CN114213209B - Ethylene purification method - Google Patents
Ethylene purification method Download PDFInfo
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- CN114213209B CN114213209B CN202111681341.6A CN202111681341A CN114213209B CN 114213209 B CN114213209 B CN 114213209B CN 202111681341 A CN202111681341 A CN 202111681341A CN 114213209 B CN114213209 B CN 114213209B
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- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 title claims abstract description 172
- 239000005977 Ethylene Substances 0.000 title claims abstract description 172
- 238000000746 purification Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000002808 molecular sieve Substances 0.000 claims abstract description 163
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 163
- 238000001179 sorption measurement Methods 0.000 claims abstract description 78
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910001868 water Inorganic materials 0.000 claims abstract description 31
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002994 raw material Substances 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims description 9
- 238000011049 filling Methods 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 239000012535 impurity Substances 0.000 abstract description 37
- 230000000694 effects Effects 0.000 abstract description 18
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 238000005516 engineering process Methods 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 5
- 239000007789 gas Substances 0.000 description 66
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 24
- 238000012360 testing method Methods 0.000 description 14
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 13
- 229910001431 copper ion Inorganic materials 0.000 description 13
- 239000003463 adsorbent Substances 0.000 description 12
- 229910052742 iron Inorganic materials 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
- -1 iron ions Chemical class 0.000 description 10
- 239000003054 catalyst Substances 0.000 description 9
- 239000010949 copper Substances 0.000 description 9
- 238000001514 detection method Methods 0.000 description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229930195733 hydrocarbon Natural products 0.000 description 5
- 150000002430 hydrocarbons Chemical class 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000004215 Carbon black (E152) Substances 0.000 description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- 238000009835 boiling Methods 0.000 description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 description 4
- 239000006096 absorbing agent Substances 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005530 etching Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000015654 memory Effects 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000000927 vapour-phase epitaxy Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/12—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers
- C07C7/13—Purification; Separation; Use of additives by adsorption, i.e. purification or separation of hydrocarbons with the aid of solids, e.g. with ion-exchangers by molecular-sieve technique
Abstract
The invention discloses an ethylene purification method, which comprises the following steps: introducing ethylene gas raw material into a first adsorber, wherein a first molecular sieve is arranged in the first adsorber, and the first molecular sieve adsorbs and removes water; introducing the mixture into a second adsorber, wherein the second adsorber is internally provided with active alumina, and the active alumina adsorbs and removes ethane; introducing the mixture into a third adsorber, wherein a second molecular sieve is arranged in the third adsorber, and the second molecular sieve is used for removing heavy components through adsorption; introducing the mixture into a first rectifying tower for rectifying treatment, and separating and removing heavy components by the first rectifying tower; and (3) introducing the mixture into a second rectifying tower for rectifying treatment, and separating and removing light components by the second rectifying tower. The technology can firstly remove part of impurities in an adsorption separation mode, reduce impurity components entering the first rectifying tower and the second rectifying tower, and improve the production efficiency while improving the purification effect; and the effect of removing heavy components is better, and the purity of the obtained ethylene is higher.
Description
Technical Field
The invention relates to the technical field of ethylene production, in particular to an ethylene purification method.
Background
In the integrated circuit manufacturing, the high-purity ethylene is mainly applied to dielectric layer film etching of aluminum metal surfaces in chip manufacturing, chemical vapor deposition and vapor phase epitaxy growth process stages of third-generation SiC, or manufacturing processes of semiconductor devices such as 64-128 layers of 3D NAND memories, and along with the rapid development of the semiconductor industry, the application of the high-purity ethylene is continuously increased, and the purity requirement is continuously improved. The main impurities contained in the ethylene gas raw material include oxygen, nitrogen, carbon monoxide, carbon dioxide, water and other hydrocarbon impurities such as methane, ethane, acetylene, propylene, propane, butene and the like, and the high-purity ethylene is obtained after the impurities are purified.
The purification degree of the prior general ethylene purification process on the ethylene gas raw material is not high enough, and the obtained ethylene finished product can not meet the use requirement of high purity, or the production efficiency of the high purity ethylene is lower.
In addition, the difficulty in ethylene purification is that ethylene contains carbon-carbon double bonds, 1 sigma bond and 1 pi bond respectively, wherein pi bonds are unstable, carbon bonds are easily broken in the existing purification process, loss of ethylene main components is caused, and new impurities are generated. Therefore, it is necessary to select an appropriate purification process to adsorb impurities, reduce the loss rate of ethylene, and improve the purity of ethylene.
Disclosure of Invention
The invention mainly aims to provide an ethylene purification method, and aims to solve the technical problems that the ethylene finished product obtained by the ethylene purification method in the prior art is not high enough in purity and low in production efficiency.
In order to achieve the above object, the present invention provides a method for purifying ethylene, comprising the steps of:
s1: introducing an ethylene gas raw material into a first adsorber, wherein a first molecular sieve is arranged in the first adsorber, and the first molecular sieve adsorbs and removes water in the ethylene gas raw material;
s2: introducing the ethylene gas with the water removed into a second adsorber, wherein the second adsorber is internally provided with activated alumina, and the activated alumina adsorbs and removes ethane in the ethylene gas;
s3: introducing ethylene gas from which ethane is removed into a third adsorber, wherein a second molecular sieve is arranged in the third adsorber, and the second molecular sieve adsorbs and removes heavy components in the ethylene gas;
s4: introducing ethylene gas adsorbed by the second molecular sieve into a first rectifying tower for rectification treatment, and separating and removing heavy components in the ethylene gas by the first rectifying tower;
s5: introducing ethylene gas flowing out from the top of the first rectifying tower into a second rectifying tower for rectification treatment, and separating and removing light components in the ethylene gas by the second rectifying tower;
s6: discharging light components from the top of the second rectifying tower, detecting the content of the light components in the gas flowing out from the top of the second rectifying tower, and filling ethylene finished products from the top of the second rectifying tower outwards when detecting that the content of the light components is reduced to be qualified.
