CN110871013A - Method for adsorbing and desorbing benzene in acetylene - Google Patents

Method for adsorbing and desorbing benzene in acetylene Download PDF

Info

Publication number
CN110871013A
CN110871013A CN201811013642.XA CN201811013642A CN110871013A CN 110871013 A CN110871013 A CN 110871013A CN 201811013642 A CN201811013642 A CN 201811013642A CN 110871013 A CN110871013 A CN 110871013A
Authority
CN
China
Prior art keywords
acetylene
benzene
activated carbon
detected out
gas
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201811013642.XA
Other languages
Chinese (zh)
Inventor
何志群
陈仕萍
杨中明
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Chongqing Vico Technology Co Ltd
China Petroleum and Chemical Corp
Sinopec Chongqing Chuanwei Chemical Co Ltd
Original Assignee
Chongqing Vico Technology Co Ltd
China Petroleum and Chemical Corp
Sinopec Chongqing Chuanwei Chemical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Chongqing Vico Technology Co Ltd, China Petroleum and Chemical Corp, Sinopec Chongqing Chuanwei Chemical Co Ltd filed Critical Chongqing Vico Technology Co Ltd
Priority to CN201811013642.XA priority Critical patent/CN110871013A/en
Publication of CN110871013A publication Critical patent/CN110871013A/en
Pending legal-status Critical Current

Links

Images

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2256/00—Main component in the product gas stream after treatment
    • B01D2256/24—Hydrocarbons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/702—Hydrocarbons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/80—Water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/40083—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
    • B01D2259/40088—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention belongs to the technical field of separation of free carbon by chemical or physical change of substances through a method of adsorption, regeneration or reactivation, and particularly relates to a method for adsorbing and desorbing benzene in acetylene, which comprises the following steps: A. placing unpurified acetylene into an adsorption tower filled with activated carbon, and returning the purified acetylene to a vinyl acetate synthesis system; B. activated carbon desorption and regeneration: placing the activated carbon which is saturated in adsorption into a reaction kettle with a jacket for heating for desorption and regeneration, introducing inert gas into the bottom of the reaction kettle to be connected with a gas distributor at the bottom of the reaction kettle, heating the reaction kettle through the jacket, blowing out benzene and water in the activated carbon by the inert gas after the benzene and the water are gasified, and sending the blown gas to a boiler for combustion treatment. The method can remove benzene and saturated water in acetylene, and the activated carbon which is adsorbed to saturation can be regenerated and recycled after treatment.

