CN110132700B - Device and process for removing acrolein, acrylic acid and water in gas inlet of on-line propylene infrared analyzer - Google Patents
Device and process for removing acrolein, acrylic acid and water in gas inlet of on-line propylene infrared analyzer Download PDFInfo
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- CN110132700B CN110132700B CN201910448698.6A CN201910448698A CN110132700B CN 110132700 B CN110132700 B CN 110132700B CN 201910448698 A CN201910448698 A CN 201910448698A CN 110132700 B CN110132700 B CN 110132700B
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- acrylic acid
- gas
- water
- propylene
- acrolein
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- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 title claims abstract description 70
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 56
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 title claims abstract description 42
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 title claims abstract description 41
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 14
- 238000005406 washing Methods 0.000 claims abstract description 22
- 238000001816 cooling Methods 0.000 claims abstract description 21
- 238000001035 drying Methods 0.000 claims abstract description 16
- 230000003647 oxidation Effects 0.000 claims abstract description 16
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 16
- 239000012528 membrane Substances 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000010521 absorption reaction Methods 0.000 claims description 10
- 239000011148 porous material Substances 0.000 claims description 6
- 238000010612 desalination reaction Methods 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 5
- 230000008676 import Effects 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000003507 refrigerant Substances 0.000 claims description 3
- 239000002253 acid Substances 0.000 abstract description 8
- 238000004458 analytical method Methods 0.000 abstract description 7
- 230000014759 maintenance of location Effects 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 239000002826 coolant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
- G01N21/3518—Devices using gas filter correlation techniques; Devices using gas pressure modulation techniques
Abstract
The invention relates to a device and a process for removing acrolein (acid) and water in inlet air of an on-line propylene infrared analyzer in an acrylic acid oxidation device, wherein the device comprises a water washing tower, a deep cooling tank, a filter and a drying tower, the water washing tower is used for washing and absorbing acrylic acid and acrolein in gas, the washed gas enters from the bottom of the deep cooling tank, is collected from the top after cooling and dewatering, is dewatered again through a pipeline connecting filter, and the gas flowing through a filtering membrane enters the on-line propylene infrared analyzer after drying. The device has the advantages of removing acrylic acid and acrolein in the gas with a removing rate of more than 98 percent, completely removing water vapor, reducing the influence of the acrylic acid and the acrolein on the online analysis result of the propylene, along with simple flow, low cost and high acrylic acid and acrolein removing efficiency.
Description
Technical Field
The invention relates to a device and a process for removing acrolein (acid) and water in the inlet gas of an on-line propylene infrared analyzer in an acrylic acid oxidation device, which reduce the influence of acrylic acid and acrolein on the analysis of propylene content by pre-treating the gas entering an on-line infrared detection instrument.
Background
The propylene on-line analysis method is that propylene-containing gas enters an infrared detector, and the detector measures the content of propylene in the gas according to the absorbed value of the intensity of infrared light with a specific wavelength. Besides propylene and propane, the circulating gas of the acrylic acid oxidation device still has certain amounts of acrolein and acrylic acid, the acrolein content is 500-2000ppm, the acrylic acid content is 50-500ppm, and the two substances also absorb infrared light in the wave band, so that the online measurement of the propylene value is larger. There is no report of the technique of acrylic acid and acrolein removal for this gas stream.
Disclosure of Invention
In view of the above, the present invention provides an apparatus and process for removing acrolein (acid) and water from the inlet gas of an on-line propylene infrared analyzer in an acrylic acid oxidation apparatus. The device is a pretreatment device used for treating acrolein (acid) and water in the sample gas of an online propylene infrared analyzer in an acrylic acid oxidation device, and the device can be used for pretreating the gas entering the online infrared detector, so that more than 98% of acrylic acid and acrolein in the gas to be detected can be removed, and the influence of the acrylic acid and the acrolein on the analysis of the content of propylene is reduced.