And purifying the ethylene gas raw material sequentially through a first adsorber, a second adsorber, a third adsorber, a first rectifying tower and a second rectifying tower to obtain an ethylene finished product with higher purity.
The technology firstly utilizes a first molecular sieve to adsorb moisture; then the activated alumina is utilized to adsorb ethane, and the test shows that the activated alumina can effectively adsorb and remove ethane; then the second molecular sieve is utilized to adsorb heavy components with boiling point higher than that of ethylene; then rectifying and separating heavy components by using a first rectifying tower, wherein the heavy components are left at the bottom of the first rectifying tower, and ethylene and light components are discharged from the top of the first rectifying tower; then separating light components by using a second rectifying tower, and discharging the light components from the top of the second rectifying tower; and then detecting the content of light components in the gas discharged from the top of the second rectifying tower, and when the content of the light components is detected to be reduced to be qualified, indicating that the light components contained in the second rectifying tower are less, the ethylene in the second rectifying tower is higher in purity, the ethylene with higher purity can be filled outwards from the top of the second rectifying tower, and the heavy components are further separated from the bottom of the second rectifying tower, so that an ethylene finished product filled from the top of the second rectifying tower is higher in purity.
The technology can firstly remove part of impurities in an adsorption separation mode, reduce impurity components entering the first rectifying tower and the second rectifying tower, so that the rectifying speed can be increased, and the production efficiency can be improved while the purifying effect is improved; and the effect of removing heavy components by using the activated alumina, the second molecular sieve, the first rectifying tower and the second rectifying tower is better, and the purity of the obtained ethylene is higher.
Preferably, the first molecular sieve is a 3A molecular sieve;
the first molecular sieve used in the step S1 is activated for 7-9 hours at the temperature of 300-400 ℃, then high-purity ethylene is introduced into the first adsorber, and pre-adsorption of the first molecular sieve is carried out under the pressure of 0.1-0.5Mpa until the temperature fluctuation of the first adsorber is within 10 ℃, and then the step S1 is carried out;
the adsorption pressure in the step S1 is 0.3-0.8Mpa, and the adsorption temperature is lower than 50 ℃.
The 3A molecular sieve can adsorb and remove water. Before the 3A molecular sieve is used for adsorption, the 3A molecular sieve is activated, so that the 3A molecular sieve has better adsorption capacity; because the 3A molecular sieve generates heat when adsorption is started, high-purity ethylene is introduced to perform pre-adsorption, so that the temperature of the 3A molecular sieve reaches a stable temperature, and then ethylene gas raw materials are introduced, thus the adsorption temperature can be stabilized, other impurities introduced due to ethylene reaction caused by unstable temperature are reduced, and impurity gas in the first adsorber can be discharged by introducing the high-purity ethylene before purification.
Preferably, step S11 is included between step S1 and step S2: detecting the water content of the ethylene gas discharged from the first adsorber, and if the water content is qualified, performing step S2; if the water content is not qualified, returning the ethylene gas to the first adsorber for re-adsorption to remove the water content.
After the water is removed by the adsorption of the first molecular sieve, the water content is detected first and then the subsequent process is carried out, so that the lower water content of the ethylene gas can be further ensured.
Preferably, the activated alumina used in step S2 is activated for 7-9 hours at a temperature of 200-250 ℃, then high purity ethylene is introduced into the second adsorber and pre-adsorption of the activated alumina is performed at a pressure of 0.1-0.5Mpa until the temperature of the second adsorber fluctuates within 10 ℃, and then step S2 is performed;
the adsorption pressure in the step S2 is 0.3-0.8Mpa, and the adsorption temperature is lower than 50 ℃.
The activated alumina can effectively adsorb and remove ethane, and has no reaction or little reaction with ethylene, thereby reducing the treatment amount of subsequent heavy component removal. Activating the activated alumina before using the activated alumina for adsorption, so that the activated alumina has better adsorption capacity; because the activated alumina generates heat when adsorption is started, high-purity ethylene is introduced to perform pre-adsorption, so that the temperature of the activated alumina is stabilized, ethylene gas is introduced after the temperature of the activated alumina is stabilized, the adsorption temperature can be stabilized, other impurities introduced due to ethylene reaction caused by unstable temperature are reduced, and the impurity gas in the second adsorber can be discharged after the high-purity ethylene is introduced before purification.
Preferably, the second molecular sieve is a modified 10X molecular sieve;
the preparation steps of the second molecular sieve comprise:
cu is added with 2+ Soaking the mixture with 10X molecular sieve powder for 5-10 hours according to the mass ratio of (1:30-1:15); or,
fe is added to 3+ Soaking the mixture with 10X molecular sieve powder for 5-10 hours according to the mass ratio of (1:43-1:21);
granulating and roasting to form modified 10X molecular sieve particles;
the second molecular sieve used in the step S3 is activated for 7-9 hours at the temperature of 300-400 ℃, then high-purity ethylene is introduced into the third adsorber, and pre-adsorption of the second molecular sieve is carried out under the pressure of 0.1-0.5Mpa until the temperature fluctuation of the third adsorber is within 10 ℃, and then the step S3 is carried out;
the adsorption pressure in the step S3 is 0.3-0.8Mpa, and the adsorption temperature is lower than 50 ℃.