Description

Method for adsorbing and desorbing benzene in acetylene
Technical Field
The invention belongs to the technical field of separation of substances by chemical or physical changes through a method of adsorbing, regenerating or reactivating free carbon, and particularly relates to a method for adsorbing and desorbing benzene in acetylene.
Background
Vinyl acetate (VAC for short), also known as vinyl acetate, is an important organic chemical raw material, is mainly used for producing derivatives such as polyvinyl acetate (PVAC), polyvinyl alcohol (PVOH), vinyl acetate-ethylene copolymer emulsion (VAE) or copolymer resin (EVA), vinyl acetate-vinyl chloride copolymer (EVC), polyacrylonitrile comonomer, acetal resin, and the like, and is widely used in the fields of coatings, slurries, adhesives, vinylon, films, leather processing, synthetic fibers, soil improvement, and the like ("technical research progress of vinyl acetate synthesis by acetylene method", niee, chemical engineering of acetaldehyde and acetic acid, paragraph 9 in 2015, paragraph 1 in the left column on page 11, and published as 12/31/2015).
The synthesis of vinyl acetate has evolved over decades and currently uses acetylene gas phase and ethylene gas phase for industrial production. From 1960 to 2011, China has 18 sets of VAC production devices, and 15 sets of VAC production devices adopt an acetylene method to prepare vinyl acetate. The abundant reserves of coal resources and natural gas resources produced in China are important reasons why the acetylene method synthesized vinyl acetate is mainstream at home and has market prospect. Acetylene and acetic acid can be catalytically reacted to synthesize vinyl acetate CH ≡ CH + CH3COOH→CH2＝CHOOCCH3(progress of research on catalyst for synthesizing vinyl acetate by acetylene method, Lidonxia et al, coal chemical engineering, volume 38, stage 10 in 2015, page 39, left column, penultimate stage 1, published as 2015, 8 months and 31 days).
Before crude acetylene with purity of about 98.5% produced in acetylene workshops and containing saturated water is sent to a vinyl acetate device to synthesize vinyl acetate, 98 wt% concentrated sulfuric acid is needed to be used for acid cleaning to remove higher Alkyne (AS) (comprising allene, methylacetylene, butadiene, vinyl acetylene, diacetylene and benzene) and saturated water in the crude acetylene, so that the acetylene purity reaches over 99.5%, and simultaneously, a large amount of waste sulfuric acid is generated. The concentration of the waste sulfuric acid absorbing the higher Alkyne (AS) and water is about 83 wt% -85 wt%, the waste sulfuric acid contains 8 wt% -15 wt% of organic matters and carbon impurities and about 2 wt% of water, the density is 1.65-1.75g/ml, the appearance is brown or blackish brown, and the waste sulfuric acid has strong pungent smell and foul smell, thereby bringing great difficulty to the treatment and the utilization.
Disclosure of Invention
In view of the above, the present invention provides a method for adsorbing and desorbing benzene in acetylene. The method can remove benzene and saturated water in acetylene, then remove other impurities through a subsequent separation process, and the activated carbon which is adsorbed to saturation can be regenerated and recycled after treatment to replace or partially replace concentrated sulfuric acid, so that the consumption of the concentrated sulfuric acid is reduced, and the pressure of subsequent treatment and utilization is relieved.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the method for adsorbing and desorbing benzene in acetylene comprises the following steps:
A. feeding unpurified acetylene into an adsorption tower filled with activated carbon, and returning the purified acetylene to a vinyl acetate synthesis system;
B. activated carbon desorption and regeneration: placing the activated carbon which is saturated in adsorption into a reaction kettle with a jacket for heating for desorption and regeneration, introducing inert gas into the bottom of the reaction kettle to be connected with a gas distributor at the bottom of the reaction kettle, heating the reaction kettle through the jacket, and blowing out gas to be sent to a boiler for combustion treatment.
The bottom is a clear concept for a person skilled in the art.
The inert gas refers to nitrogen, helium, neon, argon, krypton, xenon and the like.
The method can remove benzene and saturated water in acetylene, and the activated carbon with saturated adsorption can be regenerated and recycled after treatment, so as to replace or partially replace concentrated sulfuric acid, reduce the consumption of concentrated sulfuric acid, and relieve the pressure of subsequent treatment and utilization
Further, the space velocity of acetylene is 129--1。
Further, the inert gas space velocity is 114--1。
Further, the jacket heating temperature in step B was 120-150 ℃.
Further, the benzene content in the acetylene at the outlet of the adsorption tower and the benzene content in the blown-out gas are measured by adopting a gas chromatography, and the water content in the purified acetylene is measured by adopting a dew point measuring instrument.
The invention has the beneficial effects that:
the method of the invention treats crude acetylene, the benzene content in the purified acetylene is lower than 1ppm, and the activated carbon which is adsorbed to saturation is recycled after regeneration.
The method can remove benzene and saturated water in acetylene, and the activated carbon with saturated adsorption can be regenerated and recycled after treatment, so that concentrated sulfuric acid is replaced or partially replaced, the consumption of the concentrated sulfuric acid is reduced, and the pressure of subsequent treatment and utilization is relieved.
Drawings
FIG. 1 is a diagram of an adsorption apparatus in step A of example 1;
fig. 2 is a diagram of the desorption regeneration apparatus in step B in example 1.
Detailed Description
