A morpholine production system

Abstract

The present invention relates to the technical field of morpholine synthesis, and specifically to a morpholine production system comprising a reactor, a diethylene glycol vaporizer, an ammonia vaporizer, and a hydrogen supply unit connected to the reactor. The product outlet of the reactor is sequentially connected to a heat exchanger, a condenser, and a gas-liquid separator. The hydrogen supply unit comprises an ammonia scrubbing tower, a pressure swing adsorption tower, and a circulating fan. The liquid outlet of the gas-liquid separator is connected to a crude morpholine processing unit, the tail gas outlet of the gas-liquid separator is connected to the ammonia scrubbing tower, the outlet of the ammonia scrubbing tower and an off-site hydrogen device are connected to the pressure swing adsorption tower, and the purified gas outlet of the pressure swing adsorption tower, the hydrogen outlet of the gas-liquid separator, and the outlet of the ammonia vaporizer are sequentially connected to the reactor through a heat exchanger, a heating device, and the diethylene glycol vaporizer. The morpholine production system facilitates the recycling of hydrogen-containing waste gas from the system or the off-site hydrogen device, reduces material input, increases revenue, reduces waste gas emissions, and is environmentally friendly.

Description

Technical Field

[0001] The invention relates to the technical field of morpholine synthesis, and in particular to a morpholine production system. Background Art

[0002] Morpholine is an organic compound with the molecular formula C₄H₄NO₄. It is a colorless, oily liquid at room temperature. Industrially synthesized from diethylene glycol and ammonia in the presence of hydrogen and a catalyst, it is widely used in rubber, pharmaceuticals, pesticides, dyes, coatings, and other fields, serving as an important chemical raw material.

[0003] The existing technology uses a low-pressure gas-phase catalytic amination method for diethylene glycol. A certain proportion of diethylene glycol, liquid ammonia and hydrogen are vaporized and then enter a degassing device. The amination reaction is carried out under low pressure using a catalyst gas-solid phase catalytic reaction. This process requires the use of large amounts of hydrogen and catalyst. Therefore, how to improve the utilization rate of hydrogen and catalyst or reduce their usage is one of the important ways to increase corporate benefits.

[0004] In view of this, this application is hereby filed. Summary of the Invention

[0005] The present invention aims to overcome at least one defect in the prior art and provide a morpholine production system that can coordinate the use of multiple hydrogen sources and reduce material input. The morpholine production system can not only reduce the input of hydrogen raw materials, but also produce qualified morpholine products.

[0006] In order to solve the above technical problems and achieve the corresponding technical effects, the basic concept of the technical solution is as follows:

[0007] A morpholine production system includes a reactor and a diethylene glycol vaporizer, an ammonia vaporizer, and a hydrogen supply unit connected to the reactor. The product outlet of the reactor is sequentially connected to a heat exchanger, a condenser, and a gas-liquid separator. The hydrogen supply unit includes an ammonia scrubbing tower, a pressure swing adsorption tower, and a circulating fan.

[0008] The liquid outlet of the gas-liquid separator is connected to the crude morpholine processing unit, the tail gas outlet of the gas-liquid separator is connected to the ammonia washing tower, the outlet of the ammonia washing tower and the off-site hydrogen device are connected to the pressure swing adsorption tower, and the purified gas outlet of the pressure swing adsorption tower, the hydrogen outlet of the gas-liquid separator and the outlet of the ammonia vaporizer are connected to the reactor after passing through the heat exchanger, the heating device and the diethylene glycol vaporizer in sequence.

[0009] As one embodiment, a decarbonizer is provided on the connecting pipelines connecting the purified gas outlet of the pressure swing adsorption tower, the hydrogen outlet of the gas-liquid separator, and the outlet of the ammonia vaporizer to the heat exchanger.

[0010] As one method, a circulating fan I is provided on the pipeline connecting the purified gas outlet of the pressure swing adsorption tower to the decarbonizer, and a circulating fan II is provided on the pipeline connecting the hydrogen outlet of the gas-liquid separator to the decarbonizer.

[0011] As one approach, the off-site hydrogen device is a hydrogen output device of an off-site ammonia synthesis system; the desorption gas vent of the pressure swing adsorption tower is connected to a flare.

