reactor liquid inlet and a reactor gas outlet at the top, a reactor gas inlet and a reactor liquid outlet at the bottom, and a constant temperature heat exchanger is provided on the outer wall. The reactor liquid inlet is connected to the packing tower discharge port through a pipeline, and is connected in series with a valve, a flow meter and a transmission pump. The packing tower feed port is connected to the alcohol delivery pipeline through a pipeline, and is connected in series with a valve, a flow meter and a transmission pump.

[0010] The distillation tower is provided with a distillation tower gas outlet at the top, a distillation tower liquid inlet at the middle, and a distillation tower liquid outlet at the bottom. The distillation tower liquid inlet is connected to the reactor liquid outlet through a pipeline, and is connected in series with a valve, a flow meter and a transmission pump. The distillation tower gas outlet is connected to the alcohol recovery pipeline through a pipeline, and is connected in series with a valve and a transmission pump. The distillation tower liquid outlet is connected to the product transmission pipeline through a pipeline, and is connected in series with a valve and a transmission pump.

[0011] The gas outlet of the reactor is connected in series with the second gas-liquid separator and the second gas heater through a pipeline.

[0012] According to the production device of bis(octyl / decyl)methyl tertiary amine,

[0013] The first gas-liquid separator is provided with a first gas-liquid separator air inlet, a first gas-liquid separator air outlet and a first gas-liquid separator liquid outlet. The first gas-liquid separator air inlet is connected to the packing tower air outlet through a pipeline, the first gas-liquid separator liquid outlet is connected to the recovery water pipeline through a pipeline, and the valve, flow meter and transmission pump are connected in series.

[0014] According to the production device of di(octyl / decyl)methyl tertiary amine, the first air heater is provided with a first air heating air inlet and a first air heating air outlet, the first air heating air inlet is respectively connected to the first gas-liquid separator air outlet and the gas transmission pipeline through a pipeline and a tee, and the first air heating air outlet is connected to the packing tower air inlet through a pipeline;

[0015] According to the production device of bis(octyl / decyl)methyl tertiary amine, the second gas-liquid separator is provided with a second gas-liquid separator air inlet, a second gas-liquid separator air outlet and a second gas-liquid separator liquid outlet, the second gas-liquid separator air inlet is connected to the reactor air outlet through a pipeline, the second gas-liquid separator liquid outlet is connected to the recovery water pipeline through a pipeline, and a valve, a flow meter and a transmission pump are connected in series;

[0016] According to the production device of di(octyl / decyl)methyl tertiary amine, the second air heater is provided with a second air heating inlet and a second air heating outlet, the second air heating inlet is connected to the second gas-liquid separator outlet through a pipeline, and is connected in series with a one-way valve, a circulation pump and a barometer, and the outlet is connected to the reactor inlet through a pipeline.

[0017] According to the production device of bis(octyl / decyl)methyl tertiary amine, the tower diameter ratio of the packed tower is (3~5):1, and 0.7~0.8 volumes of fillers and composite solid metal catalysts are randomly piled in the packed tower. The fillers are made of ceramic material with an outer diameter of 25~50 mm, preferably ball rings made of ceramic material. The volume ratio of the fillers to the composite solid metal catalyst is 2:1.

[0018] According to the production device of di(octyl / decyl)methyl tertiary amine, the three ports of the tee are respectively connected to the first gas-liquid separation outlet through pipelines, and are connected in series with a one-way valve; connected to the first air heating inlet through a pipeline, and are connected in series with a transmission pump and a barometer; connected to the gas delivery pipeline through a pipeline, and are connected in series with a one-way valve, a gas flow meter and an air pressure pump.

[0019] According to the production device of di(octyl / decyl)methyl tertiary amine, an atomizing nozzle is installed at the air inlet of the reaction kettle, and the nozzle diameter is 0.1-0.15 mm.

