CN111116548A - Inferior sulfolane regeneration equipment, system and method - Google Patents

Inferior sulfolane regeneration equipment, system and method Download PDF

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Publication number
CN111116548A
CN111116548A CN201811277820.XA CN201811277820A CN111116548A CN 111116548 A CN111116548 A CN 111116548A CN 201811277820 A CN201811277820 A CN 201811277820A CN 111116548 A CN111116548 A CN 111116548A
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exchange resin
sulfolane
pipe
regeneration
inferior
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CN111116548B (en
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唐晓津
侯栓弟
刘铮
杨玉蕊
胡立峰
朱振兴
毛俊义
许育鹏
褚小立
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D333/00—Heterocyclic compounds containing five-membered rings having one sulfur atom as the only ring hetero atom
    • C07D333/02—Heterocyclic compounds containing five-membered rings having one sulfur atom as the only ring hetero atom not condensed with other rings
    • C07D333/46—Heterocyclic compounds containing five-membered rings having one sulfur atom as the only ring hetero atom not condensed with other rings substituted on the ring sulfur atom
    • C07D333/48—Heterocyclic compounds containing five-membered rings having one sulfur atom as the only ring hetero atom not condensed with other rings substituted on the ring sulfur atom by oxygen atoms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J41/00—Anion exchange; Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
    • B01J41/04—Processes using organic exchangers
    • B01J41/07—Processes using organic exchangers in the weakly basic form
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J41/00—Anion exchange; Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
    • B01J41/08—Use of material as anion exchangers; Treatment of material for improving the anion exchange properties
    • B01J41/12—Macromolecular compounds
    • B01J41/14—Macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J47/00—Ion-exchange processes in general; Apparatus therefor
    • B01J47/02—Column or bed processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
    • B01J49/05—Regeneration or reactivation of ion-exchangers; Apparatus therefor of fixed beds
    • B01J49/07—Regeneration or reactivation of ion-exchangers; Apparatus therefor of fixed beds containing anionic exchangers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
    • B01J49/60—Cleaning or rinsing ion-exchange beds

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Abstract

一种劣质环丁砜再生的设备、系统和方法，所述的劣质环丁砜再生设备为立式筒体结构，筒体(1)内从上到下设置上分布器(7)、上隔栅(5)、离子交换树脂床层(4)、下隔栅(6)和下分布器(8)；其中所述的上分布器(7)与入口管(2)连通，所述的下分布器(8)与出口管(3)相通，所述的反应器筒体顶部设置排气口(9)，所述的离子交换树脂床层(4)设置于下隔栅(6)上，所述上隔栅(5)底部设有支脚组件(10)。本发明提供的劣化环丁砜再生设备和方法通过阴离子交换树脂去除劣质环丁砜中的酸性物质，使劣质环丁砜恢复到新鲜状态。能够防止设备内上隔栅及上分布器堵塞变形，延长装置运行时间。

Figure 201811277820

A device, system and method for regenerating inferior sulfolane, wherein the inferior sulfolane regeneration device is a vertical cylinder structure, and an upper distributor (7) and an upper grille (5) are arranged in the cylinder (1) from top to bottom. , ion exchange resin bed (4), lower grille (6) and lower distributor (8); wherein the upper distributor (7) is communicated with the inlet pipe (2), and the lower distributor (8) ) is communicated with the outlet pipe (3), the top of the reactor barrel is provided with an exhaust port (9), the ion exchange resin bed (4) is arranged on the lower grid (6), and the upper The bottom of the grid (5) is provided with a support foot assembly (10). The degraded sulfolane regeneration equipment and method provided by the present invention remove the acidic substances in the inferior sulfolane through an anion exchange resin, so that the inferior sulfolane is restored to a fresh state. It can prevent the upper grille and the upper distributor in the equipment from being blocked and deformed, and prolong the operation time of the device.

Figure 201811277820

Description

Inferior sulfolane regeneration equipment, system and method
Technical Field
The present invention relates to an apparatus, system and method for regenerating poor quality sulfolane, and more particularly, to a liquid-solid contact apparatus and method suitable for removing acidic species from poor quality sulfolane via anion exchange resins.
Background
Sulfolane is an important aromatic hydrocarbon extracting agent and is widely used in aromatic hydrocarbon extracting devices. However, in industrial application, sulfolane is degraded, acidic substances generated by degradation and chlorine in an aromatic extraction raw material are enriched in a sulfolane solvent, and the acidic substances and chlorine generated by poor sulfolane can cause the pH value of the sulfolane to be continuously reduced and the color of the sulfolane to be dark. The generation of acidic substances and chlorine also causes serious problems of corrosion of equipment, and therefore the regeneration of inferior sulfolane is very critical.