[0012] As one embodiment, the crude morpholine processing unit includes a deamination tower, a dehydration tower, a lightness removal tower and a product tower connected in sequence, the liquid outlet of the gas-liquid separator is connected to the deamination tower, and the liquid ammonia outlet of the deamination tower is connected to the ammonia vaporizer;

[0013] The liquid outlet of the deamination tower is connected to the dehydration tower, the top of the dehydration tower is provided with an impurity outlet for outputting water, N-methylmorpholine and N-ethylmorpholine, the bottom outlet of the dehydration tower is connected to the light component removal tower, the light component removal tower is provided with an outlet for outputting water and ethylene glycol monomethyl ether, the bottom of the light component removal tower is connected to the product tower, the top of the product tower is provided with a morpholine product outlet, and the bottom outlet of the product tower is connected to a high-boiling-point storage tank.

[0014] As one method, a synthesis intermediate tank for temporarily storing crude morpholine is provided between the liquid outlet of the gas-liquid separator and the deamination tower.

[0015] As a method, when the liquid level of the intermediate tank reaches 1 / 2~2 / 3 of the tank capacity and the pressure is 0.6~1.5MPa, the cooling water of the condenser of the deamination tower is kept in a circulating state, and the material is discharged from the synthesis intermediate tank to the deamination tower, and then heated at a rate of 30~80℃ / hour. The circulation volume of the cooling water is adjusted to control the top pressure of the deamination tower to 0.8~1.8Mpa, and then the ammonia production amount is adjusted according to the top temperature of the deamination tower, and the bottom temperature of the deamination tower is adjusted to 160~240℃.

[0016] Optionally, the bottom liquid level of the deamination tower is adjusted to maintain at 65-92% of the deamination tower capacity.

[0017] Optionally, the deamination tower controls the top temperature to be 30-35° C. and the pressure to be 0.8-1.8 MPa by adjusting the ammonia production rate.

[0018] As one embodiment, the pressure swing adsorption tower is provided with an inlet at the lower portion of the cylinder and a purified gas outlet at the upper portion, and a first porcelain ball layer, a first wire mesh layer, an adsorbent layer, a second wire mesh layer, and a second porcelain ball layer are provided in the cylinder from top to bottom between the purified gas outlet and the inlet.

[0019] The adsorbent layer consists of an activated carbon layer, a molecular sieve layer and an aluminum oxide layer from bottom to top.

[0020] As a method, the first wire mesh layer is fixed below the bed limiting structure provided on the inner wall of the cylinder, the first porcelain ball layer is provided with porcelain balls of φ15~25mm, and the second porcelain ball layer is provided with porcelain balls of φ2~5mm.

[0021] As one embodiment, based on the total mass of the adsorbent layers being 100%, the loading amount of the activated carbon layer is 25-32%, the loading amount of the molecular sieve layer is 65-72%, and the loading amount of the alumina layer is 1-3%.

[0022] As a method, the interior of the decarbonizer includes a cylindrical metal material filter layer and a cylindrical filter paper filter layer concentrically arranged from the inside to the outside; the cylindrical metal material filter layer is made of one or more of stainless steel mesh, sintered mesh or sintered felt.

[0023] As one approach, the carbon remover is provided with a filter element consisting of a primary wire mesh demister, a secondary microfiltration dust removal filter element, and a tertiary high-efficiency liquid removal filter element, performing a three-stage separation and filtration process;

[0024] The gas containing oil, dirt and solid particles enters from the inlet at the bottom of the decarbonizer, first passes through the first-stage wire mesh demister to separate large liquid droplets in the gas, then passes through the second-stage microfiltration dust removal filter element in an outside-in and inside-out manner to intercept solid particle impurities carried in the gas, and then passes through the third-stage high-efficiency liquid removal filter element in an inside-out manner to remove small droplets, thereby obtaining clean and dry gas.

[0025] As a method, the filter element is detachably suspended inside the shell of the carbon remover.

[0026] The technical solution of the present invention has the following advantages compared with the prior art:

[0027] 1. The hydrogen supply unit of the morpholine production system of the present invention can adapt to various hydrogen input conditions (including pure hydrogen and hydrogen to be recovered inside and outside the system) for processing, ensuring the purity of the hydrogen entering the reactor. It also facilitates the use of recovered hydrogen from hydrogen devices inside and outside the system, such as recovered hydrogen from the synthetic ammonia system, thereby reducing material input, increasing profits, and reducing waste gas emissions, which is environmentally friendly.

[0028] 2. The present invention further provides a carbon remover to prevent the alkane impurities produced by the side reaction from forming particulate carbon that affects the performance of the catalyst, and at the same time prevent the particulate carbon from flowing into other devices in the system with the circulating gas to cause blockage and affect the operating stability of the system.

[0029] 3. Furthermore, the internal filling structure of the pressure swing adsorption tower of the present invention helps to improve the purification effect of hydrogen, ensure the purity of hydrogen, and enable the recycled hydrogen to be used for the production of qualified morpholine products after treatment.