The modified 10X molecular sieve can adsorb and remove heavy components; the modified 10X molecular sieve is formed by soaking, granulating and roasting iron or copper ions and 10X molecular sieve powder, and the iron or copper ions are used for modifying the 10X molecular sieve through experiments, so that heavy components can be effectively removed, the heavy components do not react with ethylene, and the modification cost is low.
Before the modified 10X molecular sieve is used for adsorption, the modified 10X molecular sieve is activated, so that the modified 10X molecular sieve has better adsorption capacity; because the modified 10X molecular sieve generates heat when adsorption is started, high-purity ethylene is introduced to perform pre-adsorption, so that the temperature of the modified 10X molecular sieve reaches a stable temperature, and then ethylene gas is introduced, thus the adsorption temperature can be stabilized, other impurities introduced due to ethylene reaction caused by unstable temperature are reduced, and the impurity gas in the third adsorber can be discharged by introducing the high-purity ethylene before purification.
Preferably, in step S4, the ethylene gas is fed into the first rectifying tower at a pressure of 0.2-0.6Mpa, a flow rate of 80-120L/min, a rectifying pressure of 0.1-0.5Mpa, and a rectifying temperature of-50 ℃ to-10 ℃.
The rectification pressure and the rectification temperature in the first rectification column are controlled so that gaseous ethylene and light component impurities can flow upwards and liquid heavy component impurities with boiling point higher than that of ethylene flow downwards, thereby removing heavy components.
Preferably, in step S4, a liquid level of at least 20% of the bottom of the first rectification column is maintained.
In the rectification process of the first rectification tower, the liquid level of at least 20% is reserved at the bottom of the first rectification tower, so that more heavy components are reserved at the bottom of the first rectification tower and do not rise, and the separation effect is improved.
Preferably, step S41 is included between step S4 and step S5: introducing ethylene gas flowing out of the top of the first rectifying tower into a fourth adsorber, wherein the second molecular sieve is arranged in the fourth adsorber, the second molecular sieve in the fourth adsorber adsorbs and removes heavy components in the ethylene gas, and then introducing the ethylene gas into the second rectifying tower.
The second molecular sieve in the fourth adsorber can adsorb and separate the ethylene gas flowing out from the top of the first rectifying tower, and the second molecular sieve adsorbs the heavy component again, so that the content of the heavy component is further reduced, the treatment capacity of the first rectifying tower is also reduced, the production efficiency is improved, and the purity of ethylene is improved.
Preferably, the rectification pressure in the step S5 is 0.2-0.55Mpa, and the rectification temperature is-50 ℃ to-10 ℃. The rectification pressure and the rectification temperature in the second rectification tower can be controlled by separating light components first and discharging the light components out of the second rectification tower, and then the high-purity ethylene finished product is obtained in the second rectification tower after the light components are discharged.
Preferably, in step S6, the filling is stopped when the liquid level of the second rectification column is low to at least 10%. And a certain liquid level is reserved in the second rectifying tower during filling, so that heavy component impurities are more left at the bottom of the second rectifying tower, the content of heavy components in the filled ethylene finished product is further reduced, and the purity of the ethylene finished product is improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to the structures shown in these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic flow diagram of an ethylene purification process of the present invention;
FIG. 2 is a schematic diagram of the structure of an ethylene purification system employing the present invention.
In the accompanying drawings: 1-first adsorber, 11-first feed inlet, 12-first discharge outlet, 13-first detection discharge outlet, 131-first valve, 14-return pipe, 2-second adsorber, 21-second feed inlet, 22-second discharge outlet, 3-third adsorber, 31-third feed inlet, 32-third discharge outlet, 4-first rectifying tower, 41-fourth feed inlet, 42-fourth discharge outlet, 43-first liquid level gauge, 44-gas mass flow controller, 5-second rectifying tower, 51-fifth feed inlet, 52-fifth discharge outlet, 53-second liquid level gauge, 6-fourth adsorber, 61-sixth feed inlet, 62-sixth discharge outlet, 7-membrane press.
The achievement of the objects, functional features and advantages of the present invention will be further described with reference to the accompanying drawings, in conjunction with the embodiments.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is evident that the embodiments described are only some, but not all embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the case where a directional instruction is involved in the embodiment of the present invention, the directional instruction is merely used to explain the relative positional relationship, movement condition, etc. between the components in a specific posture, and if the specific posture is changed, the directional instruction is changed accordingly.
In addition, if there is a description of "first", "second", etc. in the embodiments of the present invention, the description of "first", "second", etc. is for descriptive purposes only and is not to be construed as indicating or implying a relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include at least one such feature. In addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to base that the technical solutions can be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent and not within the scope of protection claimed in the present invention.
The produced ethylene gas raw material contains more impurities, the main impurity components are shown in the following table 1, and high-purity ethylene is obtained after purification treatment.
TABLE 1
As shown in fig. 1 and 2, a method for purifying ethylene comprises the steps of:
step S1: introducing an ethylene gas raw material into a first adsorber 1, wherein a first molecular sieve is arranged in the first adsorber 1, and the first molecular sieve adsorbs and removes moisture in the ethylene gas raw material.
The first molecular sieve is a 3A molecular sieve.
