Preparation device of methyl monoethanolamine and methyldiethanolamine or dimethylethanolamine

Abstract

The utility model provides a preparation device of methyl monoethanolamine and methyldiethanolamine or dimethylethanolamine, which comprises the following steps: ethylene oxide and raw materials react in a reactor, and one part of a material discharged from the top of the reactor enters the middle part of a downstream deamination tower; a stabilizer A and a stabilizer B are introduced into the lower part of the deamination tower, a material obtained at the bottom of the deamination tower sequentially enters the middle part of a stabilizer A removal tower, a material obtained at the bottom of the stabilizer A removal tower enters the middle part of a product light component removal tower, and the top of the product light component removal tower is subjected to condensation treatment to obtain a first product; or materials obtained at the bottom of the product light component removal tower enter a product refining tower, and a second product is obtained at the top of the product refining tower. The raw material conversion rate is increased from about 95% to 99.9% or above, the processing cost is reduced by about 10,000,000 yuan every year by taking 20,000 tons / year productivity as an example, and the economic benefit is increased.

Description

Technical Field

[0001] The utility model belongs to the field of organic synthesis, in particular to a preparation device for methylmonoethanolamine and methyldiethanolamine or dimethylethanolamine. Background Art

[0002] The methylethanolamine series products mainly include N-methylmonoethanolamine (MMEA), N-methyldiethanolamine (MDEA) and N,N-dimethylethanolamine (DMEA).

[0003] The methylethanolamine series of products is a novel solvent with excellent selective desulfurization and decarbonization properties, boasting high selectivity, low solvent consumption, significant energy savings, and resistance to degradation. It is widely used as an emulsifier for desulfurization and purification of oilfield and coal gas, as an acid gas absorbent, an acid-base control agent, and a polyurethane foam catalyst. With the presence of an activator, it can remove carbon dioxide from synthetic ammonia, leading to its widespread use in recent years in the absorption of carbon dioxide from flue gases. MDEA can also be used as a pesticide, emulsifier, semi-finished product for textile auxiliaries, an intermediate for the anti-tumor drug nitrogen mustard hydrochloride, a catalyst for carbamate coatings, a fiber auxiliaries, and as a drying accelerator for paints.

[0004] Currently, methylethanolamine products are all prepared through the amination reaction of methylamine (monomethylamine or dimethylamine) with ethylene oxide. Current production methods suffer from issues such as backward batch reactions, untimely heat removal, and poor product distillation processes. These methods result in low raw material conversion rates, low product yields, high energy consumption, and poor product stability, impacting economic benefits and product competitiveness.

[0005] The key points of this technical solution are how to take effective measures to solve the problems existing in the current production methods, and to improve the raw material conversion rate, product yield, product stability and reduce energy consumption. Utility Model Content

[0006] In view of this, the present invention aims to provide a device for preparing methyl monoethanolamine and methyl diethanolamine or dimethylethanolamine to solve at least one technical problem in the background technology.

[0007] In order to achieve the above-mentioned purpose, the technical solution of the utility model is achieved as follows:

[0008] A device for preparing methylmonoethanolamine and methyldiethanolamine or dimethylethanolamine, comprising a reactor, an amine removal tower, a stabilizer removal tower, a product lightness removal tower, and a product refining tower;

[0009] A raw material inlet pipe is provided at the bottom or below of the reactor;

[0010] An ethylene oxide inlet pipe is provided at the bottom or below of the reactor;

[0011] The top of the reactor is connected to the middle of the deamine tower, the bottom of the deamine tower is connected to the destabilizer A tower, and the bottom of the destabilizer A tower is connected to the middle of the product lightness removal tower;

[0012] If the raw material is monomethylamine, the top output material of the product light removal tower is cooled and then output as the first product, and the bottom of the product light removal tower is connected to the middle of the product refining tower; the top output material of the product refining tower is cooled and then output as the second product.

[0013] If the raw material is dimethylamine, the material output from the top of the product light-removal tower is cooled and then output as the first product, and the heavy component is output from the bottom of the product light-removal tower.

[0014] Furthermore, a first valve is provided on both the raw material inlet pipe and the ethylene oxide inlet pipe;

[0015] And / or, the top of the reactor is connected to the middle of the deamine tower through a pipeline, and the top of the reactor is connected to the first branch pipe and the second branch pipe respectively through a reflux pipeline; the first branch pipe is connected to the upper part of the reactor; and the second branch pipe is connected to the bottom of the reactor;

[0016] And / or, a second valve is provided on the return pipe;

[0017] And / or, a third valve is provided on the first branch pipe;

[0018] And / or, a reaction circulation heat collector and a reaction circulation pump are sequentially provided on the second branch pipe.

[0019] The present application relates to an amination reaction, which is a highly exothermic reaction. Heat must be removed promptly during the reaction process, otherwise excessive local heat release will occur, causing equipment overheating and the risk of equipment container rupture.