[0030] 4. The internal structure of the carbon remover of the present invention can ensure the carbon removal effect and is easy to replace. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] In order to more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the specific embodiments or the description of the prior art. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0032] Figure 1 This is a structural schematic diagram of a morpholine production system provided by the present invention.

[0033] Figure 2 The figure is a partial structural diagram of a pressure swing adsorption tower used in the morpholine production system of the present invention.

[0034] Figure 3 This is a schematic structural diagram of the decarbonizer of Example 3 of the present invention.

[0035] Figure 4 for Figure 3 Schematic diagram of the microfiltration filter structure shown.

[0036] Figure 5 for Figure 3 The ultrafiltration filter structure diagram is shown.

[0037] Figure 6 for Figure 3 The schematic diagram of the structure of the first-stage filtration device is shown.

[0038] Markings in the figure: 1-head; 2-first magnetic ball layer; 3-bed limiting structure; 4-first wire mesh layer; 5-adsorbent layer; 6-cylinder; 7-second wire mesh layer; 8-second magnetic ball layer; 9-gas distributor; 10-inlet; 11-purified gas outlet;

[0039] 1'-process gas outlet; 2'-pressure relief port; 3'-upper head; 4'-container flange; 5'-oil drain port; 6'-wire mesh demister; 7'-upper remote level port; 8'-lower head; 9'-lower remote level port; 10'-sewage outlet; 11'-hot water inlet; 12'-process gas inlet; 13'-tray; 14'-support; 15'-lower on-site level gauge port; 16'-upper on-site level gauge port; 17'-microfiltration filter; 18'-ultrafiltration filter; 19'-hanging box; 20'- Tank body; 21'-microfiltration filter lower head; 22'-microfiltration filter element; 23'-microfiltration filter support tube; 24'-microfiltration filter upper head; 25'-microfiltration filter oil-proof sealing ring; 26'-ultrafiltration filter element connector; 27'-ultrafiltration filter sealing ring; 28'-ultrafiltration filter rod; 29'-ultrafiltration filter element; 30'-ultrafiltration filter rod sealing ring; 31'-ultrafiltration filter nut; 32'-oil tank; 33'-pressure plate; 34'-bracket l. DETAILED DESCRIPTION

[0040] The technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. All other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making any creative efforts shall fall within the scope of protection of the present invention. Example 1

[0041] A morpholine production system, such as Figure 1 As shown, it includes a reactor and a diethylene glycol vaporizer, an ammonia vaporizer and a hydrogen supply unit connected to the reactor. The product outlet of the reactor is connected to a heat exchanger, a condenser and a gas-liquid separator in sequence. The hydrogen supply unit includes an ammonia washing tower, a pressure swing adsorption tower and a circulating fan.

[0042] The liquid outlet of the gas-liquid separator is connected to the crude morpholine processing unit, the tail gas outlet of the gas-liquid separator is connected to the ammonia washing tower, the outlet of the ammonia washing tower and the off-site hydrogen device are connected to the pressure swing adsorption tower, and the purified gas outlet 10 of the pressure swing adsorption tower, the hydrogen outlet of the gas-liquid separator and the outlet of the ammonia vaporizer are connected to the reactor after passing through the heat exchanger, the heating device and the diethylene glycol vaporizer in sequence.

[0043] The above-mentioned off-site hydrogen devices include pure hydrogen supply devices and devices for recovering gases discharged from other production systems whose main component is hydrogen, including but not limited to hydrogen discharge devices of ammonia synthesis systems.

[0044] As a solution, a decarbonizer is provided on the connecting pipelines connecting the purified gas outlet 10 of the pressure swing adsorption tower, the hydrogen outlet of the gas-liquid separator, and the outlet of the ammonia vaporizer to the heat exchanger.

[0045] In the morpholine production process of the present invention, a portion of the gas must be vented to control the methane content (an impurity formed by side reactions in the reactor) in the production system. Simultaneously, to recover ammonia from the vented air, the vented air is passed into an ammonia scrubber to remove ammonia, then into a pressure swing adsorption tower to remove methane from the vented air. The vented air is then returned to the production system as supplemental hydrogen, thereby improving material utilization.

[0046] The carbon remover can prevent carbon deposition on the catalyst, thus preventing carbon deposition from affecting the activity of the catalyst and the conversion rate of morpholine, thereby extending the service life of the catalyst and increasing production capacity.

[0047] As a solution, a circulating fan I is provided on the pipeline connecting the purified gas outlet 10 of the pressure swing adsorption tower to the decarbonizer, and a circulating fan II is provided on the pipeline between the hydrogen outlet of the gas-liquid separator and the decarbonizer.