The device for removing acrolein (acid) and water in the inlet gas (or circulating gas) of the on-line propylene infrared analyzer in the acrylic acid oxidation device comprises a water washing tower, a deep cooling tank, a filter and a dryer which are connected in sequence,
the utility model discloses a deep cooling device, including wash tower, water scrubber, lower part connection propylene air inlet pipeline, the shower nozzle of upper portion (preferred upper portion position in the middle) is located the absorption tower to the desalination water line connection, and the bottom liquid outlet of absorption tower passes through pipe connection to buffer memory jar, and the bottom of the upper portion gas outlet connection deep cooling jar of absorption tower, the top exit linkage filter import of deep cooling jar, the filter export and the access connection of desicator, the online propylene infrared analyzer of exit linkage (infrared ray on-line detector) introduction port of desicator.
Further, the cryogenic tank is connected with a refrigerant pipeline for cooling the gas. The cooling medium is introduced into an external jacket of the deep cooling tank to cool the gas in the tank.
Furthermore, the flow rate of the nozzle is 3-8L/h, preferably 4-5L/h, the pressure is 100-300kPa, preferably 150-200kPa, more preferably 110-200 kPa, and the water temperature can be 20-60 ℃.
Furthermore, the working temperature of the deep cooling tank is generally 1 to 10 ℃ and the pressure is 110 to 200 kPa. The deep cooling tank DN can be 100-500mm, the height can be 150-400mm, and in one embodiment, the deep cooling tank DN is 150mm, the height is 200mm, and the material is 316L.
Further, the DN of the water washing tower can be 150-400mm, the height can be 300-600mm, and in one embodiment, the DN is 200mm and the height is 400 mm.
Further, the pore size of the filtration membrane of the filter is in the range of 0.1 to 2 μm.
Further, the working temperature of the dryer is 10-40 ℃, the pressure is 110-200 kpa, and the retention (drying) time is 1-2 seconds.
Further, the dryer (drying column) DN can be 150-400mm and the height can be 150-400mm, in one embodiment DN200mm, height 200 mm. Silica gel was filled in the drying column.
The process for removing acrolein (acid) and water in the inlet gas (or circulating gas) of an on-line propylene infrared analyzer in an acrylic acid oxidation device comprises the following steps:
introducing sample gas of an online propylene infrared analyzer of an acrylic acid oxidation device into a water washing tower from the lower part of the water washing tower, washing the sample gas by desalted water sprayed downwards from the upper part in the water washing tower, absorbing acrylic acid and acrolein in the sample gas, introducing the gas subjected to acrylic acid and acrolein removal from the bottom of a cryogenic tank, extracting the gas from the top after cooling and water removal, removing water through a pipeline connection filter, introducing the gas flowing through a filtering membrane from the bottom of a drying tower, and introducing the gas after drying into an online propylene infrared analyzer (an online infrared detector).
Further, the introduction flow rate of the injection gas is 20 to 80L/h, typically 50 to 70L/h, for example 60L/h.
Furthermore, the desalted water is sprayed downwards through a spray head, the flow rate of the spray head is 3-8L/h, preferably 4-5L/h, the pressure is 100-300kPa, preferably 150-200kPa, more preferably 110-200 kPa, and the water temperature can be 20-60 ℃.
Further, the operating temperature range of the deep cooling tank is 1-10 ℃, and the pressure is 110-200 kPa.
Furthermore, the pore size of the filter membrane of the filter is 0.1-2 μm.
Furthermore, the operation temperature of the drying tower is 10-40 ℃, the pressure is 110-200 kPa, and the retention (drying) time is 1-2S.
THE ADVANTAGES OF THE PRESENT INVENTION
The device and the process can remove more than 98 percent of acrylic acid and acrolein in the gas to be detected by pretreating the gas entering the online infrared detection instrument, completely remove water vapor, reduce the influence of the acrylic acid and the acrolein on the online analysis result of the propylene, and have the advantages of simple flow, low cost and high acrylic acid and acrolein removal efficiency.
Drawings
FIG. 1 is a schematic diagram showing the structure of an apparatus for removing acrolein (acid) and water from an intake gas of an on-line infrared analyzer for propylene in an acrylic acid oxidation apparatus according to the present invention.