[0020] The reactor in this application features material extraction ports in the upper middle and top sections, which deliver high-temperature material to a reaction cycle heat exchanger. This heat is then used to generate low-pressure steam within the reaction cycle heat exchanger, thereby removing the heat of reaction. By installing a reaction cycle heat exchanger, the reactor generates low-pressure steam, which can be used to heat the reboiler in the distillation system, thereby reducing production energy consumption.

[0021] Furthermore, the top of the deamine tower is connected to the first reflux tank through a pipeline, and a first condenser is provided on the pipeline between the first reflux tank and the deamine tower; the bottom of the first reflux tank is connected to the upper part of the deamine tower through a pipeline, and the bottom of the first reflux tank is connected to the raw material inlet pipe through a pipeline;

[0022] Below the deamine tower are provided a stabilizer A inlet pipeline and a first stabilizer B inlet pipeline;

[0023] And / or, the bottom of the deamine tower is connected to the middle of the destabilizer A tower through a pipeline; the bottom of the deamine tower is connected to the bottom of the deamine tower through a pipeline, and a first heat exchanger is provided on the pipeline connecting the bottom of the deamine tower and the bottom of the deamine tower;

[0024] And / or, the top of the destabilizer tower A is connected to the second reflux tank via a pipeline; a second condenser is provided on the pipeline between the deamine tower and the second reflux tank; the bottom of the destabilizer tower A is connected to the middle of the product lightness removal tower via a pipeline;

[0025] And / or, the bottom of the second reflux tank is connected to the top of the destabilizer A tower through a pipeline, the bottom of the second reflux tank outputs stabilizer A through a pipeline, the bottom of the destabilizer A tower is connected to the bottom of the destabilizer A tower through a pipeline, and a second heat exchanger is provided on the pipeline between the bottom of the destabilizer A tower and the bottom of the destabilizer A tower.

[0026] Furthermore, a second stabilizer B inlet pipe is provided below the product lightness removal tower;

[0027] And / or, a third condenser is provided on the pipeline between the product lightness removal tower and the third reflux tank, the bottom of the third reflux tank is connected to the upper part of the product lightness removal tower through a pipeline, the bottom of the third reflux tank outputs the first product, and the upper part of the third reflux tank is connected to the vacuum system;

[0028] And / or, the bottom of the product lightness removal tower is connected to the middle of the product lightness removal tower via a pipeline, and the bottom of the product lightness removal tower is connected to the bottom of the product lightness removal tower via a pipeline; a third heat exchanger is provided on the pipeline between the bottom of the product lightness removal tower and the bottom of the product lightness removal tower;

[0029] And / or, a fourth condenser is provided on the pipeline between the product refining tower and the fourth reflux tank; the bottom of the fourth reflux tank is connected to the upper part of the product refining tower via a pipeline, the bottom of the fourth reflux tank outputs the second product, and the upper part of the fourth reflux tank is connected to the vacuum system;

[0030] and / or, the bottom of the product refining tower is connected to the lower portion of the product refining tower via a pipeline, and a fourth heat exchanger is provided on the pipeline between the bottom of the product refining tower and the lower portion of the product refining tower;

[0031] And / or, if the product is monomethylamine, a first heavy component output pipeline is provided at the bottom of the product refining tower;

[0032] If the product is dimethylamine, a second heavy component output pipeline is provided at the bottom of the product light component removal tower.

[0033] Compared with the prior art, the device for preparing methylmonoethanolamine and methyldiethanolamine or dimethylethanolamine described in the present invention has the following advantages:

[0034] 1. This application solves the problem of low raw material reaction conversion rate by setting up multiple feeding points in the reactor. Through this process technology, the raw material conversion rate is increased from about 95% to more than 99.9%. Taking a production capacity of 20,000 tons / year as an example, the annual processing cost is reduced by about 10 million yuan, thereby improving economic benefits.

[0035] 2. This application is equipped with an external circulation heat extraction system for the reactor, which solves the problem of production energy consumption. Taking a production capacity of 20,000 tons / year as an example, through this process technology, steam consumption is reduced by about 3.0t / h and annual processing costs are reduced by about 6.8 million yuan.

[0036] 3. This application solves the problem of low product yield by providing an injection method of stabilizer A. Through this process technology, the product yield is increased from about 92% to more than 99%. Taking a production capacity of 20,000 tons / year as an example, the annual economic benefit increases by about 20 million yuan. In addition, by providing an injection method of stabilizer B, the problem of poor product stability is solved. Through this process technology, the color of the product can be stably maintained below 20, and basically no exceeding the standard will occur. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] The accompanying drawings, which constitute part of the present invention, are intended to provide a further understanding of the present invention. The exemplary embodiments of the present invention and their descriptions are intended to explain the present invention and do not constitute an improper limitation of the present invention. In the accompanying drawings:

[0038] Figure 1 This is a schematic diagram of an apparatus used in the method for preparing methylmonoethanolamine or methyldiethanolamine described in Example 1 of the present utility model;

[0039] Figure 2 This is a schematic diagram of the apparatus used in the method for preparing dimethylethanolamine described in Example 7 of the present invention.