[0048] In addition, the company also has an operating synthetic ammonia project, and hydrogen is also one of its important raw materials and is used in large quantities. Therefore, how to integrate the raw material utilization between the morpholine and synthetic ammonia projects in order to reduce raw material input while obtaining qualified products and increasing profits is an important direction worthy of research.

[0049] As a solution, the off-site hydrogen device is a hydrogen output device of the off-site ammonia synthesis system; the desorption gas vent of the pressure swing adsorption tower is connected to a flare.

[0050] As a solution, the crude morpholine processing unit includes a deamination tower, a dehydration tower, a lightness removal tower and a product tower connected in sequence, the liquid outlet of the gas-liquid separator is connected to the deamination tower, and the liquid ammonia outlet of the deamination tower is connected to the ammonia vaporizer;

[0051] The liquid outlet of the deamination tower is connected to the dehydration tower, and an impurity outlet including water, methylmorpholine (N-methylmorpholine) and ethylmorpholine (N-ethylmorpholine) is provided at the top of the dehydration tower. The bottom outlet of the dehydration tower is connected to the light component removal tower, and the light component removal tower is provided with an outlet for outputting water and ethylene glycol monomethyl ether. The bottom of the light component removal tower is connected to the product tower, and a morpholine product outlet is provided at the top of the product tower. The bottom outlet of the product tower is connected to a high-boiling-point storage tank.

[0052] After the crude morpholine product synthesized by the production system of the present invention undergoes the above treatment, the final product obtained has high purity and good quality, and ammonia is fully recovered and utilized.

[0053] As a solution, a synthesis intermediate tank for temporarily storing crude morpholine is provided between the liquid outlet of the gas-liquid separator and the deamination tower.

[0054] The above-mentioned synthesis intermediate tank is convenient for timely adjusting the production rhythm according to the progress of the production system, improving the flexibility of the production system, helping to reduce the power consumption of the production system, and improving the operational stability and sustainability of the system.

[0055] The following describes part of the workflow of the morpholine production system when an intermediate tank is set up:

[0056] When the liquid level of the intermediate tank reaches 2 / 3 of the tank capacity and the pressure is 1.5MPa, the cooling water of the condenser of the deamination tower is kept in a circulating state, and the material is discharged from the synthesis intermediate tank to the deamination tower, and then heated (the heating rate can be adjusted to 30-80℃ / hour, specifically 50℃ / hour here), and the circulation volume of the cooling water is adjusted to control the top pressure of the deamination tower to 1.8Mpa, and then the ammonia production volume is adjusted according to the top temperature of the deamination tower, and the bottom temperature of the deamination tower is adjusted to 240℃, and the discharge volume of the deamination tower is adjusted to adjust the bottom liquid level of the deamination tower to maintain at 65% of the deamination tower capacity.

[0057] like Figure 2 As shown, as a solution, the lower part of the cylinder of the pressure swing adsorption tower is provided with an inlet 10, the upper part is provided with a purified gas outlet 11, and the interior of the cylinder is provided with a first porcelain ball layer 2, a first wire mesh layer 4, an adsorbent layer 5, a second wire mesh layer 7 and a second porcelain ball layer 8 from top to bottom between the purified gas outlet 11 and the inlet 10;

[0058] The adsorbent layer 5 consists of an activated carbon layer, a molecular sieve layer and an aluminum oxide layer from bottom to top.

[0059] Specifically, based on the total mass of each layer of the adsorbent layer being 100%, the filling amount of the activated carbon layer is 32%, the filling amount of the molecular sieve layer is 65%, and the filling amount of the alumina layer is 3%.

[0060] The above-mentioned filling method of the adsorbent layer is helpful to improve the recovery rate and purity of hydrogen, can save materials, reduce costs, and can improve the purity of the final morpholine product produced.

[0061] As a solution, the first wire mesh layer 4 is fixed below the bed limiting structure 3 provided on the inner wall of the cylinder, the first porcelain ball layer 2 is provided with porcelain balls of φ15~25mm, and the second porcelain ball layer 8 is provided with porcelain balls of φ2~5mm.

[0062] The internal structure of the pressure swing adsorption tower can further improve the purification and adsorption effect. It can not only purify the hydrogen outside the boundary with higher precision, but also adsorb the hydrogen to be recycled inside or outside the system to meet the purity standards for reactor synthesis and reduce material input.