The first molecular sieve used in the step S1 is activated for 7-9 hours at the temperature of 300-400 ℃, then high-purity ethylene is introduced into the first adsorber 1 and pre-adsorption of the first molecular sieve is carried out under the pressure of 0.1-0.5Mpa until the temperature fluctuation of the first adsorber 1 is within 10 ℃, and then the step S1 is carried out;
the adsorption pressure in the step S1 is 0.3-0.8Mpa, and the adsorption temperature is lower than 50 ℃.
Before the 3A molecular sieve is used for adsorption, the 3A molecular sieve is activated, so that the 3A molecular sieve has better adsorption capacity; because the 3A molecular sieve generates heat when adsorption is started, high-purity ethylene is introduced to perform pre-adsorption, so that the temperature of the 3A molecular sieve reaches a stable temperature, and then ethylene gas raw materials are introduced, thus the adsorption temperature can be stabilized, other impurities introduced due to ethylene reaction caused by unstable temperature are reduced, and the impurity gas in the first adsorber 1 can be discharged by introducing the high-purity ethylene before purification. Through experiments, compared with other adsorbents, the 3A molecular sieve can effectively adsorb and remove moisture, and the experimental effects are shown in the following table 2:
| adsorbent and process for producing the same | Raw material H 2 O content (ppm) | H after adsorption 2 O content (ppm) |
| 3A molecular sieve | 8.5 | 0.4 |
| Activated carbon | 8.3 | 2.8 |
| Carbon molecular sieve | 8.4 | 2.5 |
| Alumina oxide | 8.1 | 2.2 |
| 4A molecular sieve | 8.5 | 0.8 |
| 5A molecular sieve | 8.2 | 1.2 |
| 10X molecular sieve | 8.2 | 0.9 |
| 13X molecular sieve | 8.5 | 1.7 |
TABLE 2
Step S11: detecting the water content of the ethylene gas discharged from the first adsorber 1, and if the water content is qualified, performing step S2; if the water content is not acceptable, the ethylene gas is returned to the first adsorber 1 to be adsorbed again to remove the water content. The pass value for the water content detected in this example was less than 0.1ppm.
After the water is removed by the adsorption of the first molecular sieve, the water content is detected first and then the subsequent process is carried out, so that the lower water content of the ethylene gas can be further ensured. Be equipped with first detection discharge gate 13 on the first adsorber 1, first detection discharge gate 13 locates the side of first discharge gate 12, and first detection discharge gate 13 is used for detecting the moisture content of ethylene gas. The first detection discharge port 13 can be provided with a first valve 131, and when detection is needed, part of ethylene gas can flow out for detection by opening the first valve 131. The ethylene purification system further comprises a return pipe 14, one end of the return pipe 14 is connected to the first detection discharge port 13, and the other end of the return pipe 14 is connected to the first feed port 11. When the detected water content is not qualified, the ethylene gas returns to the first feed inlet 11 through the return pipe 14 and enters the first adsorber 1 again to remove the water content.
Step S2: introducing the ethylene gas with the water removed into a second adsorber 2, wherein the second adsorber 2 is internally provided with activated alumina, and the activated alumina adsorbs and removes ethane in the ethylene gas.
Activating the activated alumina used in the step S2 for 7-9 hours at the temperature of 200-250 ℃, then introducing high-purity ethylene into the second adsorber 2, and pre-adsorbing the activated alumina at the pressure of 0.1-0.5Mpa until the temperature fluctuation of the second adsorber 2 is within 10 ℃, and then performing the step S2;
activating the activated alumina before using the activated alumina for adsorption, so that the activated alumina has better adsorption capacity; because the activated alumina generates heat when adsorption is started, high-purity ethylene is introduced to perform pre-adsorption, so that the temperature of the activated alumina is stabilized, ethylene gas is introduced after the temperature of the activated alumina is stabilized, the adsorption temperature can be stabilized, other impurities introduced due to ethylene reaction caused by unstable temperature are reduced, and the impurity gas in the second adsorber 2 can be discharged after the high-purity ethylene is introduced before purification.
The adsorption pressure in the step S2 is 0.3-0.8Mpa, and the adsorption temperature is lower than 50 ℃. The adsorption is facilitated under the environment of the adsorption pressure and the adsorption temperature, and the energy consumption is reasonable.
Activated alumina was used as a control for other adsorbents. The contents of some impurity components in the raw materials before adsorption are shown in table 3 below:
TABLE 3 Table 3
Under the same conditions, each group of raw materials and adsorbents were tested, and the content of the adsorbed components was as shown in table 4 below:
TABLE 4 Table 4
From the test data in tables 3 and 4, it is evident that the amount of ethane adsorbed by activated alumina is the most significant, and ethane can be effectively adsorbed and removed with less methane and other impurity hydrocarbons being produced. The adsorption of the activated carbon and the carbon molecular sieve to ethane is less; the 3A molecular sieve, the 4A molecular sieve and the 13X molecular sieve adsorb ethane in an amount less than that of activated alumina, and the 13X molecular sieve also increases the amount of methane; the adsorption capacity of the 5A molecular sieve to ethane is also good, but the content of hydrocarbon of other impurities is increased; the amount of methane and other impurities, hydrocarbon, increases after adsorption, indicating that a certain amount of decomposition occurs by the reaction of ethylene, reducing the ethylene content.
Step S3: and introducing the ethylene gas from which the ethane is removed into a third adsorber 3, wherein a second molecular sieve is arranged in the third adsorber 3, and the second molecular sieve adsorbs and removes heavy components in the ethylene gas.