[0040] Description of reference numerals:

[0041] 1. Reactor; 2. Reaction cycle heat collector; 3. Reaction circulation pump; 4. Deamine tower; 5. Destabilizer A tower; 6. Product lightness removal tower; 7. Product refining tower; 8. Third reflux tank; 9. Fourth reflux tank; 10. First valve; 11. Second valve; 12. Third valve; 13. First condenser; 14. First reflux tank; 15. First heat exchanger; 16. Second reflux tank; 17. Second condenser; 18. Second heat exchanger; 19. Fourth heat exchanger; 20. Third condenser; 21. Third heat exchanger; 22. Fourth condenser. DETAILED DESCRIPTION

[0042] It should be noted that, in the absence of conflict, the embodiments of the present invention and the features therein can be combined with each other.

[0043] The present invention will be described in detail below with reference to the accompanying drawings and in combination with embodiments.

[0044] Implementation Case 1:

[0045] A device for preparing methylmonoethanolamine and methyldiethanolamine comprises a reactor 1, an amine removal tower 4, a destabilizer A tower 5, a product lightness removal tower 6, and a product refining tower 7. A raw material inlet pipe is provided at the bottom or below of the reactor 1. An ethylene oxide inlet pipe is provided at the bottom or below of the reactor 1. The top of the reactor 1 is connected to the middle of the amine removal tower 4, the bottom of the amine removal tower 4 is connected to the destabilizer A tower 5, and the bottom of the destabilizer A tower 5 is connected to the middle of the product lightness removal tower 6. If the raw material is monomethylamine, the material output from the top of the product lightness removal tower 6 is cooled and then output as a first product. The bottom of the product lightness removal tower 6 is connected to the middle of the product refining tower 7. The material output from the top of the product refining tower 7 is cooled and then output as a second product.

[0046] A first valve 10 is provided on both the raw material inlet pipe and the ethylene oxide inlet pipe; the top of the reactor 1 is connected to the middle of the deamine tower 4 through a pipeline, and the top of the reactor 1 is connected to the first branch pipe and the second branch pipe respectively through a reflux pipe; the first branch pipe is connected to the upper part of the reactor 1; the second branch pipe is connected to the bottom of the reactor 1, a second valve 11 is provided on the reflux pipe, and a third valve 12 is provided on the first branch pipe; a reaction cycle heat collector 2 and a reaction circulation pump 3 are provided on the second branch pipe in sequence.

[0047] The top of the deamine tower 4 is connected to the first reflux tank 14 via a pipeline, and a first condenser 13 is provided on the pipeline between the first reflux tank 14 and the deamine tower 4; the bottom of the first reflux tank 14 is connected to the upper part of the deamine tower 4 via a pipeline, and the bottom of the first reflux tank 14 is connected to the raw material inlet pipe via a pipeline; a stabilizer A inlet pipeline and a first stabilizer B inlet pipeline are provided below the deamine tower 4;

[0048] The bottom of the deamine tower 4 is connected to the middle of the destabilizer A tower 5 through a pipeline; the bottom of the deamine tower 4 is connected to the bottom of the deamine tower 4 through a pipeline, and a first heat exchanger 15 is provided on the pipeline connecting the bottom of the deamine tower 4 and the bottom of the deamine tower 4;

[0049] The top of the destabilizer A tower 5 is connected to the second reflux tank 16 through a pipeline; a second condenser 17 is provided on the pipeline between the deamine tower 4 and the second reflux tank 16; the bottom of the destabilizer A tower 5 is connected to the middle part of the product light removal tower 6 through a pipeline, the bottom of the second reflux tank 16 is connected to the top of the destabilizer A tower 5 through a pipeline, and the bottom of the second reflux tank 16 outputs stabilizer A through a pipeline; the bottom of the destabilizer A tower 5 is connected to the bottom of the destabilizer A tower 5 through a pipeline, and a second heat exchanger 18 is provided on the pipeline between the bottom of the destabilizer A tower 5 and the bottom of the destabilizer A tower 5.