[0063] As a solution, a gas distributor 9 is arranged above the inlet 10. The gas distributor 9 is a hollow conical structure with the upper bottom facing upward, including an upper bottom covering the inlet 10 and a fan-shaped structure extending downward along the circumference of the upper bottom. The lower edge of the fan-shaped structure is provided with a mounting structure that is detachably connected to the outer periphery of the inlet 10.

[0064] On the one hand, the above-mentioned gas distributor 9 can evenly distribute the incoming gas to be treated to improve the adsorption purification effect. On the other hand, it can serve as a supporting structure to support the second magnetic ball layer 8 arranged thereon, reducing the internal structure setting. In addition, the gas distributor 9 is also easy to disassemble and replace.

[0065] As a solution, the interior of the decarbonizer is provided with a cylindrical metal material filter layer and a cylindrical filter paper filter layer arranged concentrically from the inside to the outside; the cylindrical metal material filter layer is made of one or more of stainless steel mesh, sintered mesh or sintered felt.

[0066] The carbon remover of the above structure can effectively remove carbon, has a simple structure, is low in cost, and is easy to replace the internal filler. Example 2

[0067] The difference from Example 1 is that a decarbonizer with a different structure is adopted.

[0068] The carbon remover is provided with a filter element consisting of a first-stage wire mesh demister, a second-stage microfiltration dust removal filter element and a third-stage high-efficiency liquid removal filter element, performing a three-stage separation and filtration process;

[0069] The gas containing oil, dirt and solid particles enters from the inlet at the bottom of the decarbonizer, first passes through the first-stage wire mesh demister to separate large liquid droplets in the gas, then passes through the second-stage microfiltration dust removal filter element in an outside-in and inside-out manner to intercept solid particle impurities carried in the gas, and then passes through the third-stage high-efficiency liquid removal filter element in an inside-out manner to remove small droplets, thereby obtaining clean and dry gas.

[0070] As an optimization, the filter element can be detachably mounted inside the housing of the decarbonizer, for example, hung on the top of the housing of the decarbonizer, or detachably mounted inside the housing of the decarbonizer through a threaded structure or a snap.

[0071] The carbon remover effectively removes crystalline carbon formed during the reaction, preventing it from affecting catalyst performance and reducing product yield. It also prevents particulate carbon from entering other components of the system with the circulating gas, potentially blocking them and affecting system stability. Furthermore, the filter element is easy to install and replace, making it convenient and efficient.

[0072] The catalyst service life of this morpholine production system was extended by an average of 8 months, the product yield increased by an average of 5%, the probability of production system failure was lower, and the product purity increased by 1.8%. Example 3

[0073] The difference from Example 1 is that the Figure 3-6 A decarbonizer of the structure shown.

[0074] like Figure 3 The decarbonizer includes a tank body 20', a support 14' for supporting the tank body 20', an upper head 3' arranged at one end of the tank body 20' and a lower head 8' at the other end of the tank body 20', the tank body 20' is provided with a process gas inlet 12', an oil discharge port 5' and a process gas outlet 1', a primary filter device and a filter assembly are provided in the tank body 20', the primary filter device is flatly installed on the inner wall of the tank body 20 above the process gas inlet 12', the filter assembly includes a secondary filter device, a hanging filter assembly, a secondary ... Box 19' and a three-stage filtering device, one end of the hanging box 19' is connected to the secondary filtering device, and the other end of the hanging box 19' is connected to the three-stage filtering device. The hanging box 19' can provide process gas circulation, and the filtering assembly is at least one group. The hanging box 19' is installed on the tray 13', and the tray 13' is installed on the inner wall of the tank body 20'. The tray 13' is provided with a downwardly recessed oil groove 32' on the side close to the wall of the tank body 20', and the oil groove 32' is connected to the oil drain port 5' installed on the outer surface of the tank body.

[0075] The first-level separation area is between the lower head 8' and the first-level filtering device, the second-level separation area is between the first-level filtering device and the tray 13', and the third-level separation area is between the tray 13' and the upper head 3'. A hanging box 19' is provided on the tray 13' for process gas circulation. One end of the hanging box 19' is connected to the second-level filtering device, and the other end of the hanging box 19' is connected to the third-level filtering device.

[0076] like Figure 6The primary filtration device is a wire mesh demister 6', which is supported on the tank body 20' by a bracket 34' and equipped with a pressure plate 33' for compacting the wire mesh demister 6'. When process gas enters the decarbonizer through the process gas inlet 12', the process gas containing oil, fine catalyst powder, and crystallized impurities passes through the wire mesh demister 6', effectively separating larger particles from the gas and discharging them through the drain port 10', achieving primary filtration of the process gas.