The second molecular sieve is a modified 10X molecular sieve. The modified 10X molecular sieve may be modified using copper ions or iron ions.
The preparation steps of the second molecular sieve comprise:
the modified 10X molecular sieve using copper ions was: cu is added with 2+ Soaking the mixture with 10X molecular sieve powder for 5-10 hours according to the mass ratio of (1:30-1:15);
the modified 10X molecular sieve using iron ions was: fe is added to 3+ Soaking the mixture in 10X molecular sieve powder in the mass ratio of (1:43-1:21) for 5-10 hours.
And after soaking, granulating and roasting to form modified 10X molecular sieve particles.
The modified 10X molecular sieve is formed by soaking, granulating and roasting 10X molecular sieve powder with iron ions or copper ions at 300-500 ℃. Specifically, the copper nitrate powder and the 10X molecular sieve powder can be weighed in the preparation process, the mass ratio is about (1:10-1:5), and Cu is obtained after conversion 2+ And 10X molecular sieve powder in the mass ratio of (1:30-1:15), and then adding water for soaking.
The second molecular sieve used in the step S3 is activated for 7-9 hours at the temperature of 300-400 ℃, then high-purity ethylene is introduced into the third adsorber 3, and pre-adsorption of the second molecular sieve is carried out under the pressure of 0.1-0.5Mpa until the temperature fluctuation of the third adsorber 3 is within 10 ℃, and then the step S3 is carried out. Before the modified 10X molecular sieve is used for adsorption, the modified 10X molecular sieve is activated, so that the modified 10X molecular sieve has better adsorption capacity.
Because the modified 10X molecular sieve generates heat when adsorption is started, high-purity ethylene is introduced to perform pre-adsorption, so that the temperature of the modified 10X molecular sieve reaches a stable temperature, and then ethylene gas is introduced, thus the adsorption temperature can be stabilized, other impurities introduced due to ethylene reaction caused by unstable temperature are reduced, and the impurity gas in the third adsorber 3 can be discharged by introducing the high-purity ethylene before purification.
The adsorption pressure in the step S3 is 0.3-0.8Mpa, and the adsorption temperature is lower than 50 ℃.
The modified 10X molecular sieve was used as a comparison with other adsorbents. The contents of heavy components C3, C4 in the raw material before adsorption are shown in Table 5 below, and the raw material was used to test different adsorbents under the same conditions.
| C3 | C4 |
| 58ppm | 45ppm |
TABLE 5
Example 1:
modified 10X molecular sieves using copper ions were modified with the same mass of 10X molecular sieve to different mass ratios of copper ions and the test results are shown in table 6 below.
| Adsorbent and process for producing the same | C3 content (ppm) | C4 content (ppm) |
| Cu 2+ The mass ratio of the catalyst to the 10X molecular sieve is 1:30 | 2.5 | 1.6 |
| Cu 2+ The mass ratio of the molecular sieve to the 10X molecular sieve is 1:22 | 2.0 | 1.8 |
| Cu 2+ The mass ratio of the molecular sieve to the 10X molecular sieve is 1:15 | 2.3 | 1.5 |
| Cu 2+ The mass ratio of the molecular sieve to the 10X molecular sieve is 1:6 | 15 | 10.8 |
| Cu 2+ The mass ratio of the molecular sieve to the 10X molecular sieve is 1:45 | 7.8 | 6.7 |
TABLE 6
As can be seen from the test results in Table 6, cu 2+ When the mass ratio of the catalyst to the 10X molecular sieve is (1:30-1:15), the effect of adsorbing C3 and C4 is better.
Example 2:
modified 10X molecular sieves using iron ions were modified with the same mass of 10X molecular sieves and different mass ratios of copper ions, the mass of 10X molecular sieves was the same as in example 1, and the test results were as shown in table 7 below.
| Adsorbent and process for producing the same | C3 content (ppm) | C4 content (ppm) |
| Fe 3+ The mass ratio of the molecular sieve to the 10X molecular sieve is 1:43 | 2.3 | 1.8 |
| Fe 3+ The mass ratio of the catalyst to the 10X molecular sieve is 1:30 | 2.5 | 1.6 |
| Fe 3+ The mass ratio of the molecular sieve to the 10X molecular sieve is 1:21 | 1.8 | 2.0 |
| Fe 3+ The mass ratio of the molecular sieve to the 10X molecular sieve is 1:10 | 12 | 15 |
| Fe 3+ The mass ratio of the catalyst to the 10X molecular sieve is 1:60 | 9.4 | 8.8 |
TABLE 7
As is clear from the test results in Table 7, in Fe 3+ When the mass ratio of the catalyst to the 10X molecular sieve is (1:43-1:21), the effect of adsorbing C3 and C4 is better.
Comparative example 1:
the same mass of 10X, 3A, 4A, 5A, and 13X molecular sieves were used, and the mass was the same as that of the 10X molecular sieve in example 1, and the test results were as shown in table 8 below.
| Adsorbent and process for producing the same | C3 content (ppm) | C4 content (ppm) |
| 10X molecular sieve | 8.4 | 6.5 |
| 3A molecular sieve | 25 | 28 |
| 4A molecular sieve | 23 | 25 |
| 5A molecular sieve | 62 | 48 |
| 13X molecular sieve | 35 | 42 |
TABLE 8
As can be seen from the test results in Table 8, the 10X molecular sieve has a certain adsorption effect on the heavy components, but the adsorption effect is inferior to Cu 2+ The mass ratio of the catalyst to the 10X molecular sieve is (1:30-1:15) and Fe 3+ The mass ratio of the modified 10X molecular sieve to the 10X molecular sieve is (1:43-1:21). And the adsorption effect of other adsorbents is poor.