[0020] According to the production device of di(octyl / decyl)methyl tertiary amine, the reaction kettle and the distillation tower can be connected in parallel in N numbers according to actual needs, N≥2, and the other connecting pipelines are all connected in series with one-way valves.

[0021] Beneficial effects of the present invention:

[0022] The utility model provides a production device for di(octyl / decyl)methyl tertiary amine, which can produce di(octyl / decyl)methyl tertiary amine by continuous feeding and discharging. While realizing continuous production, the generation of octyl / decyl octyl / decanoate and octyl / decyl aldehyde condensation products is effectively suppressed, thereby improving the utilization rate of raw materials, reducing the generation of by-products, improving product quality, and reducing production costs. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 This is a schematic diagram of the overall structure of the utility model

[0024] In the figure: 1. Packing tower, 101. Packing tower air inlet, 102. Packing tower feed inlet, 103. Packing tower air outlet, 104. Packing tower discharge port, 105. Constant temperature heat exchanger, 2. Reactor, 201. Reactor air inlet, 202. Reactor liquid inlet, 203. Reactor feed inlet, 204. Reactor air outlet, 205. Reactor liquid outlet, 206. Constant temperature heat exchanger, 3. Distillation tower, 301. Distillation tower liquid inlet, 302. Distillation tower air outlet, 303. Distillation tower liquid outlet, 4. First Gas-liquid separator, 401, first gas-liquid separation air inlet, 402, first gas-liquid separation air outlet, 403, first gas-liquid separation liquid outlet, 5, first gas heater, 501, first gas heating air inlet, 502, first gas heating air outlet, 6, second gas-liquid separator, 601, second gas-liquid separation air inlet, 602, second gas-liquid separation air outlet, 603, second gas-liquid separation liquid outlet, 7, second gas heater, 701, second gas heating air inlet, 702, second gas heating air outlet. DETAILED DESCRIPTION

[0025] The specific contents of the utility model are described in detail below:

[0026] The utility model discloses a production device for disoctyl / decylmethyl tertiary amine, comprising a packing tower 1, at least two groups of reaction kettles 2, at least two groups of rectification towers 3, a first gas-liquid separator 4, a second gas-liquid separator 6, a first air heater and a second air heater.

[0027] Specifically, the packed tower 1 is filled with ceramic fillers and composite solid metal catalysts, the bottom discharge port of the packed tower 1 is connected to the liquid inlet of the reactor 2, the top of the packed tower 1 is provided with a packed tower feed port 102 and a packed tower gas outlet 103, a packed tower gas inlet 101 is provided on one side of the lower part, and a constant temperature heat exchanger 105 is provided on the outer wall, the packed tower feed port 102 is connected to the alcohol delivery pipeline through a pipeline, and a valve, a flow meter and a transmission pump are connected in series on the alcohol delivery pipeline;

[0028] The first gas-liquid separator 4 and the first gas heater 5 are connected in series to the pipeline connected to the gas outlet of the packing tower 1, and the pipeline between the first gas-liquid separator 4 and the first gas heater 5 is connected to the gas inlet pipe through a tee;

[0029] The reactor 2 is provided with a reactor feed port 203, a reactor 2 liquid inlet and a reactor gas outlet 204 at the top, a reactor gas inlet 201 and a reactor liquid outlet 205 at the bottom, and a constant temperature heat exchanger 105 is provided on the outer wall. The reactor 2 liquid inlet is connected to the packing tower discharge port 104 through a pipeline, and is connected in series with a valve, a flow meter and a transmission pump. The packing tower feed port 102 is connected to the alcohol delivery pipeline through a pipeline, and is connected in series with a valve, a flow meter and a transmission pump.

[0030] The distillation tower 3 is provided with a distillation tower gas outlet 302 at the top, a distillation tower liquid inlet 301 in the middle, and a distillation tower liquid outlet 303 at the bottom. The distillation tower liquid inlet 301 is connected to the reactor liquid outlet 205 through a pipeline, and is connected in series with a valve, a flow meter and a transmission pump. The distillation tower gas outlet 302 is connected to the alcohol recovery pipeline through a pipeline, and is connected in series with a valve and a transmission pump. The distillation tower liquid outlet 303 is connected to the product transmission pipeline through a pipeline, and is connected in series with a valve and a transmission pump.