[0077] The secondary filtration device is a microfiltration filter 17', which is installed on the hanging box 19' in a hanging manner. After the process gas passes through the wire mesh demister 6', the gas passes through the microfiltration filter 17' in an external-in and internal-out manner, intercepting tiny catalyst powder and crystal impurities carried in the gas, achieving a secondary separation of the process gas. The filtration efficiency of the microfiltration filter 17' is 99.7%.

[0078] like Figure 4 As shown, the microfiltration filter 17' comprises an upper end cap 24', a lower end cap 21', a support tube 23', an oil-resistant seal 25', and a filter element 22'. The filter element 22' is a double-layer structure with the support tube 23' at its center. The filter element 22' is constructed of stainless steel fiber sintered felt, with the fibers sintered together at their contact points for a secure and foldable structure. Its gradient pore size design represents a fixed, irregular-pore deep-layer filter medium, eliminating media migration and impact unloading, thus preventing secondary contamination.

[0079] The microfiltration filter upper head 24' and the microfiltration filter lower head 21' are connected through a microfiltration filter element 22'. The microfiltration filter element 22' is a double-layer structure. A microfiltration filter support tube 23' is provided in the double-layer structure of the microfiltration filter element 22'. The microfiltration filter upper head 24' is provided with a microfiltration filter oil-proof sealing ring 25'.

[0080] The stainless steel fiber felt is made of micron-level ultrafine fibers, boasting a high porosity (up to 90%) and excellent air permeability. The porosity and air permeability are 2-3 times and 30-100 times greater than those of sintered powder materials, respectively. This filter element boasts extremely low fluid resistance and high filtration precision. Its unique three-dimensional, multi-layered, deep filtration structure allows for a high contaminant capacity, 3-5 times greater than that of sintered powder materials. The folded filter area is 3-4 times greater than that of a cylindrical filter, extending its service life by 10-20 times. Sintered stainless steel fiber felt exhibits exceptional mechanical strength and toughness at high temperatures, enabling operation in both high and low temperatures and corrosive environments. The filter element can be cleaned, regenerated, and reused repeatedly.

[0081] In this embodiment, the microfiltration filter element 22' is made of stainless steel fiber sintered felt in a cylindrical shape and fully welded, which provides high strength and good sealing performance, and can withstand a pressure difference ΔP ≥ 0.5 MPa. Of course, the microfiltration filter element 22' can also be made into a folded cylindrical structure to achieve the same separation effect.

[0082] The three-stage filtration device is an ultrafiltration filter 18', which is installed in an inverted manner on the hanging box 19'. The microfiltration filter 17' and the ultrafiltration filter 18' correspond one to one. After the process gas completes the secondary separation, it directly enters the ultrafiltration filter 18' for tertiary separation. The gas passes through the ultrafiltration filter 18' in an inward-outward manner to remove tiny droplets, ultimately achieving a liquid removal efficiency of more than 99.99%.

[0083] like Figure 5 As shown, the ultrafiltration filter 18' includes an ultrafiltration filter element connector 26', an ultrafiltration filter sealing ring 27', an ultrafiltration filter rod 28', an ultrafiltration filter element 29', an ultrafiltration filter rod sealing ring 30' and an ultrafiltration filter nut 31', one end of the ultrafiltration filter rod 28' and the ultrafiltration filter element connector 26' are installed on the upper head of the ultrafiltration filter through the ultrafiltration filter sealing ring 27', and the other end of the ultrafiltration filter rod 28' is installed on the lower head of the ultrafiltration filter through the ultrafiltration filter nut 31', and the ultrafiltration filter rod 28' can adjust the installation length of the ultrafiltration filter 18', so that the ultrafiltration filter 18' is easy to assemble and disassemble.

[0084] The ultrafiltration filter element 29' adopts three-dimensional ultrafine silicon boron fiber, and performs deep filtration by the combined action of diffusion, interception, collision, bridging, charge adsorption, Brownian motion and other comprehensive mechanisms. Micron and submicron particles are captured by the fiber filaments and condensed on the fiber surface. Due to the huge specific surface area of ​​the separation element and the surface tension of the condensed droplets, a liquid film is quickly formed on the fiber surface. Under the action of gravity, it flows downward along the fiber surface and is collected and discharged.

[0085] The specific separation mechanism of the ultrafiltration filter element 29' can be described by the following steps: 1) small droplets are adsorbed on the medium fibers; 2) small droplets are transferred to the fiber intersection through the main flow; 3) two small droplets coalesce into a larger droplet; 4) the process of small droplets coalescing into large droplets is repeated at the fiber intersection; 5) due to the gradually increasing pulling force of the main flow on the droplets, the droplets detach from the medium intersection; 6) steps 1 to 5 are repeated, the droplets gradually become larger, and the medium porosity also gradually increases.