Comparative example 2:
modified 10X molecular sieves using silver ions were modified with the same mass of 10X molecular sieve and different mass ratios of silver ions, the mass of 10X molecular sieve was the same as in example 1, and the test results were as shown in table 9 below.
| Adsorbent and process for producing the same | C3 content (ppm) | C4 content (ppm) |
| Ag + The mass ratio of the catalyst to the 10X molecular sieve is 1:30 | 5.4 | 3.8 |
| Ag + The mass ratio of the molecular sieve to the 10X molecular sieve is 1:22 | 6.8 | 4.5 |
| Ag + The mass ratio of the molecular sieve to the 10X molecular sieve is 1:15 | 5.2 | 4.2 |
| Ag + The mass ratio of the molecular sieve to the 10X molecular sieve is 1:6 | 26 | 18 |
| Ag + The mass ratio of the molecular sieve to the 10X molecular sieve is 1:45 | 15 | 20 |
TABLE 9
As can be seen from the test results in Table 9, the modified 10X molecular sieve of silver ions has a certain adsorption effect on heavy components, but the adsorption effect is inferior to that of the modified 10X molecular sieves of copper ions and iron ions.
Comparative example 3:
the 4A molecular sieve and the 13X molecular sieve were modified with copper ions and iron ions, and the molecular sieve mass was the same as the 10X molecular sieve mass of example 1, and the test results are shown in table 10 below.
| Adsorbent and process for producing the same | C3 content (ppm) | C4 content (ppm) |
| Cu 2+ The mass ratio of the catalyst to the 4A molecular sieve is 1:30 | 25 | 28 |
| Cu 2+ The mass ratio of the catalyst to the 13X molecular sieve is 1:30 | 32 | 38 |
| Fe 3+ Mass ratio to 4A molecular sieve 1:43 | 28 | 32 |
| Fe 3+ Mass ratio to 13X molecular sieve 1:43 | 26 | 30 |
Table 10
From the test results in table 10, it is clear that the effect of adsorbing heavy components when copper ions and iron ions are modified with other molecular sieves is generally inferior to that of modifying 10X molecular sieves.
Therefore, according to the above experiments, it is known that the modification of 10X molecular sieves with iron or copper ions can effectively remove heavy components, has less effect on ethylene, and has lower modification cost using iron or copper ions.
Step S4: and introducing ethylene gas adsorbed by the second molecular sieve into a first rectifying tower 4 for rectifying treatment, and separating and removing heavy components in the ethylene gas by the first rectifying tower 4.
In the step S4, the feeding pressure of ethylene gas into the first rectifying tower 4 is 0.2-0.6Mpa, the flow is 80-120L/min, the rectifying pressure is 0.1-0.5Mpa, and the rectifying temperature is-50 ℃ to-10 ℃.
The rectification pressure and the rectification temperature in the first rectification column 4 are controlled so that gaseous ethylene and light component impurities flow upward and liquid heavy component impurities having a boiling point higher than that of ethylene flow downward, thereby removing heavy components. The fourth feed inlet 41 is provided with a gas mass flow controller 44, and the gas mass flow controller 44 is used for controlling the flow of ethylene gas entering the first rectifying tower 4, so that the rectifying amount and the rectifying speed can be conveniently controlled.
In some embodiments, a liquid level of at least 20% of the bottom of the first rectification column 4 is maintained in step S4.
In the rectification process of the first rectification column 4, the liquid level of at least 20% is reserved at the bottom of the first rectification column 4, so that more heavy components are reserved at the bottom of the first rectification column 4 and do not rise, and the separation effect is improved. The first rectifying tower 4 is provided with a first liquid level meter 43, and the liquid level in the first rectifying tower 4 can be measured by the first liquid level meter 43.
In some embodiments, step S41 is further included: introducing ethylene gas flowing out from the top of the first rectifying tower 4 into a fourth adsorber 6, wherein a second molecular sieve is arranged in the fourth adsorber 6, the second molecular sieve in the fourth adsorber 6 adsorbs and removes heavy components in the ethylene gas, and then introducing the ethylene gas into a second rectifying tower 5.
The fourth adsorber 6 is provided with a sixth feed port 61 and a sixth discharge port 62, the sixth feed port 61 being in communication with the fourth discharge port 42 and the sixth discharge port 62 being in communication with the fifth feed port 51.
The second molecular sieve in the fourth adsorber 6 can adsorb and separate the ethylene gas flowing out from the top of the first rectifying tower 4, and the second molecular sieve adsorbs the heavy component again, so that the content of the heavy component is further reduced, the treatment capacity of the first rectifying tower 4 is reduced, the production efficiency is improved, and the purity of ethylene is improved.
Step S5: and introducing the ethylene gas flowing out of the top of the first rectifying tower 4 into a second rectifying tower 5 for rectifying treatment, and separating and removing light components in the ethylene gas by the second rectifying tower 5.
The rectification pressure in the step S5 is 0.2-0.55Mpa, and the rectification temperature is-50 ℃ to-10 ℃.
The rectification pressure and the rectification temperature in the second rectification tower 5 can be controlled by separating light components first and discharging the light components out of the second rectification tower 5, and then obtaining high-purity ethylene finished products in the second rectification tower 5 after discharging the light components.