The examples are provided for better illustration of the present invention, but the present invention is not limited to the examples. Therefore, those skilled in the art should make insubstantial modifications and adaptations to the embodiments of the present invention in light of the above teachings and remain within the scope of the invention.
Example 1
The method for adsorbing and desorbing benzene in acetylene comprises the following steps:
A. treating acetylene according to the device shown in figure 1, passing unpurified acetylene in an acetylene workshop through a rotor flow meter, then feeding the acetylene into an adsorption tower filled with activated carbon, feeding the purified acetylene into a synthesis section, arranging a sampling point at an outlet, connecting an inlet and an outlet of the adsorption tower with a differential pressure gauge for measuring the pressure difference of the inlet and the outlet, wherein the loading amount of the activated carbon is 350ml, the acetylene flow is 90L/h, and the acetylene space velocity is 257h-1During the operation, the pressure difference between the inlet and the outlet of the adsorption tower is 5mm of water column, and the benzene content and the water content in the acetylene at the outlet of the adsorption tower are respectively measured after 0h, 1h, 3h, 5h, 7h, 9h, 11h, 13h, 15h, 17h, 19h, 21h, 23h, 25h, 27h, 29h, 31h, 33h, 35h, 37h, 39h and 41h, and the results are shown in table 1; the method for measuring the content of benzene in acetylene adopts a gas chromatography, and specifically comprises the following steps: the instrument is Agilent7890A gas chromatograph, the detector is a hydrogen flame ionization detector, the chromatographic column is a Porapakn column, and the size and material of the column tube are stainless steel with the diameter of 2mm multiplied by 0.5 m; the operating conditions were: the temperature of the vaporizing chamber is 125 ℃, the column temperature is 110 ℃, the detector temperature is 200 ℃ and the carrier gas (N)2) The flow rate is 40mL/min, the hydrogen flow rate is 40mL/min, the air flow rate is 400mL/min, and the sample injection amount is 1 mL; the gas chromatography quantitative method adopts an external standard method, and the measuring method of the correction factor is as follows: after the operation conditions of each instrument are stable, respectively injecting samples, saturating the chromatographic column by the first sample injection, continuously injecting samples twice, measuring peak areas, calculating an average value, and calculating a correction factor; the water content in acetylene is measured by an SADP type dew point measuring instrument, and the method comprises the following specific steps: connecting any one of two interfaces of a dew point instrument with a sampling port by using a polytetrafluoroethylene tube, and controlling the gas flow rate to be (5-10) L/min; replacing the pipeline with sample gas for 3-5min, then plugging the outlet of the instrument with a finger, the pressure of the sample gas will open the detection head, and when the detection head of the instrument is completely opened, removing the finger (if the pressure of the sample gas is not large enough, connecting a proper pipe with the length of 1-2m to the outlet of the instrument, and then slowly lifting the detection head of the instrument with a hand); the instrument reading will move over the scale and then stabilize; when there is no large change in the reading, the final result is read. And (4) returning the purified acetylene to a vinyl acetate synthesis system.
TABLE 1 determination results of benzene content and water content in acetylene at the outlet of adsorption tower
Time/h Benzene content/ppm in acetylene Water content/ppm
0 Not detected out Not detected out
1 Not detected out Not detected out
3 Not detected out Not detected out
5 Not detected out Not detected out
7 Not detected out Not detected out
9 Not detected out Not detected out
11 Not detected out Not detected out
13 Not detected out Not detected out
15 Not detected out Not detected out
17 Not detected out Not detected out
19 Not detected out Not detected out
21 Not detected out Not detected out
23 Not detected out Not detected out
25 0.3 Not detected out
27 0.5 Not detected out
29 0.3 Not detected out
31 0.3 Not detected out
33 1.2 Not detected out
35 1.2 Not detected out
37 1.1 Not detected out
39 1.4 Not detected out
41 1.1 Not detected out
As can be seen from Table 1, benzene was not detected in the acetylene at the outlet of the adsorption column in the first 23 hours, the benzene content in the acetylene at the outlet of the adsorption column after 33 hours reached 1.2ppm, and the benzene content was greater than 1ppm in the sampling results of 35 hours, 37 hours, 39 hours and 41 hours. This demonstrated that the adsorption capacity of the activated carbon was saturated at 33 h. Water is not detected in the purified acetylene, so that the method is proved to be capable of removing saturated water in the acetylene, and the subsequent process does not need to separately measure the water content.
B. Activated carbon desorption regeneration was carried out according to the apparatus shown in fig. 2: placing the activated carbon which is saturated in adsorption into a reaction kettle with a clamping sleeve for heating, performing desorption regeneration, and introducing nitrogen into the bottom of the reaction kettle through a rotor flow meter to be connected with a gas distributor at the bottom of the reaction kettle; the filling amount of the activated carbon is 350ml, the jacket is heated by heat conduction oil, the oil temperature is 120 ℃, the temperature of the activated carbon is 115 ℃, benzene and water in the activated carbon are gasified and then blown out by nitrogen, the flow rate of the nitrogen is 60L/h, and the space velocity of the nitrogen is 171h-1Blowing air to a boiler device for combustion treatment; a thermometer is arranged in the reaction kettle and used for measuring the temperature of the activated carbon; and the benzene content in the blown gas is measured after 0h, 0.5h, 1h, 1.5h, 2h, 2.5h, 4.5h and 6.5h respectively, the measuring method is the same as the measuring method of the benzene content in the acetylene in the step A, and the results are shown in Table 2.