[0050] A second stabilizer B inlet pipe is provided below the product lightness removal tower 6;

[0051] A third condenser 20 is provided on the pipeline between the product light-removing tower 6 and the third reflux tank 8, the bottom of the third reflux tank 8 is connected to the upper part of the product light-removing tower 6 through a pipeline, the bottom of the third reflux tank 8 outputs the first product, and the upper part of the third reflux tank 8 is connected to the vacuum system; the bottom of the product light-removing tower 6 is connected to the bottom of the product light-removing tower 6 through a pipeline; a third heat exchanger 21 is provided on the pipeline between the bottom of the product light-removing tower 6 and the bottom of the product light-removing tower 6; a fourth condenser 22 is provided on the pipeline between the product refining tower 7 and the fourth reflux tank 9; the bottom of the fourth reflux tank 9 is connected to the upper part of the product refining tower 7 through a pipeline, the bottom of the fourth reflux tank 9 outputs the second product, and the upper part of the fourth reflux tank 9 is connected to the vacuum system;

[0052] The bottom of the product refining tower 7 is connected to the bottom of the product refining tower 7 through a pipeline. A fourth heat exchanger 19 is provided on the pipeline between the bottom of the product refining tower 7 and the bottom of the product refining tower 7. The bottom of the product refining tower 7 is provided with a first heavy component output pipeline.

[0053] Reaction process: Ethylene oxide and monomethylamine are mixed and then enter the reaction process. Amination reaction occurs in reactor 1. The reaction product enters the deamination process 4 from the top of the reactor. Part of the circulating material enters the reaction circulation heat exchanger 2. After cooling, the material enters the reaction circulation pump 3, and is returned to the reactor after being pressurized by the reaction circulation pump.

[0054] There are two feed inlets below the reactor and one feed inlet at the bottom of the reactor;

[0055] The operating pressure of the reactor is 4 MPaG and the operating temperature is 140°C;

[0056] Two discharge ports are provided at the upper middle portion of the reactor, and one discharge port is provided at the top of the reactor.

[0057] The ratio of the material circulation volume of the other part of the top discharge of the reactor or the material extracted from the side line after cooling to the reaction circulation volume of ethylene oxide and raw materials is 80.

[0058] Deamination process: The reaction product enters the deamination process 4, and the material at the top of the deamination tower enters the first condenser 13 at the top of the tower, and enters the first reflux tank 14 after cooling. The material at the bottom of the tank is used to recover methylamine and is reused as raw material to the reactor 1.

[0059] The operating pressure of the deamine tower is 0.4 MPaG and the operating temperature is 140°C;

[0060] Stabilizer A is water, and the injection rate is 500 kg / h.

[0061] Stabilizer B is monoethanolamine, and the injection rate is 5 kg / h.

[0062] Destabilizer A process: The reaction product enters the destabilizer A tower 5, and the material at the top of the tower enters the second condenser 17 at the top of the tower. After cooling, the material at the bottom of the second reflux tank 16 is stabilizer A and can be recycled.

[0063] The operating temperature of the destabilizer tower A is 45~135℃, and the operating pressure is 8~15KPaA.

[0064] Product light removal process: After demethylamine, the material enters the product light removal tower 6. The material at the top of the product light removal tower enters the third condenser 20 at the top of the tower, and after cooling, enters the third reflux tank 8. The material at the bottom of the tank is sent out of the entire production unit as MMEA product (first product).

[0065] Stabilizer A enters the bottom of the deamine tower 4 after being accurately measured from the metering pump, and enters the subsequent destabilizer A process along with the reaction product.

[0066] Industrial verification has shown that the product of this project begins to thermally decompose at 130~140℃. The thermal decomposition rate is not high within 180℃, generally 1~5%. The thermal decomposition rate gradually increases around 200℃, and can reach up to 8~10%, causing serious product losses.

[0067] The operating pressure of the deamination process is 0.3~0.6MPaG, and reduced pressure operation cannot be used. Under this condition, the maximum operating temperature of the deamination process is 210℃. In order to lower the operating temperature, the process technology of injecting stabilizer A is adopted, and the operating temperature can be reduced to within 150℃, thereby achieving the purpose of improving product yield.

[0068] Stabilizer B enters the bottom of the deamine tower 4 after being accurately measured from the metering pump, and stabilizer B enters into the product and is sold with the product.

[0069] The product of the present application is prone to problems such as excessive chroma. After industrial application, the addition of stabilizer B can effectively prevent the product chroma from exceeding the standard, thereby achieving the purpose of improving product stability.

[0070] The operating temperature of the product lightness removal tower 6 is 55~170℃, and the operating pressure is 3~14KPaA.

[0071] Product refining process: The material produced by the product light removal process enters the product refining tower 7. The material at the top of the product refining tower 7 enters the fourth condenser at the top of the tower, and after cooling, enters the fourth reflux tank 9. The material at the bottom of the tank is sent out of the entire production unit as the MDEA product (second product), and the material at the bottom of the tower is sent out of the entire production unit as the heavy component.

[0072] The operating temperature of the product refining tower 7 is 130~170℃, and the operating pressure is 3~7KPaA.