Step S6: discharging light components from the top of the second rectifying tower 5, detecting the content of the light components in the gas flowing out from the top of the second rectifying tower 5, and filling ethylene finished products from the top of the second rectifying tower 5 outwards when detecting that the content of the light components is reduced to be qualified.
In some embodiments, in step S6, the filling is stopped when the liquid level of the second rectification column 5 is low to at least 10%. The second rectifying tower 5 is provided with a second liquid level meter 53, and the second liquid level meter 53 is used for measuring the liquid level at the bottom of the second rectifying tower 5. When the ethylene product is filled, a certain liquid level is reserved in the second rectifying tower 5, so that heavy component impurities are more reserved at the bottom of the second rectifying tower 5, the content of heavy components in the filled ethylene product is further reduced, and the purity of the ethylene product is improved.
The final high purity ethylene product obtained by the purification method has the components shown in Table 11, and can be applied to the process production using high purity ethylene.
| Composition of the components | Content of |
| Ethylene (C) 2 H 4 ) (volume fraction)/10 -2 | ≥99.999 |
| Oxygen (O) 2 ) Content (volume fraction)/l 0 -6 | ≤1.0 |
| Nitrogen (N) 2 ) Content (volume fraction)/l 0 -6 | ≤1.0 |
| Carbon monoxide (CO) content (volume fraction)/l 0 -6 | ≤1.0 |
| Carbon dioxide (CO) 2 ) Content (volume fraction)/l 0 -6 | ≤0.5 |
| Ethane (C) 2 H 6 ) Content (volume fraction)/l 0 -6 | ≤4.0 |
| Other hydrocarbon content (volume fraction)/10 -6 | ≤4.0 |
| Acetylene (C) 2 H 2 ) Content (volume fraction)/10 -6 | ≤0.5 |
| Water (H) 2 O) content (volume fraction)/10 -6 | ≤0.5 |
| Total impurity content (volume fraction)/10 -6 | ≤10.0 |
TABLE 11
The ethylene gas raw material is purified by a first absorber 1, a second absorber 2, a third absorber 3, a first rectifying tower 4 and a second rectifying tower 5 in sequence to obtain an ethylene finished product with higher purity.
The technology firstly utilizes a first molecular sieve to adsorb moisture; then the activated alumina is utilized to adsorb ethane, and the test shows that the activated alumina can effectively adsorb and remove ethane; then the second molecular sieve is utilized to adsorb heavy components with boiling point higher than that of ethylene; then the heavy components are rectified and separated by the first rectifying tower 4, the heavy components are left at the bottom of the first rectifying tower 4, and ethylene and light components are discharged from the top of the first rectifying tower 4; then separating light components by using a second rectifying tower 5, and discharging the light components from the top of the second rectifying tower 5; and then detecting the content of light components in the gas discharged from the top of the second rectifying tower 5, and when the content of the light components is detected to be reduced to be qualified, indicating that the light components contained in the second rectifying tower 5 are less, the ethylene in the second rectifying tower 5 is higher in purity, the ethylene with higher purity can be filled outwards from the top of the second rectifying tower 5, and the heavy components are further separated from the bottom of the second rectifying tower 5, so that the ethylene finished product filled from the top of the second rectifying tower 5 is higher in purity.
The technology can firstly remove part of impurities in an adsorption separation mode, reduce impurity components entering the first rectifying tower 4 and the second rectifying tower 5, so that the rectifying speed can be increased, and the production efficiency can be improved while the purifying effect is improved; and the effect of removing heavy components by using the activated alumina, the second molecular sieve, the first rectifying tower 4 and the second rectifying tower 5 is better, the ethylene is more stable in the purification process, less introduced impurities are generated, and the purity of the obtained ethylene is higher.
As shown in fig. 2, an ethylene purification system using the above-described ethylene purification method comprises a first adsorber 1, a second adsorber 2, a third adsorber 3, a first rectifying column 4, and a second rectifying column 5, which are connected in this order.
The first adsorber 1 is provided with a first feed inlet 11 and a first discharge outlet 12, and a first molecular sieve is arranged in the first adsorber 1 and is used for adsorbing moisture. The second adsorber 2 is provided with a second feed inlet 21 and a second discharge outlet 22, the second feed inlet 21 is communicated with the first discharge outlet 12, and activated alumina is arranged in the second adsorber 2 and used for adsorbing ethane. The third adsorber 3 is provided with a third feed inlet 31 and a third discharge outlet 32, the third feed inlet 31 is communicated with the second discharge outlet 22, and a second molecular sieve is arranged in the third adsorber 3 and is used for adsorbing heavy components. The first rectifying tower 4 is provided with a fourth feed port 41 and a fourth discharge port 42, the fourth feed port 41 is arranged in the middle of the first rectifying tower 4, the fourth discharge port 42 is arranged at the top of the first rectifying tower 4, and the fourth feed port 41 is communicated with the third discharge port 32. The second rectifying tower 5 is provided with a fifth feed inlet 51 and a fifth discharge outlet 52, the fifth feed inlet 51 is arranged in the middle of the second rectifying tower 5, the fifth discharge outlet 52 is arranged at the top of the second rectifying tower 5, and the fifth feed inlet 51 is communicated with the fourth discharge outlet 42. At the fifth outlet 52, a film press 7 is connected, which can be filled into an external container under pressure.