TABLE 2 determination of benzene content in the reactor outlet blow-off gas
Time/h Acetylene content/ppm
0 0.8
0.5 0.4
1 Not detected out
1.5 Not detected out
2 Not detected out
2.5 Not detected out
4.5 Not detected out
6.5 Not detected out
As can be seen from Table 2, after the activated carbon was desorbed and regenerated for 1 hour, no benzene was detected in the blown gas. This demonstrates that the activated carbon is free of benzene after 1h of desorption.
C. Adsorption by regenerated active carbon: and (3) placing the activated carbon desorbed and regenerated in the step (B) in an adsorption device in the step (A) for testing, wherein the test method and parameters are the same as those in the step (A), and the benzene content in the acetylene at the outlet of the adsorption tower is measured after 0h, 1h, 3h, 5h, 7h, 9h, 11h, 13h, 15h, 17h, 19h, 21h, 23h, 25h, 27h, 29h, 31h, 33h, 35h, 37h, 39h, 41h, 43h, 45h, 47h and 49h respectively, and the measurement method of the benzene content in the acetylene at the outlet of the adsorption tower is the same as that in the step (A), and the results are shown in Table 3.
TABLE 3 determination of benzene content in acetylene at the outlet of the adsorption column
Figure BDA0001785644000000041
Figure BDA0001785644000000051
As can be seen from Table 3, benzene was not detected in the acetylene at the outlet of the adsorption column in the first 29 hours, the benzene content in the acetylene at the outlet of the adsorption column after 41 hours was 1.2ppm, and the benzene content in the sampling results of 43 hours, 45 hours, 47 hours and 49 hours was more than 1 ppm. Therefore, the active carbon adsorption capacity is saturated at 41h, and the active carbon desorbed and regenerated by the method can be used for adsorbing benzene in acetylene.
Example 2
The method for adsorbing and desorbing benzene in acetylene comprises the following steps:
the experimental device, the steps and the parameters are the same as those of the example 1, except that the air input of acetylene and nitrogen is 45L/h, the air input of acetylene in the steps A and C is 45L/h, and the space velocity of acetylene is 129h-1In the step B, the nitrogen air inflow is 40L/h, and the nitrogen airspeed is 114h-1In the step A, the benzene content and the water content in the acetylene at the outlet of the adsorption tower are measured after 0h, 4h, 8h, 12h, 16h, 20h, 24h, 26h, 28h, 30h, 32h, 34h, 36h, 38h, 40h, 42h, 44h, 46h, 48h, 50h, 52h, 54h and 56h respectively, and the results are shown in Table 4; the method for measuring the content of benzene in acetylene is the same as the method for measuring the content of benzene in acetylene at the outlet of the adsorption tower in the step A in the example 1; in the step B, the benzene content in the outlet blown gas of the reaction kettle is measured after 0h, 0.5h, 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 6.5h and 8.5h respectively, and the results are shown in Table 5; the method for measuring the benzene content in the reaction kettle outlet blown-out gas is the same as the method for measuring the benzene content in the reaction kettle outlet blown-out gas in the step B of the embodiment 1; in the step C, the reaction time is respectively 0h, 4h, 8h, 12h, 16h, 20h, 24h, 26h, 28h, 30h and 32hAnd 34h, 36h, 38h, 40h, 42h, 44h, 46h, 48h, 50h, 52h, 54h, 56h, 58h, 60h, 62h, 64h, 66h, 68h, 70h, 72h and 74h, and determining the benzene content and the water content in the acetylene at the outlet of the adsorption tower, wherein the determination method of the benzene content in the acetylene at the outlet of the adsorption tower is the same as that of the step A, and the results are shown in Table 6.
TABLE 4 determination results of benzene content and water content in acetylene at the outlet of adsorption tower
Figure BDA0001785644000000052
Figure BDA0001785644000000061
As can be seen from Table 4, benzene was not detected in the acetylene at the outlet of the adsorption column within 32 hours from the start, the benzene content in the acetylene at the outlet of the adsorption column after 52 hours was 1.2ppm, and the benzene content was more than 1ppm in the sampling results of 54 hours and 56 hours. It was thus confirmed that the adsorption amount of activated carbon was saturated at 52 hours. Water is not detected in the purified acetylene, so that the method is proved to be capable of removing saturated water in the acetylene, and the subsequent process does not need to separately measure the water content.
TABLE 5 determination of benzene content in the reactor outlet blow-off gas
Time/h Acetylene content/ppm
0 0.7
0.5 0.6
1 0.4
1.5 0.5
2 0.2
2.5 0.3
3 0.4
3.5 0.3
4 Not detected out
4.5 Not detected out
6.5 Not detected out
8.5 Not detected out
As can be seen from Table 5, after the activated carbon was desorbed and regenerated for 4 hours, no benzene was detected in the blown gas. This demonstrates that the activated carbon is free of benzene after 4h desorption.
TABLE 6 determination results of benzene content in acetylene at the outlet of adsorption column
Figure BDA0001785644000000062
Figure BDA0001785644000000071
As can be seen from Table 6, benzene was not detected in the acetylene at the outlet of the adsorption column in the first 38 hours, the benzene content in the acetylene at the outlet of the adsorption column after 68 hours was 1.1ppm, and the benzene content was more than 1ppm in the sampling results of 70 hours, 72 hours and 74 hours. This demonstrated that the amount of adsorbed activated carbon was saturated at 68 h.
Example 3
The method for adsorbing and desorbing benzene in acetylene comprises the following steps:
the experimental device, the steps and the parameters are the same as those of the example 1, except that the air input of acetylene and nitrogen is 175L/h, the air input of acetylene in the steps A and C is 175L/h, and the space velocity of acetylene is 500h-1In the step C, the nitrogen gas inflow is 140L/h, and the nitrogen airspeed is 400h-1In the step A, the benzene content and the water content in the acetylene at the outlet of the adsorption tower are measured after 0h, 2h, 4h, 6h, 8h, 12h, 13h, 14h, 15h, 16h, 17h, 18h, 19h, 20h, 21h, 22h and 23h respectively, and the results are shown in Table 7; the determination method is the same as the detection method of the benzene content and the water content in the acetylene at the outlet of the adsorption tower in the step A of the embodiment 1; in the step B, the benzene content in the air blown out from the outlet of the reaction kettle is measured after 0min, 5min, 10min, 15min, 20min, 25min, 30min and 35min respectively, and the results are shown in Table 8; the method for measuring the benzene content in the reaction kettle outlet blown-out gas is the same as the method for measuring the benzene content in the reaction kettle outlet blown-out gas in the step B of the embodiment 1; and C, respectively measuring the benzene content in the acetylene at the outlet of the adsorption tower after 0h, 2h, 4h, 6h, 8h, 10h, 12h, 14h, 16h, 20h, 22h, 24h, 25h, 26h, 27h, 28h, 29h, 30h, 31h and 32h in the step C, wherein the measuring method is the same as the measuring method of the benzene content in the acetylene in the step A, and the results are shown in Table 9.
TABLE 7 determination results of benzene content and water content in acetylene at the outlet of adsorption column
Time/h Benzene content/ppm in acetylene Water content/ppm
0 Not detected out Not detected out
2 Not detected out Not detected out
4 Not detected out Not detected out
6 Not detected out Not detected out
8 Not detected out Not detected out
10 Not detected out Not detected out
12 Not detected out Not detected out
13 Not detected out Not detected out
14 Not detected out Not detected out
15 Not detected out Not detected out
16 Not detected out Not detected out
17 Not detected out Not detected out
18 0.5 Not detected out
19 0.6 Not detected out
20 0.8 Not detected out
21 1.1 Not detected out
22 1.3 Not detected out
23 1.2 Not detected out
As can be seen from Table 7, benzene was not detected in the outlet acetylene of the adsorption column in the first 17 hours, the benzene content in the outlet acetylene of the adsorption column after 21 hours was 1.2ppm, and the benzene content in the sampling results of 22 hours and 23 hours was more than 1 ppm. This proves that the adsorption amount of activated carbon is saturated at 21 hours. Water is not detected in the purified acetylene, so that the method is proved to be capable of removing saturated water in the acetylene, and the subsequent process does not need to separately measure the water content.
TABLE 8 determination of benzene content in the reactor outlet blow-off gas
Time/min Acetylene content/ppm
0 0.6
5 0.4
10 0.5
15 0.3
20 Not detected out
25 Not detected out
30 Not detected out
35 Not detected out
As can be seen from Table 8, after 20min of desorption and regeneration of the activated carbon, no benzene was detected in the blown gas. This demonstrates that the activated carbon is free of benzene after 20 minutes of desorption.
TABLE 9 determination of benzene content in acetylene at the outlet of the adsorption column
Time/h Benzene content/ppm in acetylene
0 Not detected out
2 Not detected out
4 Not detected out
6 Not detected out
8 Not detected out
10 Not detected out
12 Not detected out
14 Not detected out
16 Not detected out
18 Not detected out
20 Not detected out
22 Not detected out
24 Not detected out
25 Not detected out
26 0.3
27 0.6
28 0.5
29 0.8
30 1.2
31 1.4
32 1.8
As can be seen from Table 9, benzene was not detected in the acetylene at the outlet of the adsorption column within 25 hours from the start, the benzene content in the acetylene at the outlet of the adsorption column after 30 hours was 1.2ppm, and the benzene content was more than 1ppm in both the sampling results of 31 hours and 32 hours. This proves that the adsorption amount of activated carbon is saturated at 30 hours.
Comparative example 1
The method for desorbing benzene in acetylene comprises the following steps:
the experimental setup, procedure and parameters used were the same as in step B of example 2, except that the jacket heating temperature was increased to 150 ℃, and the benzene content in the reactor outlet blow-off gas was measured after 0h, 0.5h, 1h, 1.5h, 2h, 2.5h, 3h, 3.5h and 4h, respectively, with the results shown in table 10:
TABLE 10 determination of benzene content in the reactor outlet blow-off gas
Time/h Acetylene content/ppm
0 0.8
0.5 0.6
1 0.7
1.5 0.5
2 0.2
2.5 0.3
3 Not detected out
3.5 Not detected out
4 Not detected out
As can be seen from Table 10, after 3 hours of desorption and regeneration of the activated carbon, no benzene was detected in the blown gas; thus, the activated carbon does not contain benzene after being desorbed for 3 hours, and the regeneration time is shortened by 1 hour compared with that under the condition of 120 ℃.
As can be seen from examples 1-3 and comparative example 1, the method of the present invention can treat benzene in acetylene to make the benzene content in acetylene lower than 1ppm, and meet the requirements of the subsequent process; the time for the activated carbon adsorption to reach saturation is prolonged as the space velocity of acetylene is reduced. The method can regenerate the activated carbon with saturated adsorption, the regeneration time is prolonged along with the reduction of the airspeed of the nitrogen, and the regeneration time is shortened along with the increase of the heating temperature of the jacket; the regenerated active carbon can be used for adsorbing benzene in acetylene.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (5)