[0086] like Figure 3As shown, a downwardly recessed oil groove 32' is provided on one side of the tray 13' close to the wall of the tank body 20'. The oil groove 32' is connected to the oil drain pipe 5'. When the process gas enters the three-stage filtration device, large droplets collected on the ultrafiltration filter 18' drip downward onto the tray 13' due to gravity. The oil droplets on the tray 13' gather and eventually flow into the recessed oil groove 32', and are finally discharged through the oil drain pipe 5', thereby achieving the effect of removing the oil components in the process gas.

[0087] In addition, the secondary separation area of ​​the tank body 20' is provided with a hot water inlet 11'. As needed, when the wire mesh demister 6' and the microfiltration filter element 22' need to be regenerated, hot water can be poured into the tank body 20' through the hot water inlet 11' to achieve the regeneration of the wire mesh demister 6' and the microfiltration filter element 22'.

[0088] The three-stage separation area of ​​the tank body 20' is provided with a container flange 4'. When the equipment is repaired or the filter element is replaced, the container flange 4' needs to be opened to complete the corresponding equipment maintenance or filter element replacement.

[0089] The catalyst service life of this morpholine production system has been extended by an average of 10 months, the product yield has increased by an average of 10%, the probability of production system failure has been lowered, and the product purity has been increased by 5%. Example 4

[0090] The difference from Example 1 is that no intermediate tank is provided.

[0091] The continuous production cycle of this production system is shortened by an average of 3-5 months, electricity consumption increases by an average of 35%, and annual production capacity decreases by 20%. Example 5

[0092] The difference from Example 1 is that the filling conditions of the adsorbent layer 5 in the pressure swing adsorption tower are different, as follows:

[0093] Based on the total mass of the adsorbent layers being 100%, the loading amount of the activated carbon layer is 35%, the loading amount of the molecular sieve layer is 60%, and the loading amount of the alumina layer is 5%.

[0094] The hydrogen recovery rate during operation of the morpholine production system decreased by 7% compared with that in Example 1, and the purity of the morpholine product decreased by 2.5%. Example 6

[0095] The difference from Example 1 is that the liquid level control of the intermediate tank and the control of relevant parameters of the deamination tower are different from those in Example 1, as follows:

[0096] When the liquid level of the intermediate tank reaches 1 / 2 and the pressure is 1.7 MPa, the cooling water of the condenser of the deamination tower is kept in a circulating state, and the material is discharged from the synthesis intermediate tank to the deamination tower, and then heated at a heating rate of 45°C / hour. The circulation amount of the cooling water is adjusted to control the top pressure of the deamination tower to 1.6 MPa, and then the ammonia production amount is adjusted according to the top temperature of the deamination tower, and the top temperature of the deamination tower is adjusted to 30°C and the bottom temperature of the deamination tower is adjusted to 245°C, and the bottom liquid level of the deamination tower is adjusted to maintain at 60% of the deamination tower capacity.

[0097] The continuous production cycle of this production system was shortened by an average of 3 months, electricity consumption increased by an average of 24%, and annual production capacity decreased by 18%.

[0098] Obviously, the above embodiments are merely examples for clarity of explanation and are not intended to limit the implementation methods. Those skilled in the art will readily appreciate that other variations or modifications based on the above descriptions are possible. It is not necessary and impossible to enumerate all implementation methods here. Obvious variations or modifications arising therefrom remain within the scope of protection of the present invention.