[0031] The reactor gas outlet 204 is connected in series with the second gas-liquid separator 6 and the second gas heater 7 through a pipeline. The first gas-liquid separator 4 is provided with a first gas-liquid separator 4 gas inlet, a first gas-liquid separator 4 gas outlet and a first gas-liquid separator 4 liquid outlet. The first gas-liquid separator 4 gas inlet is connected to the packing tower gas outlet 103 through a pipeline, and the first gas-liquid separator 4 liquid outlet is connected to the recovery water pipeline through a pipeline, and is connected in series with a valve, a flow meter and a transmission pump.

[0032] The first air heater is provided with a first air heating inlet and a first air heating outlet. The first air heating inlet is connected to the outlet of the first gas-liquid separator 4 and the gas transmission pipeline through pipelines and tees respectively, and the first air heating outlet is connected to the packing tower inlet 101 through a pipeline.

[0033] The second gas-liquid separator 6 is provided with a second gas-liquid separator 6 air inlet, a second gas-liquid separator 6 air outlet and a second gas-liquid separator 6 liquid outlet. The second gas-liquid separator 6 air inlet is connected to the reactor air outlet 204 via a pipeline, the second gas-liquid separator 6 liquid outlet is connected to a recovery water pipeline via a pipeline, and valves, flow meters and transmission pumps are connected in series.

[0034] The second air heater is provided with a second air heating inlet and a second air heating outlet, the second air heating inlet is connected to the outlet of the second gas-liquid separator 6 via a pipeline, and is connected in series with a one-way valve, a circulation pump and a barometer, and the outlet is connected to the reactor inlet 201 via a pipeline.

[0035] The tower diameter ratio of the packed tower 1 is 3-5:1. 0.7-0.8 volumes of fillers and composite solid metal catalysts are randomly stacked in the packed tower 1. The fillers are made of ceramic material with an outer diameter of 25-50 mm, preferably ball rings made of ceramic material. The volume ratio of the fillers to the composite solid metal catalyst is 2:1.

[0036] The three ports of the tee are respectively connected to the first gas-liquid separation outlet 402 through pipelines, and connected in series with a one-way valve; connected to the first air heating inlet through pipelines, and connected in series with a transmission pump and a barometer; connected to the gas delivery pipeline through pipelines, and connected in series with a one-way valve, a gas flow meter and an air pressure pump.

[0037] The reactor air inlet 201 is equipped with an atomizing nozzle with a nozzle diameter of 0.1-0.15 mm. The reactor 2 and the distillation tower 3 can be connected in parallel in N numbers according to actual needs, N≥2, and the other connecting pipelines are all connected in series with one-way valves.

[0038] The present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0039] Main raw material equipment specifications:

[0040] The tower diameter ratio of the packing tower is 4:1, the volume is 5000L, and the packing is a cylindrical ball ring made of ceramic material, with an outer diameter of 38mm, a height of 38mm, and a thickness of 4mm;

[0041] The reactor volume is 3000L, and 3 reactors are connected in parallel;

[0042] The distillation tower has a capacity of 3000L and 3 are connected in parallel;

[0043] Atomizing nozzle diameter 0.1mm;

[0044] The catalyst is a solid copper-nickel catalyst;

[0045] The fatty alcohol used was industrial grade n-decanol.