Detailed Description
Referring to fig. 1, an apparatus for removing acrolein (acid) and water from an on-line propylene infrared analyzer inlet gas (or a recycle gas) in an acrylic acid oxidation apparatus, which comprises a water washing column 3, a cryogenic tank 5, a filter 7 and a dryer 8 connected in sequence,
absorption tower upper portion is equipped with desalination water line 1, sub-unit connection propylene inlet line 2, desalination water line connection is located the shower nozzle (not shown) of upper portion (preferred upper portion position between two parties) in the absorption tower, the bottom liquid outlet of absorption tower is connected to buffer tank 4 through pipeline 10, the upper portion gas outlet of absorption tower passes through pipeline 11 and connects the bottom of cryogenic tank 5, the top exit linkage filter 7 import of cryogenic tank, the exit of filter 7 is connected with the access connection of desicator 8, the export of desicator is passed through pipeline 9 and is connected online propylene infrared analyzer (infrared ray on-line detector) introduction port.
The cryogenic tank is connected with a refrigerant pipeline 6 for cooling the gas.
The flow rate of the spray head is generally 3-8L/h, preferably 4-5L/h, and the pressure is generally 100-300kPa, preferably 150-200 kPa.
The working temperature of the deep cooling tank is generally 1-10 ℃, and the pressure is 110-200 kPa.
The pore diameter of the filter membrane of the filter is 0.1-2 μm.
The working temperature of the dryer is generally 10-40 ℃, the pressure is 110-200 kpa, and the retention (drying) time is 1-2 seconds.
The process comprises introducing sample gas of an online propylene infrared analyzer of an acrylic acid oxidation device into a water washing tower 3 from the lower part of the water washing tower 3, washing the sample gas by desalted water sprayed downwards from the upper part in the water washing tower, absorbing acrylic acid and acrolein in the sample gas, introducing the gas subjected to acrylic acid and acrolein removal from the bottom of a cryogenic tank 5, collecting the gas from the top after cooling and water removal, further removing water through a pipeline connection filter 7, introducing the gas flowing through a filter membrane from the bottom of a drying tower 8, drying and then introducing the gas into the online propylene infrared analyzer.
Example 1
In the (meth) acrylic acid oxidation apparatus, raw material propylene gas (60L/h) for oxidation was fed from the lower part of a water washing column (DN 200mm, height 400 mm), desalted water (flow rate 6L/h pressure 150kPa, introduced through a nozzle) was introduced from the upper part of the water washing column to wash and absorb the propylene gas, the washed propylene gas was introduced into the bottom of a deep cooling tank (DN 150mm, height 200mm, capped material 316L) through a pipeline, cooled by 5 ℃ chilled water (pressure 130 kPa) and then discharged from the top, and further removed water by entering a filter (filter membrane pore size 0.1 μm), and then entered from the bottom of a drying column (DN 200mm, height 200mm, internally filled with silica gel), dried at 15 ℃ for 2S (pressure 120 kPa) and entered an on-line propylene infrared analyzer (Emerson Smoke analysis System, model X-STREAM series). The gas (injection gas) which had not been subjected to this step had an actual propylene content of 1897ppm, an actual acrylic acid content of 160ppm, and an acrolein content of 1400ppm, and the on-line chart showed a reading of 3109 ppm; after treatment with the system of the present invention, the on-line propylene showed a reading of 1951ppm, no acrylic acid was detected in the gas, the acrolein content was 25ppm, and no water vapor was detected after treatment. The results show that the invention can remove more than 98 percent of acrylic acid and acrolein in the gas to be detected, completely remove water vapor and reduce the influence of the acrylic acid and the acrolein on the online analysis result of propylene.
Claims (12)
1. A device for removing acrolein, acrylic acid and water in the inlet gas of an on-line propylene infrared analyzer, wherein the inlet gas of the propylene infrared analyzer is from an acrylic acid oxidation device and comprises a water washing tower, a deep cooling tank, a filter and a dryer which are connected in sequence,
the washing tower upper portion is equipped with the desalination water line, and the sub-unit connection propylene intake line, the shower nozzle on desalination water line connection upper portion in being located the absorption tower, and the bottom liquid outlet of absorption tower passes through pipe connection to buffer memory jar, and the bottom of the upper portion gas outlet connection cryogenic tank of absorption tower, the top exit linkage filter import of cryogenic tank, the filter export and the access connection of desicator, the online propylene infrared analyzer introduction port of exit linkage of desicator.