And separating light components by using the second rectifying tower 5, separating the light components, discharging the light components from a fifth discharge hole 52 at the top of the second rectifying tower 5, and obtaining an ethylene finished product with higher purity in the second rectifying tower 5. The content of light components in the discharged gas can be detected from the fifth discharge hole 52 during rectification, and when the content of the light components in the gas discharged from the fifth discharge hole 52 meets the requirements, a high-purity ethylene finished product can be discharged from the fifth discharge hole 52, and heavy components can be separated and left at the bottom of the second rectifying tower 5 to further remove the heavy components.
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the invention, and all equivalent structural changes made by the description of the present invention and the accompanying drawings or direct/indirect application in other related technical fields are included in the scope of the invention.
Claims (8)
1. A process for purifying ethylene comprising the steps of:
s1: introducing an ethylene gas raw material into a first adsorber, wherein a first molecular sieve is arranged in the first adsorber, and the first molecular sieve adsorbs and removes water in the ethylene gas raw material;
s2: introducing the ethylene gas with the water removed into a second adsorber, wherein the second adsorber is internally provided with activated alumina, and the activated alumina adsorbs and removes ethane in the ethylene gas;
s3: introducing ethylene gas from which ethane is removed into a third adsorber, wherein a second molecular sieve is arranged in the third adsorber, and the second molecular sieve adsorbs and removes heavy components in the ethylene gas;
s4: introducing ethylene gas adsorbed by the second molecular sieve into a first rectifying tower for rectification treatment, and separating and removing heavy components in the ethylene gas by the first rectifying tower;
s5: introducing ethylene gas flowing out from the top of the first rectifying tower into a second rectifying tower for rectification treatment, and separating and removing light components in the ethylene gas by the second rectifying tower;
s6: discharging light components from the top of the second rectifying tower, detecting the content of the light components in the gas flowing out from the top of the second rectifying tower, and filling ethylene finished products from the top of the second rectifying tower outwards when the content of the light components is detected to be reduced to be qualified;
the first molecular sieve is a 3A molecular sieve;
the first molecular sieve used in the step S1 is activated for 7-9 hours at the temperature of 300-400 ℃, then high-purity ethylene is introduced into the first adsorber, and pre-adsorption of the first molecular sieve is carried out under the pressure of 0.1-0.5Mpa until the temperature fluctuation of the first adsorber is within 10 ℃, and then the step S1 is carried out;
the adsorption pressure in the step S1 is 0.3-0.8Mpa, and the adsorption temperature is lower than 50 ℃;
the second molecular sieve is a modified 10X molecular sieve;
the preparation steps of the second molecular sieve comprise:
cu is added with 2+ Soaking the mixture with 10X molecular sieve powder for 5-10 hours according to the mass ratio of 1:30-1:15; or,
fe is added to 3+ Soaking the powder and 10X molecular sieve powder for 5-10 hours according to the mass ratio of 1:43-1:21;
granulating and roasting to form modified 10X molecular sieve particles;
the second molecular sieve used in the step S3 is activated for 7-9 hours at the temperature of 300-400 ℃, then high-purity ethylene is introduced into the third adsorber, and pre-adsorption of the second molecular sieve is carried out under the pressure of 0.1-0.5Mpa until the temperature fluctuation of the third adsorber is within 10 ℃, and then the step S3 is carried out;
the adsorption pressure in the step S3 is 0.3-0.8Mpa, and the adsorption temperature is lower than 50 ℃.
2. The ethylene purification process according to claim 1, characterized in that it comprises, between step S1 and step S2, step S11: detecting the water content of the ethylene gas discharged from the first adsorber, and if the water content is qualified, performing step S2; if the water content is not qualified, returning the ethylene gas to the first adsorber for re-adsorption to remove the water content.
3. The ethylene purification process according to claim 1, wherein the activated alumina used in step S2 is activated for 7-9 hours at a temperature of 200-250 ℃, and then high purity ethylene is introduced into the second adsorber and pre-adsorption of the activated alumina is performed at a pressure of 0.1-0.5Mpa until the temperature of the second adsorber fluctuates within 10 ℃, and step S2 is performed;
the adsorption pressure in the step S2 is 0.3-0.8Mpa, and the adsorption temperature is lower than 50 ℃.
4. The method for purifying ethylene according to claim 1, wherein the ethylene gas is fed into the first rectifying column at a feed pressure of 0.2 to 0.6Mpa, a flow rate of 80 to 120L/min, a rectifying pressure of 0.1 to 0.5Mpa, and a rectifying temperature of-50 ℃ to-10 ℃ in step S4.
5. The ethylene purification process according to claim 1, characterized in that in step S4 a liquid level of at least 20% of the bottom of the first rectification column is maintained.
6. The ethylene purification process according to claim 1, characterized in that it comprises step S41 between step S4 and step S5: introducing ethylene gas flowing out of the top of the first rectifying tower into a fourth adsorber, wherein the second molecular sieve is arranged in the fourth adsorber, the second molecular sieve in the fourth adsorber adsorbs and removes heavy components in the ethylene gas, and then introducing the ethylene gas into the second rectifying tower.
7. The method for purifying ethylene according to claim 1, wherein the rectification pressure in the step S5 is 0.2 to 0.55MPa, and the rectification temperature is-50 ℃ to-10 ℃.
8. The ethylene purification method according to claim 1, wherein in step S6, the charging is stopped when the liquid level of the second rectification column is as low as 10%.
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Application publication date: 20220322 Assignee: JIANGXI HUATE ELECTRONIC CHEMICALS CO.,LTD. Assignor: GUANGDONG HUATE GASES Co.,Ltd. Contract record no.: X2024980004229 Denomination of invention: A method for ethylene purification Granted publication date: 20231222 License type: Common License Record date: 20240411 |
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