[0046] Preliminary preparation:

[0047] Fill the packing tower with packing and catalyst in a volume ratio of 2:1, and fill to a liquid level of 4000L; open and close the corresponding valves, replace the air in the equipment system with hydrogen, close the valves, and keep the system airtight; pre-add 20kg of catalyst to the reactor. Example

[0048] Step 1: switch the corresponding valves, pump methylamine from the gas delivery pipeline through the tee from the air inlet 501 into the first air heater 5 for heating, and then enter the packed tower 1 through the packed tower air inlet 101, maintain a certain gas pressure in the system, open the constant temperature heat exchanger 105 to raise the temperature in the tower to 180±20°C, pump decanol from the feed port 102 at a certain flow rate, and the gas enters the first gas-liquid separator 4 through the air inlet 401 from the gas outlet 103 to remove water. After dehydration, the gas enters the first air heater 5 again through the gas outlet 402 and the tee for heating circulation. During the reaction process, methylamine gas is added through the gas delivery pipeline to maintain a constant gas pressure in the system. After 2 hours, when the liquid in the tower submerges the solid filler, the reaction liquid is continuously discharged from the discharge port 104 into the reactor 2, and the liquid level in the tower is maintained constant by controlling the discharge rate.

[0049] Step 2: After a certain amount of reaction liquid is enriched in the reactor, the reaction liquid is enriched in the parallel reactor by controlling the valve, the temperature in the reactor 2 is raised to 190±20°C by the constant temperature heat exchanger 206, and decanol is pumped into from the feed port 203 at a certain flow rate. The gas enters the second gas-liquid separator 6 from the gas outlet 204 for dehydration, and then enters the second air heater 7. After being heated, it is pumped into the reactor 2 for circulation again.

[0050] Step 3: After reacting for 2 hours, the liquid in the reactor 2 is filtered through a filter pump and pumped into the distillation tower 3 from the liquid inlet 301. The decanol and didecylmethyl tertiary amine are distilled out in turn and collected separately through the gas outlet 302. The remaining high-boiling point liquid is released from the liquid outlet 303 and pumped into the hydrolysis kettle for separation and reuse after hydrolysis.

[0051] The products from three kettles were collected to obtain 5278.7 kg of didecylmethyl tertiary amine, with a primary conversion rate (based on decanol) of 91.43% and a primary yield (based on decanol) of 94.62%.

[0052] The above is a preferred embodiment of the present invention. For ordinary technicians in this field, according to the teachings of the present invention, without departing from the principles and spirit of the present invention, changes, modifications, substitutions and variations made to the implementation methods are still within the scope of protection of the present invention.

Claims

1. A production device for bis(octyl / decyl)methyl tertiary amine, characterized in that: The invention comprises a packed tower (1), at least two groups of reaction kettles (2), at least two groups of distillation towers (3), a first gas-liquid separator (4), a second gas-liquid separator (6), a first air heater and a second air heater, The packed tower (1) is filled with ceramic fillers and composite solid metal catalysts. The bottom discharge port of the packed tower (1) is connected to the liquid inlet of the reaction kettle (2). The top of the packed tower (1) is provided with a packed tower feed port (102) and a packed tower gas outlet (103). A packed tower gas inlet (101) is provided on one side of the lower part. A constant temperature heat exchanger (105) is provided on the outer wall. The packed tower feed port (102) is connected to an alcohol delivery pipeline via a pipeline. A valve, a flow meter and a transmission pump are connected in series on the alcohol delivery pipeline. A first gas-liquid separator (4) and a first gas heater (5) are connected in series to a pipeline connected to a gas outlet of the packed tower (1); and a pipeline between the first gas-liquid separator (4) and the first gas heater (5) is connected to an air inlet pipe via a tee; The reactor (2) is provided with a reactor feed port (203), a reactor liquid inlet and a reactor gas outlet (204) at the top, a reactor gas inlet (201) and a reactor liquid outlet (205) at the bottom, and a constant temperature heat exchanger (105) is provided on the outer wall. The reactor (2) liquid inlet is connected to the packing tower discharge port (104) via a pipeline, and is connected in series with a valve, a flow meter and a transmission pump. The packing tower feed port (102) is connected to an alcohol delivery pipeline via a pipeline, and is connected in series with a valve, a flow meter and a transmission pump. The distillation tower (3) is provided with a distillation tower gas outlet (302) at the top, a distillation tower liquid inlet (301) at the middle, and a distillation tower liquid outlet (303) at the bottom. The distillation tower liquid inlet (301) is connected to the reactor liquid outlet (205) via a pipeline, and is connected in series with a valve, a flow meter, and a transmission pump. The distillation tower gas outlet (302) is connected to an alcohol recovery pipeline via a pipeline, and is connected in series with a valve and a transmission pump. The distillation tower liquid outlet (303) is connected to a product transmission pipeline via a pipeline, and is connected in series with a valve and a transmission pump. The reactor gas outlet (204) is connected in series to a second gas-liquid separator (6) and a second gas heater (7) via a pipeline.

2. The production device of bis(octyl / decyl)methyl tertiary amine according to claim 1, characterized in that: The first gas-liquid separator (4) is provided with a first gas-liquid separator (4) air inlet, a first gas-liquid separator (4) air outlet and a first gas-liquid separator (4) liquid outlet, the first gas-liquid separator (4) air inlet is connected to the packing tower air outlet (103) via a pipeline, the first gas-liquid separator (4) liquid outlet is connected to a recovery water pipeline via a pipeline, and a valve, a flow meter and a transmission pump are connected in series.

3. The production device of bis(octyl / decyl)methyl tertiary amine according to claim 1, characterized in that: The first air heater is provided with a first air heating inlet and a first air heating outlet, the first air heating inlet being connected to the outlet of the first gas-liquid separator (4) and the gas transmission pipeline respectively through a pipeline and a tee, and the first air heating outlet being connected to the air inlet (101) of the packing tower through a pipeline.

4. The production device of bis(octyl / decyl)methyl tertiary amine according to claim 1, characterized in that: The second gas-liquid separator (6) is provided with a second gas-liquid separator (6) air inlet, a second gas-liquid separator (6) air outlet and a second gas-liquid separator (6) liquid outlet, the second gas-liquid separator (6) air inlet is connected to the reactor air outlet (204) via a pipeline, the second gas-liquid separator (6) liquid outlet is connected to a recovery water pipeline via a pipeline, and is connected in series with a valve, a flow meter and a transmission pump.

5. The production device of bis(octyl / decyl)methyl tertiary amine according to claim 1, characterized in that: The second air heater is provided with a second air heating inlet and a second air heating outlet. The second air heating inlet is connected to the outlet of the second gas-liquid separator (6) via a pipeline, and is connected in series with a one-way valve, a circulation pump and a barometer. The outlet is connected to the air inlet (201) of the reactor via a pipeline.

6. The production device of bis(octyl / decyl)methyl tertiary amine according to claim 1, characterized in that: The tower diameter ratio of the packed tower (1) is (3-5):

1. 0.7-0.8 volume of packing and composite solid metal catalyst are randomly stacked in the packed tower (1). The packing is made of ceramic material with an outer diameter of 25-50 mm and a ball ring made of ceramic material. The volume ratio of the packing to the composite solid metal catalyst is 2:

1.

7. The production device of bis(octyl / decyl)methyl tertiary amine according to claim 1, characterized in that the three-way The three ports are respectively connected to the first gas-liquid separation outlet (402) through pipelines, and are connected in series with a one-way valve; connected to the first air heating inlet through pipelines, and are connected in series with a transmission pump and a barometer; connected to the gas delivery pipeline through pipelines, and are connected in series with a one-way valve, a gas flow meter and an air pressure pump.

8. The production device of bis(octyl / decyl)methyl tertiary amine according to claim 1, characterized in that: The air inlet (201) of the reactor is equipped with an atomizing nozzle, the nozzle diameter of which is 0.1-0.15 mm.

9. The production device of bis(octyl / decyl)methyl tertiary amine according to claim 1, characterized in that: The reactor (2) and the distillation tower (3) can be connected in parallel in N numbers according to actual needs, where N≥2, and the other connecting pipelines are all connected in series with one-way valves.

Images