2. The apparatus of claim 1, wherein a refrigerant line for cooling the gas is connected to the cryogenic tank.
3. The apparatus as claimed in claim 1, wherein the flow rate of the spray head is 3-8L/h, and the pressure is 100 kPa and 300 kPa.
4. The apparatus as claimed in claim 3, wherein the flow rate of the spray head is 4-5L/h, and the pressure is 150kPa and 200 kPa.
5. The apparatus according to claim 1, wherein the cryogenic tank has an operating temperature of 1 to 10 ℃ and a pressure of 110 to 200 kPa.
6. The apparatus according to claim 1, wherein the filter has a membrane pore size in the range of 0.1 to 2 μm.
7. The apparatus according to claim 1, wherein the dryer is operated at 10 to 40 ℃ under a pressure of 110 to 200kPa for 1 to 2 seconds.
8. A process for the removal of acrolein, acrylic acid and water from an on-line propylene infrared analyzer feed from an acrylic acid oxidation plant, based on the plant of claim 1, comprising the steps of:
introducing sample gas of an online propylene infrared analyzer of an acrylic acid oxidation device into a water washing tower from the lower part of the water washing tower, washing the sample gas by desalted water sprayed downwards from the upper part in the water washing tower, absorbing acrylic acid and acrolein in the sample gas, introducing the gas subjected to acrylic acid and acrolein removal from the bottom of a cryogenic tank, extracting the gas from the top after cooling and water removal, removing water through a pipeline connection filter, introducing the gas flowing through a filtering membrane from the bottom of a drying tower, and introducing the gas into the online propylene infrared analyzer after drying.
9. The process as claimed in claim 8, wherein the flow rate of the desalted water sprayed is 3-8L/h, the pressure is 100 kPa and 300kPa, and the temperature of the water is 20-60 ℃.
10. The process as set forth in claim 9 wherein the pressure is 150kPa and 200 kPa.
11. The process according to claim 8, wherein the cryogenic tank operates at a temperature in the range of 1 to 10 ℃ and a pressure in the range of 110 to 200 kPa; and/or
The pore diameter of the filter membrane of the filter is 0.1-2 μm.
12. The process according to claim 8, wherein the drying tower is operated at 10-40 ℃, under 110-200 kPa for 1-2S.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910448698.6A CN110132700B (en) | 2019-05-27 | 2019-05-27 | Device and process for removing acrolein, acrylic acid and water in gas inlet of on-line propylene infrared analyzer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910448698.6A CN110132700B (en) | 2019-05-27 | 2019-05-27 | Device and process for removing acrolein, acrylic acid and water in gas inlet of on-line propylene infrared analyzer |
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| CN110132700A CN110132700A (en) | 2019-08-16 |
| CN110132700B true CN110132700B (en) | 2022-08-02 |
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| CN111879594A (en) * | 2020-07-29 | 2020-11-03 | 濮阳市盛源能源科技股份有限公司 | Water washing device for reaction generated gas in process of preparing maleic anhydride by oxidizing n-butane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| FR2798382B1 (en) * | 1999-09-14 | 2001-10-26 | Atofina | PROCESS FOR THE PURIFICATION OF ACRYLIC ACID OBTAINED BY OXIDATION OF PROPYLENE AND / OR ACROLEIN |
| CN101835736B (en) * | 2007-10-23 | 2013-06-12 | Lg化学株式会社 | Method for collecting (meth)acrylic acid and apparatus for collecting (meth)acrylic acid |
| CN101260032B (en) * | 2008-01-27 | 2010-09-29 | 中国石油集团工程设计有限责任公司东北分公司 | Modified technique for preparing acrylic acid by propylene two-step oxygenation method |
| JP5654469B2 (en) * | 2008-10-01 | 2015-01-14 | アーケマ・インコーポレイテッド | Control the process to purify (meth) acrylic acid using online near infrared analysis |
| CN109232232B (en) * | 2018-11-19 | 2021-06-22 | 平湖石化有限责任公司 | Refining method of acrylic acid |
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