[0073] The product of the lightness removal tower is methyl monoethanolamine (MMEA), and the parameters are shown in Table 1.

[0074] Table 1 Main process operating parameters

[0075] Serial number Process Device Name Operational parameters 1 Reaction process Reactor 1 2 feeding ports 2 Reaction process Reaction cycle heat exchanger 2 Circulation ratio 80 3 Deamination process Deamine tower 4 Stabilizer A (water) injection rate 500 kg / h Stabilizer B (monoethanolamine) injection rate 5 kg / h

[0076] According to the process flow of Implementation Case 1 and the operating parameters in Table 1, taking a 20,000 tons / year methylethanolamine unit as an example, the raw material conversion rate of the reaction process is 97%, and the annual processing cost is reduced by approximately RMB 2 million.

[0077] The reaction process produces 1.8t / h of low-pressure steam, reducing annual processing costs by approximately RMB 4 million.

[0078] The product yield of the deamination process has increased to about 96%. Taking a production capacity of 20,000 tons / year as an example, the annual economic benefit has increased by about 10 million yuan.

[0079] The present application sets up a multi-point feed system for the reactor, allowing the raw materials ethylene oxide and methylamine to enter the reactor through multiple points, thereby achieving uniform distribution of the raw materials and avoiding local accumulation of raw materials, thereby improving the raw material conversion rate.

[0080] In addition, an external circulation heat extractor is set up in the reactor to remove the reaction heat in time to avoid reaction risks. The removed heat can be used to generate low-pressure steam, which can be used as heating steam for the distillation tower reboiler, saving the consumption of utility steam and achieving the purpose of reducing energy consumption.

[0081] The present application provides a means of injecting stabilizer A, which reduces the operating temperature of the deamination process from 210°C to about 150°C, greatly reducing the decomposition rate of the product and achieving the purpose of improving the product yield.

[0082] The present application provides a means of injecting stabilizer B, which can keep the color of the product continuously stable, thereby achieving the purpose of improving product stability.

[0083] Implementation Case 2:

[0084] Compared with Implementation Case 1, the process flow of Implementation Case 2 does not change, only the operating parameters are changed, see Table 2.

[0085] Table 2 Main process operating parameters

[0086] Serial number Process Device Name Operation parameters 1 Reaction process Reactor 1 4 feeding ports 2 Reaction process Reaction cycle heat exchanger 2 Circulation ratio 150 3 Deamination process Deamine tower 4 Stabilizer A (water) injection rate 700 kg / h Stabilizer B (monoethanolamine) injection rate 15 kg / h

[0087] According to the process flow of Implementation Case 1 and the operating parameters in Table 2, taking a 20,000 tons / year methylethanolamine unit as an example, the raw material conversion rate of the reaction process is 98%, and the annual processing cost is reduced by approximately RMB 3 million.

[0088] The reaction process produces 2.3t / h of low-pressure steam, reducing annual processing costs by approximately RMB 5 million.

[0089] The product yield of the deamination process has increased to about 98%. Taking a production capacity of 20,000 tons / year as an example, the annual economic benefit has increased by about 16 million yuan.

[0090] Implementation Case 3:

[0091] Compared with Implementation Case 1, the process flow of Implementation Case 3 does not change, only the operating parameters are changed, see Table 3.

[0092] Table 3 Main process operating parameters

[0093] Serial number Process Device Name Operation parameters 1 Reaction process Reactor 1 5 feeding ports 2 Reaction process Reaction cycle heat exchanger 2 Circulation ratio 200 3 Deamination process Deamine tower 4 Stabilizer A (water) injection rate 900 kg / h Stabilizer B (monoethanolamine) injection rate 20 kg / h

[0094] According to the process flow of Implementation Case 1 and the operating parameters in Table 3, taking a 20,000 tons / year methylethanolamine unit as an example, the raw material conversion rate of the reaction process is 99.9%, reducing the annual processing cost by approximately RMB 10 million.

[0095] The reaction process produces 2.7t / h of low-pressure steam, reducing annual processing costs by approximately RMB 6 million.

[0096] The product yield of the deamination process has increased to about 99%. Taking a production capacity of 20,000 tons / year as an example, the annual economic benefit has increased by about 20 million yuan.

[0097] Implementation Case 4:

[0098] Compared with Implementation Case 1, the process flow of Implementation Case 4 does not change. It only stipulates that the specific types of stabilizer A and stabilizer B are n-hexane and monoethanolamine, respectively, as shown in Table 4.

[0099] Table 4 Main process operating parameters

[0100] Serial number Process Device Name Operation parameters 1 Reaction process Reactor 1 2 feeding ports 2 Reaction process Reaction cycle heat exchanger 2 Circulation ratio 80 3 Deamination process Deamine tower 4 Stabilizer A (n-hexane) injection rate 500 kg / h Stabilizer B (monoethanolamine) injection rate 5 kg / h

[0101] According to the process flow of Implementation Case 1 and the operating parameters in Table 4, taking a 20,000 tons / year methylethanolamine unit as an example, the product yield of the deamination process is increased to approximately 97.5%. Taking a 20,000 tons / year production capacity as an example, the annual economic benefit increases by approximately RMB 13.3 million.

[0102] Implementation Case 5:

[0103] Compared with Implementation Case 4, the process flow of Implementation Case 5 does not change. Only the specific types of stabilizer A and stabilizer B are changed, namely water and diethanolamine, respectively. The injection amount does not change, see Table 5.

[0104] Table 5 Main process operating parameters

[0105] Serial number Process Device Name Operation parameters 1 Reaction process Reactor 1 2 feeding ports 2 Reaction process Reaction cycle heat exchanger 2 Circulation ratio 80 3 Deamination process Deamine tower 4 Stabilizer A (water) injection rate 500 kg / h Stabilizer B (diethanolamine) injection rate 5 kg / h

[0106] According to the process flow of Implementation Case 4 and the operating parameters in Table 5, taking a 20,000 tons / year methylethanolamine unit as an example, the product yield of the deamination process is increased to approximately 97.9%. Taking a 20,000 tons / year production capacity as an example, the annual economic benefit increases by approximately RMB 15 million.

[0107] Implementation Case 6:

[0108] Compared with Implementation Case 5, Implementation Case 6 does not change the process flow. Only the specific type of stabilizer B is changed. The type of stabilizer A remains unchanged, and the injection amount remains unchanged. See Table 6.

[0109] Table 6 Main process operating parameters

[0110] Serial number Process Device Name Operation parameters 1 Reaction process Reactor 1 2 feeding ports 2 Reaction process Reaction cycle heat exchanger 2 Circulation ratio 80 3 Deamination process Deamine tower 4 Stabilizer A (water) injection rate 500kg / h Stabilizer B (triethanolamine) injection rate 5kg / h

[0111] According to the process flow of Implementation Case 4 and the operating parameters in Table 6, taking a 20,000 tons / year methylethanolamine unit as an example, the product yield of the deamination process is increased to approximately 98.3%. Taking a 20,000 tons / year production capacity as an example, the annual economic benefit increases by approximately RMB 17.2 million.

[0112] Implementation Case 7:

[0113] A dimethylethanolamine preparation device comprises a reactor 1, an amine removal tower 4, a destabilizer A tower 5, a product light-removing tower 6, and a product refining tower 7; a raw material inlet pipe is provided at the bottom or below of the reactor 1; an ethylene oxide inlet pipe is provided at the bottom or below of the reactor 1; the top of the reactor 1 is connected to the middle of the amine removal tower 4, the bottom of the amine removal tower 4 is connected to the destabilizer A tower 5, and the bottom of the destabilizer A tower 5 is connected to the middle of the product light-removing tower 6; if the raw material is dimethylamine, the first product is dimethylethanolamine.

[0114] A first valve 10 is provided on both the raw material inlet pipe and the ethylene oxide inlet pipe; the top of the reactor 1 is connected to the middle of the deamine tower 4 through a pipeline, and the top of the reactor 1 is connected to the first branch pipe and the second branch pipe respectively through a reflux pipe; the first branch pipe is connected to the upper part of the reactor 1; the second branch pipe is connected to the bottom of the reactor 1, a second valve 11 is provided on the reflux pipe, and a third valve 12 is provided on the first branch pipe; a reaction cycle heat collector 2 and a reaction circulation pump 3 are provided on the second branch pipe in sequence.

[0115] The top of the deamine tower 4 is connected to the first reflux tank 14 via a pipeline, and a first condenser 13 is provided on the pipeline between the first reflux tank 14 and the deamine tower 4; the bottom of the first reflux tank 14 is connected to the upper part of the deamine tower 4 via a pipeline, and the bottom of the first reflux tank 14 is connected to the raw material inlet pipe via a pipeline; a stabilizer A inlet pipeline and a first stabilizer B inlet pipeline are provided below the deamine tower 4;

[0116] The bottom of the deamine tower 4 is connected to the middle of the destabilizer A tower 5 through a pipeline; the bottom of the deamine tower 4 is connected to the bottom of the deamine tower 4 through a pipeline, and a first heat exchanger 15 is provided on the pipeline connecting the bottom of the deamine tower 4 and the bottom of the deamine tower 4;

[0117] The top of the destabilizer A tower 5 is connected to the second reflux tank 16 through a pipeline; a second condenser 17 is provided on the pipeline between the deamine tower 4 and the second reflux tank 16; the bottom of the destabilizer A tower 5 is connected to the middle part of the product light removal tower 6 through a pipeline, the bottom of the second reflux tank 16 is connected to the top of the destabilizer A tower 5 through a pipeline, and the bottom of the second reflux tank 16 outputs stabilizer A through a pipeline; the bottom of the destabilizer A tower 5 is connected to the bottom of the destabilizer A tower 5 through a pipeline, and a second heat exchanger 18 is provided on the pipeline between the bottom of the destabilizer A tower 5 and the bottom of the destabilizer A tower 5, and a second stabilizer B inlet pipeline is provided below the product light removal tower 6.

[0118] A third condenser 20 is provided on the pipeline between the product de-lightening tower 6 and the third reflux tank 8, the bottom of the third reflux tank 8 is connected to the upper part of the product de-lightening tower 6 through a pipeline, the bottom of the third reflux tank 8 outputs the first product, and the upper part of the third reflux tank 8 is connected to the vacuum system; the bottom of the product de-lightening tower 6 is connected to the bottom of the product de-lightening tower 6 through a pipeline; a third heat exchanger 21 is provided on the pipeline between the bottom of the product de-lightening tower 6 and the bottom of the product de-lightening tower 6, and a second heavy component output pipeline is provided at the bottom of the product de-lightening tower 6.

[0119] Reaction process: Ethylene oxide and dimethylamine are mixed and then enter the reaction process. Amination reaction occurs in reactor 1. The reaction product enters the deamination process 4 from the top of the reactor. Part of the circulating material enters the reaction circulation heat exchanger 2. After cooling, the material enters the reaction circulation pump 3, and is pressurized by the reaction circulation pump and then sent back to the reactor.

[0120] There are two feed inlets below the reactor and one feed inlet at the bottom of the reactor;

[0121] The operating pressure of the reactor is 4 MPaG and the operating temperature is 140°C;

[0122] Two discharge ports are provided at the upper middle portion of the reactor, and one discharge port is provided at the top of the reactor.

[0123] The ratio of the material circulation volume of the other part of the top discharge of the reactor or the material extracted from the side line after cooling to the reaction circulation volume of ethylene oxide and raw materials is 80.

[0124] Deamination process: The reaction product enters the deamination process 4, and the material at the top of the deamination tower enters the first condenser 13 at the top of the tower, and enters the first reflux tank 14 after cooling. The material at the bottom of the tank is used to recover methylamine and is reused as raw material to the reactor 1.

[0125] The operating pressure of the deamine tower is 0.4MPaG and the operating temperature is 160℃;

[0126] Stabilizer A is water, and the injection rate is 500 kg / h.

[0127] Stabilizer B is monoethanolamine, and the injection rate is 5 kg / h.

[0128] Destabilizer A process: The reaction product enters the destabilizer A tower 5, and the material at the top of the tower enters the second condenser 17 at the top of the tower. After cooling, the material at the bottom of the second reflux tank 16 is stabilizer A and can be recycled.

[0129] The operating temperature of the destabilizer tower A is 45~135℃, and the operating pressure is 8~15KPaA.

[0130] Product light removal process: After demethylation of amine, the material enters the product light removal tower 6. The material at the top of the product light removal tower enters the third condenser 20 at the top of the tower, and after cooling, enters the third reflux tank 8. The material at the bottom of the tank is sent out of the entire production unit as DMEA product.

[0131] The operating temperature of the product lightness removal tower 6 is 60~110℃, the operating pressure is 3~7KPaA, and the operating parameters are shown in Table 7.

[0132] Table 7 Main process operating parameters

[0133] Serial number Process Device Name Operational parameters 1 Reaction process Reactor 1 2 feeding ports 2 Reaction process Reaction cycle heat exchanger 2 Circulation ratio 80 3 Deamination process Deamine tower 4 Stabilizer A (water) injection rate 500 kg / h Stabilizer B (monoethanolamine) injection rate 5 kg / h

[0134] According to the process flow of Implementation Case 1 and the operating parameters in Table 1, taking a 20,000 tons / year methylethanolamine unit as an example, the raw material conversion rate of the reaction process is 97%, and the annual processing cost is reduced by approximately RMB 2 million.

[0135] The reaction process produces 1.8t / h of low-pressure steam, reducing annual processing costs by approximately RMB 4 million.

[0136] The product yield of the deamination process has increased to about 96%. Taking a production capacity of 20,000 tons / year as an example, the annual economic benefit has increased by about 10 million yuan.

[0137] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A device for preparing methylmonoethanolamine and methyldiethanolamine or dimethylethanolamine, characterized in that: It includes a reactor, an amine removal tower, a destabilizer A tower, a product light-removal tower, and a product refining tower; a raw material inlet pipe is provided at the bottom or below of the reactor; an ethylene oxide inlet pipe is provided at the bottom or below of the reactor; the top of the reactor is connected to the middle of the amine removal tower, the bottom of the amine removal tower is connected to the destabilizer A tower, and the bottom of the destabilizer A tower is connected to the middle of the product light-removal tower; If the raw material is monomethylamine, the output material from the top of the product lightness removal tower is cooled and then output as the first product; the bottom of the product lightness removal tower is connected to the middle of the product refining tower; the output material from the top of the product refining tower is cooled and then output as the second product; If the raw material is dimethylamine, the material output from the top of the product light-removal tower is cooled and then output as the first product, and the heavy component is output from the bottom of the product light-removal tower.