1. The method for adsorbing and desorbing benzene in acetylene is characterized by comprising the following steps of:
A. placing unpurified acetylene into an adsorption tower filled with activated carbon, and returning the purified acetylene to a vinyl acetate synthesis system;
B. activated carbon desorption and regeneration: placing the activated carbon which is saturated in adsorption into a reaction kettle with a jacket for heating for desorption and regeneration, introducing inert gas into the bottom of the reaction kettle to be connected with a gas distributor at the bottom of the reaction kettle, heating the reaction kettle through the jacket, and blowing out gas to be sent to a boiler for combustion treatment.
2. The method as claimed in claim 1, wherein the space velocity of acetylene is 129-500h-1。
3. The method as claimed in claim 1 or 2, wherein the inert gas space velocity is 114--1。
4. The method for adsorbing and desorbing benzene in acetylene according to claim 1, 2 or 3, wherein the heating temperature of the jacket in step B is 120-150 ℃.
5. The method for adsorbing and desorbing benzene in acetylene according to claim 1, 2, 3 or 4, wherein the benzene content in acetylene at the outlet of the adsorption tower and the benzene content in the blown-off gas are measured by gas chromatography, and the water content in the purified acetylene is measured by a dew-point measuring instrument.
CN201811013642.XA 2018-08-31 2018-08-31 Method for adsorbing and desorbing benzene in acetylene Pending CN110871013A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201811013642.XA CN110871013A (en) 2018-08-31 2018-08-31 Method for adsorbing and desorbing benzene in acetylene