CN1230545A discloses a regeneration method of inferior sulfolane, which is characterized in that sulfolane passes through an anion exchange resin layer at a flow rate of 1.0-5.0 m/h at a temperature of 25-40 ℃, and macroporous weak-base anion exchange resin is selected, so that the inferior sulfolane can be recovered to the level of fresh materials, the pH value can be recovered to 7.5-10.0, and the color is changed from dark brown to light color or even colorless.
CN103240132B discloses sulfolane regenerating unit of being inferior, for vertical tube structure, including upper portion feed inlet and lower part discharge gate, the feed inlet is equipped with the distributor, and the discharge gate is equipped with down the distributor, is equipped with the silk screen distributor in the barrel, can fix ion exchange resin's relative position. Impurities in the inferior sulfolane can be removed through the device, and the regeneration of the sulfolane is realized.
Disclosure of Invention
The invention aims to solve the technical problem of providing equipment, a system and a method suitable for regenerating poor-quality sulfolane on the basis of the prior art.
The inferior sulfolane regeneration equipment provided by the invention is of a vertical cylinder structure, and an upper distributor 7, an upper barrier 5, an ion exchange resin bed layer 4, an auxiliary pipe branch pipe 14, a lower barrier 6 and a lower distributor 8 are arranged in a cylinder 1 from top to bottom; the upper distributor 7 is communicated with the inlet pipe 2, the lower distributor 8 is communicated with the outlet pipe 3, the top of the reactor cylinder body is provided with an exhaust port 9, the ion exchange resin bed layer 4 is arranged on the lower barrier 6, one end of the branch pipe of the auxiliary pipe is communicated with the auxiliary pipe outside the cylinder body, the other end of the branch pipe of the auxiliary pipe is opened in the ion exchange resin bed layer, and the bottom of the upper barrier 5 is provided with a support leg component 10.
The inferior sulfolane regeneration system provided by the invention adopts at least two pieces of inferior sulfolane regeneration equipment connected in parallel, and the ion exchange resin bed layer is filled with alkaline anion exchange resin.
The inferior sulfolane regeneration method provided by the invention adopts the inferior sulfolane regeneration system, the inferior sulfolane fluid enters inferior sulfolane regeneration equipment from an inlet pipe, is distributed by an upper distributor, then uniformly distributed into an alkaline anion exchange resin bed layer through an upper grid and flows downwards, impurities in the inferior sulfolane are removed by the action of the anion exchange resin, and the regenerated sulfolane fluid is discharged from the regeneration equipment through an outlet pipe after passing through a lower grid and being collected by a lower distributor.
The inferior sulfolane regeneration equipment, the system and the method provided by the invention have the beneficial effects that:
the upper distributor and the upper barrier of the inferior sulfolane regeneration equipment provided by the invention can uniformly distribute the inferior sulfolane fluid entering the regeneration equipment, and avoid deformation, impact and crushing of an ion exchange resin bed layer caused by uneven fluid distribution. The lower distributor can uniformly collect the regenerated sulfolane fluid, and unnecessary fluid back mixing is avoided. The ion exchange resin bed layer is arranged between the upper grid and the lower grid, so that the positions of the resin particles are relatively fixed, the implementation of a regeneration process is ensured, and meanwhile, the resin particles can be prevented from blocking the open pores of the distributor or deforming and damaging the distributor caused by the resin particles. The support leg group at the lower part of the upper barrier can avoid the impact of the abnormal expansion of the ion exchange resin bed layer caused by the flow of fluid from bottom to top on the barrier equipment in the regeneration process of the ion exchange resin and can also avoid the blockage of the upper distributor caused by the part of fine particles passing through the upper barrier.
Drawings
FIG. 1 is a schematic view of the inferior sulfolane regeneration apparatus according to the present invention;
FIG. 2 is a schematic view of a distributor structure of an inferior sulfolane regeneration apparatus according to the present invention;
fig. 3 is a schematic structural view of the leg assembly.
Wherein:
1-a cylinder body; 2-an inlet tube; 3-an outlet pipe;
4-ion exchange resin bed layer; 5-upper barrier; 6-lower barrier;
7-upper distributor; 8-a lower distributor; 9-exhaust port;
10-a foot assembly; 13-an auxiliary tube; 14-auxiliary pipe branch;
11-a connecting tube; 12-a loop pipe; 15-a vertical pipe;
16-a central tube; 17-needle manifold.
Detailed Description
The inferior sulfolane regeneration device, the system and the method are implemented as follows:
an inferior sulfolane regeneration device is of a vertical cylinder structure, wherein an upper distributor 7, an upper barrier 5, an ion exchange resin bed layer 4, an auxiliary pipe branch pipe 14, a lower barrier 6 and a lower distributor 8 are arranged in a cylinder 1 from top to bottom; the upper distributor 7 is communicated with the inlet pipe 2, the lower distributor 8 is communicated with the outlet pipe 3, the top of the reactor cylinder body is provided with an exhaust port 9, the ion exchange resin bed layer 4 is arranged on the lower barrier 6, one end of the branch pipe of the auxiliary pipe is communicated with the auxiliary pipe outside the cylinder body, the other end of the branch pipe of the auxiliary pipe is opened in the ion exchange resin bed layer, and the bottom of the upper barrier 5 is provided with a support leg component 10.
Preferably, an ion exchange resin bed layer is arranged between the upper grid and the lower grid, and the upper grid and the lower grid are both wire meshes, sieve plates or flat plates with slit structures.
Preferably, the height of the ion exchange resin bed layer is 50-90% of the height of the cylinder body, and the lower grid 6 is arranged at 5-20% of the cylinder body 1 from bottom to top.
Preferably, the upper distributor 7 and the lower distributor 8 each comprise a central tube 16, a connecting tube 11 and a loop 12, the central tube 16 is communicated with the loop 12 through the connecting tube 11, and the loop 12 has an opening. Preferably the diameter of the openings is 0.1-0.5 mm.
Preferably, the support leg assembly comprises a vertical tube and a plurality of needle-shaped branch tubes connected with the bottom of the vertical tube, and the vertical tube is fixedly connected with the upper barrier. More preferably, the leg assembly is composed of a vertical tube and three needle-shaped branch tubes connected to the bottom of the vertical tube, and the angle between the branch tubes and the vertical tube is 30-75 deg. The height of the supporting leg component is 10-200mm, and the bottom of the supporting leg component is 50-300mm higher than the top of the anion exchange resin bed layer.
An inferior sulfolane regeneration system adopts at least two pieces of inferior sulfolane regeneration equipment connected in parallel, and alkaline anion exchange resin is arranged in an ion exchange resin bed layer.
Preferably, the basic anion exchange resin is macroporous weak base styrene resin, and the diameter of the resin is 0.2-1.5 mm
Preferably, the height of the ion exchange resin bed layer is 60-90% of the height of the cylinder body, and the bottom of the leg component is 50-300mm higher than the top of the ion exchange resin bed layer.
The inferior sulfolane regeneration method adopts the inferior sulfolane regeneration system, inferior sulfolane material liquid enters regeneration equipment from an inlet pipe, is distributed by an upper distributor, then passes through an upper grid to be uniformly distributed in an alkaline anion exchange resin bed layer and flows downwards, impurities in the inferior sulfolane material liquid are removed under the action of anion exchange resin, and the regenerated sulfolane material liquid passes through a lower grid and is collected by a lower distributor and then is discharged out of the regeneration equipment from an outlet pipe.
In the continuous operation process, the regeneration method of the inferior sulfolane also comprises the regeneration step after the inactivation of the anion exchange resin:
(1) stopping introducing and emptying the poor-quality sulfolane fluid, introducing deionized water into the poor-quality sulfolane regeneration equipment, and soaking the ion exchange resin for 8-15 hours;
(2) using 1-5 times volume of dilute alkali solution to pass through anion exchange resin bed layer to convert it into hydroxyl type;
(3) washing the alkali liquor adsorbed in the resin bed layer by using deionized water, and then purging and drying inferior sulfolane regeneration equipment by using nitrogen;
(4) poor-quality sulfolane feed liquid is led in through the outlet pipe and the auxiliary pipe respectively, flows from bottom to top and is filled in the poor-quality sulfolane regeneration equipment, air is exhausted through the exhaust port, then the feeding of the outlet pipe 3 and the auxiliary pipe 13 is cut off, and the feeding of the inlet pipe 2 is switched to the regeneration operation of the poor-quality sulfolane. Preferably, the apparent flow velocity of the inferior sulfolane fluid in the regeneration equipment is 1.0-6.0 m/h, and the operation temperature is 25-40 ℃.
In the inferior sulfolane regeneration equipment provided by the invention, the exhaust port is positioned at the top of the cylinder body of the inferior sulfolane regeneration equipment, and the top of the cylinder body refers to the position from bottom to top of 95-100% of the height of the cylinder body. The device is used for discharging gas in the reactor during the start-up process.
An ion exchange resin bed layer is arranged between the upper barrier and the lower barrier, and the upper barrier and the lower barrier are both wire meshes, sieve plates or flat plates with slit structures. Preferably, the lower grid adopts a slotted structure.
The circular pipe of the upper distributor and the circular pipe of the lower distributor have an open pore structure, the open pore form can be a strip seam or a small pore, preferably, the width of the strip seam is 0.1-0.5mm, and the diameter of the small pore is 0.1-0.5 mm.
The upper distributor is used for uniformly distributing the feeding fluid, and the lower distributor is used for uniformly collecting the fluid to be discharged, namely the fluid flows from top to bottom in the regeneration process of poor sulfolane, so that the floating state of resin particles due to low density can be avoided, and the abrasion and the breakage of the resin particles are reduced.
The anion exchange resin is selected from macroporous basic anion exchange resin, preferably macroporous weak basic anion exchange resin, more preferably macroporous weak basic styrene resin, such as weak basic macroporous styrene-NH2Form or-N (CH)3) A resin. The diameter of the selected resin particles is 0.2-1.5 mm, preferably 0.4-1.2 mm.
When the deteriorated sulfolane regeneration reactor provided by the invention is used, poor sulfolane fluid enters the reactor from the inlet pipe and is uniformly distributed in the reactor through the upper distributor. The fluid then flows down the upper grid into the bed of anion exchange resin and interacts with the resin to remove the acidic species and chlorine from the inferior sulfolane. The sulfolane fluid leaving the anion exchange resin bed passes through the lower grid, is collected by the lower distributor and finally exits the reactor through the outlet pipe. Through the regeneration process, the sulfolane is gradually recovered to the level of a fresh material, the pH value is recovered to 7.5-10, and the color is recovered to a light color or colorless.
After the equipment for regenerating the deteriorated sulfolane provided by the invention is operated for a period of time, the regeneration of the anion exchange resin is required. Firstly, deionized water is led into degraded sulfolane regeneration equipment, and the ion exchange resin is soaked in the ionic water for 8-15 hours. Then using 1-5 times of dilute alkali solution of resin volume to pass through the degraded sulfolane regeneration equipment to convert the resin into hydroxyl type. The resin was then rinsed with deionized water until the eluate pH was between 7.0 and 8.0. And then purging the deteriorated sulfolane regeneration equipment with nitrogen for drying. After the drying is finished, poor-quality sulfolane feed liquid is respectively led in through the outlet pipe and the auxiliary pipe, so that the feed liquid in the degraded sulfolane regeneration equipment moves from bottom to top, the equipment is filled with the liquid feed liquid, then the feed of the outlet pipe and the auxiliary pipe is cut off, the feed liquid is led in through the inlet pipe, and the flow mode of the degraded sulfolane feed liquid is changed into a mode from top to bottom to carry out the regeneration operation of the degraded sulfolane. In the flowing process of the degraded sulfolane liquid from bottom to top, nitrogen in equipment can be exhausted through the exhaust port, and the device can also have a certain loosening effect on the bed layer of the anion exchange resin so as to avoid the reduction of the operation capacity of the equipment caused by overhigh pressure drop of the bed layer. In the flowing process of the degraded sulfolane liquid from bottom to top, the expansion of an anion exchange resin bed layer can be caused, usually, part of the bed layer can rapidly move upwards to reach the position of the upper grid to cause the blockage and the impact of the upper grid, so that the abrasion of particles is aggravated, and the grown part of fine particles flow upwards along with the fluid to cause the blockage of the upper distributor. The occurrence of the above phenomenon can be effectively avoided through the support leg group, the auxiliary pipe and the auxiliary pipe branch pipe. Firstly, the vertical pipe of the support leg component and the needle-shaped support legs thereof prevent the over-expanded resin bed layer from approaching the upper barrier to cause the blockage, and can play a role of disturbance, so that the over-expanded resin bed layer is converted into a bulk fluidization state from a denser packing state. Secondly, poor-quality sulfolane liquid is led in through an outlet pipe and an auxiliary pipe respectively, so that the sulfolane liquid can enter an anion exchange resin bed layer in a distributed feeding mode, loosening of liquid flowing upwards is guaranteed at different heights of the bed layer, uniform loosening of the bed layer is achieved, excessive expansion of the bed layer, particularly a high-position bed layer, caused by impact of large-flow liquid is avoided, part of the bed layer still in a close-packed state moves upwards rapidly, impact is caused on an upper barrier, and the barrier and an upper distributor are blocked. Thirdly, the feeding mode of uniform and loose bed layer avoids the generation of fine particles due to particle abrasion, and inhibits the blockage of the fine particles to the barrier and the distributor.
The present invention is not limited to the details of the embodiments described above, and various simple modifications can be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are included in the protection scope of the present invention.
Fig. 1 is a schematic structural view of the inferior sulfolane regeneration equipment provided by the invention, as shown in fig. 1, the inferior sulfolane regeneration equipment is of a cylinder structure, and an upper distributor 7, an upper barrier 5, an ion exchange resin bed layer 4, an auxiliary branch pipe 14, a lower barrier 6 and a lower distributor 8 are arranged in the cylinder 1 from top to bottom; the upper distributor 7 is communicated with the inlet pipe 2, the lower distributor 8 is communicated with the outlet pipe 3, the top of the reactor barrel is provided with an exhaust port 9, the anion exchange resin bed layer 4 is arranged on the lower barrier 6, the bottom of the upper barrier 5 is provided with a support leg assembly 10, 3 auxiliary branch pipes 14 are arranged in the barrel, one end of each auxiliary branch pipe 14 is communicated with an auxiliary branch pipe 13 outside the barrel, and the other end of each auxiliary branch pipe is opened in the ion exchange resin bed layer.
Fig. 2 is a schematic diagram of a distributor structure of inferior sulfolane regeneration equipment according to the present invention, and as shown in fig. 2, each of the upper distributor 7 and the lower distributor 8 includes a central pipe 16, a connecting pipe 11, and a loop pipe 12, the central pipe 16 is communicated with the loop pipe 12 through the connecting pipe 11, and the loop pipe 12 has an opening with a diameter of 0.1-0.5 mm.
Fig. 3 is a schematic structural view of a leg assembly of an inferior sulfolane regeneration apparatus according to the present invention, and as shown in fig. 3, the leg assembly 10 is composed of a vertical pipe 15 and three needle-shaped branch pipes 17 connected to the bottom of the vertical pipe, and the included angle between the needle-shaped branch pipes and the vertical pipe is 30-75 °.
The following examples further illustrate the practice of the invention, but are not intended to limit the invention thereto.
Example 1
The inferior sulfolane regeneration device shown in the attached figure 1 is adopted. The structure of the leg assembly is shown in fig. 3. Wherein, inferior sulfolane regeneration facility's barrel height is 6m, and the internal diameter is 0.5m, and lower retainer is apart from the bottom of the equipment 1.0 m. The height of the ion exchange resin bed layer is 3.5m, the support leg component comprises 56 groups of vertical pipes and needle-shaped branch pipes connected with the bottoms of the vertical pipes, and each vertical pipe and 3 needle-shaped branch pipes. Wherein, the diameter of the vertical pipe is 25mm, and the length is 150 mm; the diameter of the needle-shaped branch pipe is 10mm, and the length of the needle-shaped branch pipe is 40 mm; the included angle between the axis of the needle-shaped branch pipe and the axis of the vertical pipe is 45 degrees; the needle-shaped branch pipes are uniformly distributed on the circumference of the cross section of the bottom end of the vertical pipe. The height of the bottom of the leg assembly from the top of the ion exchange resin bed was 200 mm.
The ion exchange resin adopts macroporous weak base styrene-N (CH) which is commercially available3)2The particle size of the resin particle is 1 mm. The inferior sulfolane is from China petrochemical company, Inc. of China sea division, and contains acidic substances and chlorine with pH of 3.5 and chlorine content of 40ppm (chlorine content is analyzed by heavy oil chlorine content analysis standard method, microcoulomb method).
Filling ion exchange resin into an inferior sulfolane reactor, soaking the reactor for 12 hours by using deionized water, then passing dilute alkali liquor with the volume 3 times that of the resin through the reactor to convert the resin into hydroxyl type, then leaching the resin by using the deionized water until the pH of an eluate is 7.0-8.0, stopping leaching, removing water by using nitrogen, and drying. Poor quality sulfolane was passed through the reactor from top to bottom at a throughput of 2 tons/hour. And (3) measuring the pH value and the chlorine content of the sulfolane at the outlet of the reactor, wherein the sulfolane at the outlet of the reactor is light yellow and transparent, the pH value is more than 8, and the chlorine removal rate is more than or equal to 85% or the chlorine content is less than 5 ppm. When the pH value of sulfolane discharged from the outlet pipe is less than 7.0, the device is switched to the ion exchange resin regeneration state. The running period of the device is 3 months.
Example 2
The inferior sulfolane regeneration device shown in the attached figure 1 is adopted. The structure of the leg assembly is shown in fig. 3. The cylinder height of inferior sulfolane regeneration facility is 6m, and the internal diameter is 0.5m, and lower retainer is 0.6m apart from the bottom of equipment. The height of the ion exchange resin bed layer is 4.0m, the support leg component comprises 28 groups of vertical pipes and needle-shaped branch pipes connected with the bottoms of the vertical pipes, and each vertical pipe and 4 needle-shaped branch pipes. Wherein the diameter of the vertical pipe is 30mm, and the length of the vertical pipe is 100 mm; the diameter of the needle-shaped branch pipe is 15mm, and the length of the needle-shaped branch pipe is 50 mm; the included angle between the axis of the needle-shaped branch pipe and the axis of the vertical pipe is 60 degrees; the needle-shaped branch pipes are uniformly distributed on the circumference of the cross section of the bottom end of the vertical pipe. The height of the bottom of the leg assembly from the top of the ion exchange resin bed was 150 mm.
The ion exchange resin used was the same as in example 1. The inferior sulfolane is from China petrochemical company, Inc., Zhenhai division, and contains acidic substances and chlorine with pH of 4 and chlorine content of 25 ppm.
Filling ion exchange resin into an inferior sulfolane reactor, soaking the reactor for 12 hours by using deionized water, then passing dilute alkali liquor with the volume 3 times that of the resin through the reactor to convert the resin into hydroxyl type, then leaching the resin by using the deionized water until the pH of an eluate is 7.0-8.0, stopping leaching, removing water by using nitrogen, and drying. Inferior sulfolane is passed through the reactor from top to bottom with the treatment capacity of 2 tons/hour, when the difference between the pH value of the outlet sulfolane and the pH value of the inlet sulfolane of the reactor is less than 1, the sulfolane is stopped being introduced, and after the resin is regenerated according to the method, the sulfolane is continuously introduced. The running period of the ion exchange resin single device is 100 days.
Comparative example 1
Inferior sulfolane regeneration equipment in CN103240132B is adopted, the height of the cylinder is 5m, and the inner diameter is 0.5 m. The barrel comprises an upper feeding hole and a lower discharging hole, the feeding hole is provided with an upper distributor, the discharging hole is provided with a lower distributor, a silk screen distributor is arranged in the barrel, and the silk screen distributor fixes the relative position of the ion exchange resin.
The ion exchange resin and poor sulfolane feedstock used were the same as in example 1. Filling ion exchange resin into inferior sulfolane regeneration equipment, soaking the resin in deionized water for 12 hours, then using dilute alkali liquor with the volume of 3 times that of an ion exchange resin bed layer to pass through the ion exchange resin bed layer to convert the resin into an hydroxyl type, then using the deionized water to elute the resin until the pH of an eluate is 7.0-8.0, stopping elution, using nitrogen to remove water, and drying. Poor quality sulfolane was passed through the regenerator from top to bottom at a throughput of 2 tons/hour. And measuring the pH value and the chlorine content of the sulfolane fluid discharged from the outlet pipe of the regeneration equipment, wherein the sulfolane of the outlet pipe is light yellow and transparent, the pH value is more than 8, and the chlorine removal rate is more than or equal to 85% or the chlorine content is less than 5 ppm. The running period of the test device is 1 month, and meanwhile, the upper silk screen distributor is easy to deform in the regeneration process, and the opening of the upper distributor is easy to block.

Claims (13)

1.一种劣质环丁砜再生设备，为立式筒体结构，其特征在于，筒体(1)内从上到下设置上分布器(7)、上隔栅(5)、离子交换树脂床层(4)、辅助管支管(14)、下隔栅(6)和下分布器(8)；其中所述的上分布器(7)与入口管(2)连通，所述的下分布器(8)与出口管(3)相通，所述的反应器筒体顶部设置排气口(9)，所述的离子交换树脂床层(4)设置于下隔栅(6)上，所述的辅助管支管一端与筒体外的辅助管连通，另一端开口于离子交换树脂床层内，所述上隔栅(5)底部设有支脚组件(10)。1. a low-quality sulfolane regeneration equipment, is a vertical cylinder structure, it is characterized in that, in the cylinder (1) from top to bottom, upper distributor (7), upper grille (5), ion exchange resin bed are arranged from top to bottom (4), an auxiliary pipe branch pipe (14), a lower grille (6) and a lower distributor (8); wherein the upper distributor (7) communicates with the inlet pipe (2), and the lower distributor ( 8) communicated with the outlet pipe (3), the top of the reactor barrel is provided with an exhaust port (9), the ion exchange resin bed (4) is provided on the lower grille (6), the One end of the auxiliary pipe branch pipe is communicated with the auxiliary pipe outside the cylinder, and the other end is opened in the ion exchange resin bed, and the bottom of the upper grille (5) is provided with a foot assembly (10). 2.按照权利要求1所述的劣质环丁砜再生设备，其特征在于，所述的上隔栅(5)与下隔栅(6)之间设离子交换树脂床层(4)，所述上隔栅(5)与下隔栅(6)为丝网、筛板或具有条缝结构的平板。2. The inferior sulfolane regeneration device according to claim 1, characterized in that, an ion exchange resin bed (4) is set between the upper grille (5) and the lower grille (6), and the upper partition The grid (5) and the lower grid (6) are wire mesh, sieve plate or flat plate with a slot structure. 3.按照权利要求1所述的劣化环丁砜再生设备，其特征在于，所述的离子交换树脂床层的高度为筒体高度的50-90％，所述的下隔栅(6)的安装设于筒体(1)由下到上的5-20％处。3. The degraded sulfolane regeneration device according to claim 1, wherein the height of the ion exchange resin bed is 50-90% of the height of the cylinder, and the installation of the lower grille (6) At 5-20% of the cylinder (1) from bottom to top. 4.按照权利要求1、2或3所述的劣化环丁砜再生设备，其特征在于，所述的上分布器(7)和下分布器(8)均包括中心管(16)、连接管(11)和环管(12)，中心管(16)与环管(12)通过连接管(11)相通，所述的环管(12)具有开孔，所述开孔的直径为0.1-0.5mm。4. according to the described deterioration sulfolane regeneration equipment of claim 1,2 or 3, it is characterized in that, described upper distributor (7) and lower distributor (8) all comprise central pipe (16), connecting pipe (11) ) and the ring pipe (12), the central pipe (16) and the ring pipe (12) communicate with each other through the connecting pipe (11), the ring pipe (12) has an opening, and the diameter of the opening is 0.1-0.5mm . 5.按照权利要求1、2或3所述的劣质环丁砜再生设备，其特征在于，所支脚组件由竖管和与竖管底部相连的多根针形支管组成，所述的竖管与上隔栅固定连接；所述的支脚组件的高度为10-200mm。5. according to the inferior sulfolane regeneration equipment described in claim 1,2 or 3, it is characterized in that, the leg assembly is made up of a vertical pipe and a plurality of needle-shaped branch pipes that are connected with the bottom of the vertical pipe, and the vertical pipe is connected with the upper partition The grid is fixedly connected; the height of the foot assembly is 10-200mm. 6.按照权利要求2所述的劣质环丁砜再生设备，其特征在于，所述的支脚组件为竖管和与竖管底部连接的三根针形支管组成，所述的支管与竖管夹角为30-75°。6. according to the described inferior sulfolane regeneration equipment of claim 2, it is characterized in that, described leg assembly is that the vertical pipe and the three needle-shaped branch pipes that are connected with the bottom of the vertical pipe are formed, and the included angle of the described branch pipe and the vertical pipe is 30 -75°. 7.一种劣质环丁砜再生系统，其特征在于，采用至少两台并联的权利要求1-6中所述的劣质环丁砜再生设备，在其中的离子交换树脂床层中安装有碱性阴离子交换树脂。7. An inferior sulfolane regeneration system, characterized in that, at least two inferior sulfolane regeneration devices described in claims 1-6 are used in parallel, and basic anion exchange resin is installed in the ion exchange resin bed. 8.按照权利要求7所述的劣质环丁砜再生系统，其特征在于，所述的碱性阴离子交换树脂为大孔弱碱性苯乙烯系树脂，树脂颗粒粒径为0.2～1.5mm。8 . The inferior sulfolane regeneration system according to claim 7 , wherein the basic anion exchange resin is a macroporous weakly basic styrene resin, and the particle size of the resin particles is 0.2-1.5 mm. 9 . 9.按照权利要求7所述的劣质环丁砜再生系统，其特征在于，所述的离子交换树脂床层的高度为筒体高度的60-90％，所述的支脚组件的底部高于离子交换树脂床层的顶部50-300mm。