Claims

1. A morpholine production system, comprising a reactor and a diethylene glycol vaporizer, an ammonia vaporizer and a hydrogen supply unit connected to the reactor, wherein the product outlet of the reactor is sequentially connected to a heat exchanger, a condenser and a gas-liquid separator, characterized in that: The hydrogen supply unit includes an ammonia scrubbing tower, a pressure swing adsorption tower and a circulating fan; The liquid outlet of the gas-liquid separator is connected to the crude morpholine processing unit, the tail gas outlet of the gas-liquid separator is connected to the ammonia washing tower, the outlet of the ammonia washing tower and the off-site hydrogen device are connected to the pressure swing adsorption tower, and the purified gas outlet of the pressure swing adsorption tower, the hydrogen outlet of the gas-liquid separator and the outlet of the ammonia vaporizer are connected to the reactor after passing through the heat exchanger, the heating device and the diethylene glycol vaporizer in sequence; A decarbonizer is provided on the connecting pipelines connecting the purified gas outlet of the pressure swing adsorption tower, the hydrogen outlet of the gas-liquid separator, and the outlet of the ammonia vaporizer to the heat exchanger; the decarbonizer is provided with a filter element consisting of a first-stage wire mesh demister, a second-stage microfiltration dust removal filter element, and a third-stage high-efficiency liquid removal filter element, performing a three-stage separation and filtration process; the gas containing oil and solid particles enters through the lower inlet of the decarbonizer, first passes through the first-stage wire mesh demister to separate large droplets in the gas, then passes through the second-stage microfiltration dust removal filter element in an external-in and internal-out manner to intercept solid particle impurities carried in the gas, and then passes through the third-stage high-efficiency liquid removal filter element in an internal-in and external manner to remove small droplets, thereby obtaining clean and dry gas; The pressure swing adsorption tower has an inlet at the lower part of the cylinder and a purified gas outlet at the upper part, and the interior of the cylinder is provided with a first porcelain ball layer, a first wire mesh layer, an adsorbent layer, a second wire mesh layer and a second porcelain ball layer from top to bottom between the purified gas outlet and the inlet; the adsorbent layer is composed of an activated carbon layer, a molecular sieve layer and an alumina layer from bottom to top; The crude morpholine processing unit includes a deamination tower, a dehydration tower, a light component removal tower and a product tower connected in sequence. The liquid outlet of the gas-liquid separator is connected to the deamination tower, and the liquid ammonia outlet of the deamination tower is connected to the ammonia vaporizer; the liquid outlet of the deamination tower is connected to the dehydration tower, and the top of the dehydration tower is provided with an outlet for outputting impurities including water, N-methylmorpholine and N-ethylmorpholine. The bottom outlet of the dehydration tower is connected to the light component removal tower. The light component removal tower is provided with an outlet for outputting water and ethylene glycol monomethyl ether. The bottom of the light component removal tower is connected to the product tower. The top of the product tower is provided with a morpholine product outlet, and the bottom outlet of the product tower is connected to a high-boiling-point storage tank.

2. The morpholine production system according to claim 1, wherein A circulating fan I is provided on the pipeline connecting the purified gas outlet of the pressure swing adsorption tower to the decarbonizer, and a circulating fan II is provided on the pipeline connecting the hydrogen outlet of the gas-liquid separator to the decarbonizer.

3. The morpholine production system according to claim 1, wherein The off-site hydrogen device is a hydrogen output device of the off-site synthetic ammonia system; the desorption gas vent of the pressure swing adsorption tower is connected to the flare.

4. The morpholine production system according to claim 1, wherein A synthesis intermediate tank for temporarily storing crude morpholine is provided between the liquid outlet of the gas-liquid separator and the deamination tower.

5. The morpholine production system according to claim 4, wherein When the liquid level of the intermediate tank reaches 1 / 2~2 / 3 of the tank capacity and the pressure is 0.6~1.5MPa, the cooling water of the condenser of the deamination tower is kept in a circulating state, and the material is discharged from the synthesis intermediate tank to the deamination tower, and then heated at a rate of 30~80℃ / hour. The circulation volume of the cooling water is adjusted to control the top pressure of the deamination tower to 0.8~1.8Mpa, and then the ammonia production amount is adjusted according to the top temperature of the deamination tower, and the bottom temperature of the deamination tower is adjusted to 160~240℃.

6. The morpholine production system according to claim 4, wherein The bottom liquid level of the deamination tower is adjusted to maintain at 65-92% of the deamination tower capacity.

7. The morpholine production system according to claim 4, wherein The deamination tower controls the top temperature to be 30-35° C. and the pressure to be 0.8-1.8 MPa by adjusting the ammonia production rate.

8. The morpholine production system according to claim 1, wherein The first wire mesh layer is fixed below the bed limiting structure provided on the inner wall of the cylinder. The first porcelain ball layer is provided with porcelain balls of φ15-25 mm, and the second porcelain ball layer is provided with porcelain balls of φ2-5 mm.

9. The morpholine production system according to claim 8, wherein Based on the total mass of the adsorbent layers being 100%, the loading amount of the activated carbon layer is 25-32%, the loading amount of the molecular sieve layer is 65-72%, and the loading amount of the alumina layer is 1-3%.

10. The morpholine production system according to claim 1 or 2, characterized in that, The interior of the decarbonizer includes a cylindrical metal material filter layer and a cylindrical filter paper filter layer which are concentrically arranged from the inside to the outside; the cylindrical metal material filter layer is made of one or more of stainless steel mesh, sintered mesh or sintered felt.

11. The morpholine production system according to claim 1 or 2, characterized in that, The filter element is detachably mounted in the housing of the carbon remover.

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