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201811013642.XA CN110871013A (en) 2018-08-31 2018-08-31 Method for adsorbing and desorbing benzene in acetylene

Publications (1)

Publication Number Publication Date
CN110871013A true CN110871013A (en) 2020-03-10

Family

ID=69715339

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201811013642.XA Pending CN110871013A (en) 2018-08-31 2018-08-31 Method for adsorbing and desorbing benzene in acetylene

Country Status (1)

Country Link
CN (1) CN110871013A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114849417A (en) * 2022-04-26 2022-08-05 中国石油化工股份有限公司 System and method for purifying raw material acetylene
CN118654292A (en) * 2024-08-20 2024-09-17 四川天予强盛环保科技有限公司 A grate furnace system and treatment process for domestic waste treatment

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101077983A (en) * 2007-06-21 2007-11-28 苏州制氧机有限责任公司 Method for removing benzene from natural gas
CN101362076A (en) * 2007-08-06 2009-02-11 中国石油化工股份有限公司 Regeneration method of active carbon absorbent
CN101700940A (en) * 2009-11-10 2010-05-05 南京信息工程大学 Method for treatment of nitrobenzene wastewater and resource recovery
CN101721833A (en) * 2008-10-28 2010-06-09 中国石油化工股份有限公司 Method for recovering and purifying hydrocarbon wastegas by condensation and adsorption
US20100192774A1 (en) * 2006-10-12 2010-08-05 Hirokazu Aono Activated carbon and canister and intake air filter utilizing the same
CN101806784A (en) * 2010-04-29 2010-08-18 成都市疾病预防控制中心 Method for measuring content of benzene in air
CN105080287A (en) * 2015-08-13 2015-11-25 中国石油化工股份有限公司 Activated carbon desorption method of activated carbon canister in benzene vapor recovery device