9. The inferior sulfolane regeneration system according to claim 7, wherein the height of the ion exchange resin bed is 60-90% of the height of the cylinder, and the bottom of the support foot assembly is higher than the ion exchange resin The top of the bed is 50-300mm. 10.一种劣质环丁砜再生方法，其特征在于，采用权利要求7-9所述的劣质环丁砜再生系统，劣质环丁砜流体由入口管进入再生设备，经上分布器分布后，再穿过上隔栅均匀分布到碱性阴离子交换树脂床层中并向下流动，劣质环丁砜流体中的杂质与阴离子交换树脂作用而被脱除，再生后的环丁砜流体经过下隔栅，再经下分布器收集后，由出口管排出再生设备。10. an inferior sulfolane regeneration method, is characterized in that, adopts the inferior sulfolane regeneration system described in claim 7-9, inferior sulfolane fluid enters regeneration equipment by inlet pipe, after being distributed through upper distributor, then passes through upper grille It is evenly distributed into the basic anion exchange resin bed and flows downward. The impurities in the inferior sulfolane fluid are removed by the action of the anion exchange resin. The regenerated sulfolane fluid passes through the lower grille and is collected by the lower distributor. The regeneration equipment is discharged from the outlet pipe. 11.按照权利要求10所述的劣质环丁砜再生方法，其特征在于，还包括离子交换树脂失活后的再生步骤：11. according to the inferior sulfolane regeneration method described in claim 10, is characterized in that, also comprises the regeneration step after ion exchange resin deactivation: (1)停止通入并排空劣质环丁砜流体，向劣质环丁砜再生设备中通入去离子水，浸泡离子交换树脂床层8-15小时；(1) stop feeding and emptying the inferior sulfolane fluid, pass deionized water into the inferior sulfolane regeneration equipment, and soak the ion exchange resin bed for 8-15 hours; (2)用1-5倍体积的稀碱溶液通过阴离子交换树脂床层，将其转化为氢氧根型；(2) pass through the anion exchange resin bed with 1-5 times the volume of dilute alkali solution, and convert it into hydroxide form; (3)用去离子水淋洗离子交换树脂床层中吸附的碱液，然后用氮气吹扫并干燥劣质环丁砜再生设备；(3) rinse the lye adsorbed in the ion exchange resin bed with deionized water, then purge and dry the inferior sulfolane regeneration equipment with nitrogen; (4)分别由出口管和辅助管通入劣质环丁砜料液，使其由下至上流动并充满劣质环丁砜再生设备，并经排气口排空气体，而后切断出口管(3)和辅助管(13)的进料，由入口管(2)进料切换到劣质环丁砜的再生操作。(4) Pass the inferior sulfolane feed liquid through the outlet pipe and the auxiliary pipe respectively, make it flow from bottom to top and fill the inferior sulfolane regeneration equipment, and discharge the air through the exhaust port, and then cut off the outlet pipe (3) and the auxiliary pipe ( 13), the feed from the inlet pipe (2) is switched to the regeneration operation of inferior sulfolane. 12.按照权利要求10或11所述的劣质环丁砜再生方法，其特征在于，所述的劣质环丁砜流体在所述再生设备内的表观流速为1.0～6.0m/h，操作温度为25～40℃。12. The method for regenerating inferior sulfolane according to claim 10 or 11, wherein the apparent flow rate of the inferior sulfolane fluid in the regeneration device is 1.0-6.0 m/h, and the operating temperature is 25-40 °C. 13.按照权利要求11所述的劣化环丁砜再生方法，其特征在于，步骤(3)中用去离子水淋洗离子交换树脂床层至洗出液pH在7.0-8.0之间。13. The regeneration method of degraded sulfolane according to claim 11, characterized in that, in step (3), the ion exchange resin bed is rinsed with deionized water until the pH of the eluate is between 7.0-8.0.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115672410A (en) * 2022-11-07 2023-02-03 国家能源集团煤焦化有限责任公司 Regeneration systems and regeneration systems for sulfolane regeneration
CN115739206A (en) * 2022-11-27 2023-03-07 王志国 Ion exchange column

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CN1230545A (en) * 1998-03-26 1999-10-06 中国石油化工总公司 Regeneration Method of Inferior Sulfolane
CN103240132A (en) * 2012-02-10 2013-08-14 苏州艾科水处理设备工程有限公司 Inferior sulfolane regenerator

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CN1230545A (en) * 1998-03-26 1999-10-06 中国石油化工总公司 Regeneration Method of Inferior Sulfolane
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Publication number Priority date Publication date Assignee Title
CN115672410A (en) * 2022-11-07 2023-02-03 国家能源集团煤焦化有限责任公司 Regeneration systems and regeneration systems for sulfolane regeneration
CN115739206A (en) * 2022-11-27 2023-03-07 王志国 Ion exchange column

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