2. The device for preparing methylmonoethanolamine and methyldiethanolamine or dimethylethanolamine according to claim 1, wherein: The raw material inlet pipe and the ethylene oxide inlet pipe are both provided with a first valve.

3. The device for preparing methylmonoethanolamine and methyldiethanolamine or dimethylethanolamine according to claim 1, characterized in that: The top of the reactor is connected to the middle of the deamine tower through a pipeline, and the top of the reactor is connected to the first branch pipe and the second branch pipe respectively through a reflux pipeline; the first branch pipe is connected to the upper part of the reactor; the second branch pipe is connected to the bottom of the reactor.

4. The device for preparing methylmonoethanolamine and methyldiethanolamine or dimethylethanolamine according to claim 3, wherein: A second valve is provided on the return pipe; And / or, a third valve is provided on the first branch pipe; And / or, a reaction circulation heat collector and a reaction circulation pump are sequentially provided on the second branch pipe.

5. The device for preparing methylmonoethanolamine and methyldiethanolamine or dimethylethanolamine according to claim 1, characterized in that: The top of the deamine tower is connected to the first reflux tank through a pipeline, and a first condenser is provided on the pipeline between the first reflux tank and the deamine tower; the bottom of the first reflux tank is connected to the upper part of the deamine tower through a pipeline, and the bottom of the first reflux tank is connected to the raw material inlet pipe through a pipeline; Below the deamine tower are provided a stabilizer A inlet pipeline and a first stabilizer B inlet pipeline; And / or, the bottom of the deamine tower is connected to the middle of the destabilizer A tower through a pipeline; the bottom of the deamine tower is connected to the bottom of the deamine tower through a pipeline, and a first heat exchanger is provided on the pipeline connecting the bottom of the deamine tower and the bottom of the deamine tower.

6. The device for preparing methylmonoethanolamine and methyldiethanolamine or dimethylethanolamine according to claim 5, characterized in that: The top of the destabilizer tower A is connected to the second reflux tank through a pipeline; a second condenser is provided on the pipeline between the deamine tower and the second reflux tank; the bottom of the destabilizer tower A is connected to the middle of the product light removal tower through a pipeline.

7. The device for preparing methylmonoethanolamine and methyldiethanolamine or dimethylethanolamine according to claim 6, characterized in that: The bottom of the second reflux tank is connected to the top of the destabilizer A tower through a pipeline, and the bottom of the second reflux tank outputs stabilizer A through a pipeline; And / or, the bottom of the destabilizer tower A is connected to the bottom of the destabilizer tower A through a pipeline, and a second heat exchanger is provided on the pipeline between the bottom of the destabilizer tower A and the bottom of the destabilizer tower A.

8. The device for preparing methylmonoethanolamine and methyldiethanolamine or dimethylethanolamine according to claim 1, characterized in that: A second stabilizer B inlet pipe is provided below the product lightness removal tower; And / or, a third condenser is provided on the pipeline between the product light removal tower and the third reflux tank, the bottom of the third reflux tank is connected to the upper part of the product light removal tower through a pipeline, the bottom of the third reflux tank outputs the first product, and the upper part of the third reflux tank is connected to the vacuum system.

9. The device for preparing methylmonoethanolamine and methyldiethanolamine or dimethylethanolamine according to claim 8, characterized in that: The bottom of the product light-removing tower is connected to the bottom of the product light-removing tower through a pipeline; a third heat exchanger is provided on the pipeline between the bottom of the product light-removing tower and the bottom of the product light-removing tower; And / or, a fourth condenser is provided on the pipeline between the product refining tower and the fourth reflux tank; the bottom of the fourth reflux tank is connected to the upper part of the product refining tower via a pipeline, the bottom of the fourth reflux tank outputs the second product, and the upper part of the fourth reflux tank is connected to the vacuum system; And / or, the bottom of the product refining tower is connected to the lower part of the product refining tower through a pipeline, and a fourth heat exchanger is provided on the pipeline between the bottom of the product refining tower and the lower part of the product refining tower.

10. The device for preparing methylmonoethanolamine and methyldiethanolamine or dimethylethanolamine according to claim 1, characterized in that: If the product is monomethylamine, a first heavy component output pipeline is provided at the bottom of the product refining tower; If the product is dimethylamine, a second heavy component output pipeline is provided at the bottom of the product light component removal tower.

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