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20100192774A1 (en) * 2006-10-12 2010-08-05 Hirokazu Aono Activated carbon and canister and intake air filter utilizing the same
CN101077983A (en) * 2007-06-21 2007-11-28 苏州制氧机有限责任公司 Method for removing benzene from natural gas
CN101362076A (en) * 2007-08-06 2009-02-11 中国石油化工股份有限公司 Regeneration method of active carbon absorbent
CN101721833A (en) * 2008-10-28 2010-06-09 中国石油化工股份有限公司 Method for recovering and purifying hydrocarbon wastegas by condensation and adsorption
CN101700940A (en) * 2009-11-10 2010-05-05 南京信息工程大学 Method for treatment of nitrobenzene wastewater and resource recovery
CN101806784A (en) * 2010-04-29 2010-08-18 成都市疾病预防控制中心 Method for measuring content of benzene in air
CN105080287A (en) * 2015-08-13 2015-11-25 中国石油化工股份有限公司 Activated carbon desorption method of activated carbon canister in benzene vapor recovery device

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
郝利平等主编: "《食品添加剂》", 31 July 2016, 北京：中国农业大学出版社 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114849417A (en) * 2022-04-26 2022-08-05 中国石油化工股份有限公司 System and method for purifying raw material acetylene
CN118654292A (en) * 2024-08-20 2024-09-17 四川天予强盛环保科技有限公司 A grate furnace system and treatment process for domestic waste treatment

Similar Documents

Publication Publication Date Title
CN110871013A (en) Method for adsorbing and desorbing benzene in acetylene
JP2005516894A (en) Purification of organic solvents
CN102861561B (en) Desorption regeneration method of hydrophobic macroporous polymer adsorbent for adsorbing butanol
CN109694073A (en) Double high technologies of UF membrane high purity carbon monoxide and hydrogen in conjunction with pressure-variable adsorption
CN110871057A (en) Activated carbon regeneration method
CN103055676B (en) Method for purifying natural gas
US9108897B2 (en) Method for desorbing and regenerating butanol-adsorbing hydrophobic macroporous polymer adsorbent
CN104801279A (en) Method for modifying activated carbon particles with sol-gel method
CN102372595B (en) Method for separating butanol
CN212024774U (en) System for preparing 4N-purity hydrogen sulfide gas
CN210855273U (en) Purification device of high-purity hydrogen sulfide
CN111333037B (en) System and method for preparing high-purity hydrogen sulfide gas
CN101323585B (en) Enrichment and purification method of benzene acryloyl 5-hydroxytryptamine compound in safflower seed
CN114180525A (en) Separation method of hydrogen chloride/dichloromethane in synthesis of 4-chloroacetoacetic acid ethyl ester
CN204873823U (en) Coke oven gas system liquefied natural gas's rich hydrogen tail gas processing apparatus
CN204325196U (en) A kind of acetic acid aceticanhydride underpressure distillation tripping device
CN204093268U (en) A kind of temperature swing absorption unit for the protection of membrane separation plant
CN104098739A (en) Preparation method for rebaudiodside A molecularly-imprinted polymer
CN205419770U (en) Hydrogen rich gas source purification hydrogen device
CN207002279U (en) A kind of technical argon efficiently purifying device
CN109621634B (en) Method, device and system for purifying acetylene by calcium carbide
CN105820292B (en) A kind of preparation method and the application of optional removing toluene and benzene molecular imprinted polymer post
CN114624372B (en) Method for detecting acetic acid in air and gas chromatograph
CN112934185B (en) Based on supercritical CO 2 Organic acid hydrophobic modified biochar of medium, and preparation method and application thereof
CN221522483U (en) Device for producing hydrogen based on coke oven gas and high-purity hydrogen preparation device

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination