CN115491223A - Regeneration method of adsorbent for removing oxygen-containing compounds in isoparaffin - Google Patents
Regeneration method of adsorbent for removing oxygen-containing compounds in isoparaffin Download PDFInfo
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- CN115491223A CN115491223A CN202211296744.3A CN202211296744A CN115491223A CN 115491223 A CN115491223 A CN 115491223A CN 202211296744 A CN202211296744 A CN 202211296744A CN 115491223 A CN115491223 A CN 115491223A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
- C10G25/003—Specific sorbent material, not covered by C10G25/02 or C10G25/03
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G25/00—Refining of hydrocarbon oils in the absence of hydrogen, with solid sorbents
- C10G25/12—Recovery of used adsorbent
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- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a regeneration method of an adsorbent for removing oxygen-containing compounds in isoparaffin. The method comprises the following steps: purging: purging the solid adsorbent to be regenerated with at least one dry inert gas; regeneration: after purging is finished, introducing a regenerant for regeneration, wherein the volume ratio of the regenerant to the solid adsorbent is (5); and (3) drying: and after the regeneration is finished, drying the solid adsorbent. The regeneration method of the invention can completely regenerate the adsorbent and improve the stability of the adsorbent.
Description
Technical Field
The invention relates to the field of petroleum processing, in particular to a regeneration method of an adsorbent for removing oxygen-containing compounds in isoparaffin.
Background
Petroleum hydrocarbon solvents generally comprise four classes of compounds: normal paraffins, isoparaffins, naphthenes and aromatics. The influence of the four chemical compounds on the properties of the solvent oil is respectively characterized. The properties of hydrocarbon solvents are mainly odor, toxicity, solubility, low temperature performance and suitable distillation range. Aromatic hydrocarbon is a main source of smell and toxicity, is a compound which is removed as far as possible from a petroleum hydrocarbon solvent, and among the other three compounds, naphthenic hydrocarbon has better solubility and low-temperature performance but larger smell, is a main smell source of the petroleum hydrocarbon solvent except the aromatic hydrocarbon, normal alkane has less smell but poorer solubility and low-temperature performance, isoparaffin has solubility similar to that of the naphthenic hydrocarbon, good low-temperature performance and less smell, and is the hydrocarbon solvent with the best comprehensive performance. The isoparaffin solvent can be widely applied to the application fields of paint, printing ink, coating, cosmetics, metal processing, peroxide dispersant and the like.
The isoalkane solvent is produced by utilizing isoalkene for hydrogenation saturation, so that higher economic benefit can be obtained. However, the isoparaffin after hydrogenation contains trace amount of oxides, generally ethers, alcohols and other oxygen-containing compounds, which cause a great odor of the oil product. Therefore, the removal of the oxide in the isoparaffin is needed, wherein the adsorption method has the advantages of deep impurity removal, regeneration, low pollution and the like, and is suitable for the removal of the oxygen-containing compound, the adsorbent is the key point of the adsorption process, and the development of the adsorbent with high adsorption capacity and easy regeneration is the key point of the adsorption process in industrial application and popularization.
At present, the research on the adsorbent regeneration process is mainly applied to the regeneration of a dehydration and desulfurization adsorbent and the regeneration of an adsorbent in Fischer-Tropsch synthetic oil, and no method for regenerating the adsorbent in isoparaffin exists; the conventional adsorbent regeneration method has great limitations, such as that the roasting process needs great heat supply and is not beneficial to industrialized operation; the vacuuming method needs a compressor unit, and the maintenance cost is high.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a regeneration method of an adsorbent for removing oxygen-containing compounds in isoparaffin, which can completely regenerate the adsorbent and improve the stability of the adsorbent.
In order to achieve the purpose, the invention adopts the technical scheme that: a regeneration method of an adsorbent for removing oxygen-containing compounds in isoparaffin comprises the following steps:
purging: purging the solid adsorbent to be regenerated with at least one dry inert gas;
regeneration: after purging is finished, introducing a regenerant for regeneration, wherein the volume ratio of the regenerant to the solid adsorbent is 5-15;
and (3) drying: and after the regeneration is finished, drying the solid adsorbent.
The method is used for regenerating the adsorbent for removing the oxygen-containing compounds in the isoparaffin by combining purging with regeneration of the regenerant, and can completely regenerate the adsorbent and improve the stability of the adsorbent by selecting the specific regenerant and controlling the volume ratio of the regenerant to the adsorbent. When the volume ratio of the regenerant to the solid adsorbent is less than 5; when the volume ratio of the regenerant to the solid adsorbent is in the range of 5 to 1, 1 to 15, the regeneration effect of the adsorbent tends to increase first and then decrease as the volume ratio of the regenerant to the solid adsorbent increases.
Preferably, the parameters of the purge are: the purging temperature is 50-80 ℃, and the purging time is 4-8 h. For example, the purging temperature is 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃ and the like, and the purging time is 4h, 4.5h, 5h, 5.5h, 6h, 6.5h, 7h, 7.5h, 8h and the like.
Preferably, the volume space velocity of the inert gas is 100 to 400h -1 . For example, the inert gas has a volume space velocity of 100h -1 、150h -1 、200h -1 、250h -1 、300h -1 、350h -1 、400h -1 And the like.
The regeneration effect of the adsorbent is improved by adjusting parameters in the purging process. The regeneration effect of the adsorbent is gradually increased along with the increase of the purging temperature and the volume space velocity of the inert gas; the regeneration effect of the adsorbent is gradually improved along with the prolonging of the purging time.
Preferably, the parameters of the regeneration are: the regeneration temperature is 80-120 ℃, and the regeneration pressure is 0.2-0.3 MPa. For example, the regeneration temperature is 80 ℃, 85 ℃, 90 ℃, 95 ℃, 100 ℃, 105 ℃, 110 ℃, 115 ℃, 120 ℃ and the like; the regeneration pressure is 0.2MPa, 0.21MPa, 0.22MPa, 0.23MPa, 0.24MPa, 0.25MPa, 0.26MPa, 0.27MPa, 0.28MPa, 0.29MPa, 0.30MPa, etc.
Preferably, the mass space velocity of the regenerant is 1.0-5.0 h -1 . For example, the mass space velocity of the regenerant is 1.0h -1 、1.5h -1 、2.0h -1 、2.5h -1 、3.0h -1 、3.5h -1 、4.0h -1 、4.5h -1 、5.0h -1 And the like.
The parameters of regeneration affect the effectiveness of the regeneration of the adsorbent. With the increase of the regeneration temperature, the regeneration effect of the adsorbent is firstly increased and then reduced, and the regeneration temperature of the invention is lower, thereby avoiding the problem that the adsorbent is easy to deposit carbon in the adsorption process; as the mass space velocity of the regenerant is increased, the regeneration effect of the adsorbent is increased and then decreased.
Preferably, the drying parameters are: the drying temperature is 150-200 ℃, and the drying pressure is 0.5-1.0 MPa.
Preferably, the inert gas is one of nitrogen, argon and helium.
Preferably, the solid adsorbent is at least one of silica gel, activated alumina and molecular sieve.
Preferably, the regeneration process is carried out in situ in an adsorption column for removing oxygenates from isoparaffins.
Compared with the prior art, the invention has the beneficial effects that: the method is used for regenerating the adsorbent for removing the oxygen-containing compounds in the isoparaffin by combining purging with regeneration of the regenerant, and can completely regenerate the adsorbent and improve the stability of the adsorbent by selecting the specific regenerant and controlling the volume ratio of the regenerant to the adsorbent.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
The Fresh adsorbent used in the invention is recorded as Fresh, and the solid adsorbent is silica gel and is used for adsorbing and removing oxygen-containing compounds from isoparaffin. Based on the analysis of the composition of the provided isoparaffin,the content of the oxygen-containing compound was 0.271wt%. The adsorption evaluation conditions were: at 0.2MPa and 50 ℃ for 1h -1 The mass space velocity of (3) and the loading amount of the adsorbent is 80mL; after 60 times of the volume of the adsorbent is treated, the adsorbent is saturated, the adsorbent needs to be regenerated after being deactivated, and the deactivated adsorbent is marked as A-1.
Example 1
The embodiment provides a regeneration method of an adsorbent for removing oxygen-containing compounds in isoparaffin, which comprises the following steps:
purging: at 50 ℃ and the gas volume space velocity of 200h -1 Under the condition of normal pressure, blowing the deactivated adsorbent A-1 in the adsorption column by using nitrogen for 6 hours;
regeneration: after purging is finished, the temperature of the adsorption column filled with the inactivation adsorbent is raised to 100 ℃ by using an external heating belt, and then ethanol is introduced, wherein the pressure is 0.2MPa, and the mass space velocity of the ethanol is 3.0h -1 Under conditions of (1), wherein the volume ratio of ethanol to deactivated adsorbent A-1 is 10;
and (3) drying: and after the regeneration is finished, drying the regenerated adsorbent at the temperature of 180 ℃ and under the pressure of 1.0MPa to obtain the regenerated and activated adsorbent R-1.
Example 2
This example is similar to example 1 except that the inert gas in this example is helium.
Example 3
This example is similar to example 1 except that the regenerant in this example was water.
Example 4
This example is similar to example 1 except that the regenerant in this example was methanol.
Example 5
This example is similar to example 1 except that the purge temperature in this example is 65 ℃.
Example 6
This example is similar to example 1 except that the purge temperature in this example is 80 ℃.
Example 7
This example is similar to example 1 except that the volume space velocity of nitrogen in this example is 100h -1 。
Example 8
This example is similar to example 1, except that the volume space velocity of nitrogen in this example is 400h -1 。
Example 9
This example is similar to example 1 except that the purge time in this example is 4 hours.
Example 10
This example is similar to example 1 except that the purge time in this example is 8 hours.
Example 11
This example is similar to example 1 except that the regeneration temperature in this example is 80 ℃.
Example 12
This example is similar to example 1 except that the regeneration temperature in this example is 120 ℃.
Example 13
This example is similar to example 1 except that the regeneration pressure in this example is 0.5MPa.
Example 14
This example is similar to example 1 except that the regeneration pressure in this example is 1.0MPa.
Example 15
This example is similar to example 1 except that the mass space velocity of ethanol in this example is 1.0h -1 。
Example 16
This example is similar to example 1, except that the mass space velocity of ethanol in this example is 2.0h -1 。
Example 17
This example is similar to example 1, except that the mass space velocity of ethanol in this example is 5.0h -1 。
Example 18
This example is similar to example 1 except that the volume ratio of ethanol to deactivated adsorbent A-1 in this example is 5.
Example 19
This example is similar to example 1 except that the volume ratio of ethanol to deactivated adsorbent A-1 in this example is 15.
Example 20
This example is similar to example 1 except that the volume ratio of ethanol to deactivated adsorbent A-1 in this example is 8.
Example 21
This example is similar to example 1 except that the volume ratio of ethanol to deactivated adsorbent A-1 in this example is 12.
Example 22
This example is similar to example 1 except that the drying temperature in this example is 150 ℃.
Example 23
This example is similar to example 1 except that the drying temperature in this example is 200 ℃.
Example 24
This example is similar to example 1 except that the drying pressure in this example is 0.5MPa.
Example 25
This example is similar to example 1 except that the drying pressure in this example is 0.8MPa.
Comparative example 1
This comparative example is similar to example 1 except that the regeneration step is absent for this pair.
Comparative example 2
This comparative example is similar to example 1 except that the purge step is absent from this pair of examples.
Effects of the invention
The evaluation conditions for the regenerated activated adsorbent were as follows: at 2.0MPa and 35 ℃ for 2h -1 The liquid volume space velocity of (3) and the loading of the adsorbent was 2mL, and the adsorption experiment was carried out for 72 hours.Table 1 shows the adsorption performance of the regenerated activated adsorbent according to different regeneration methods.
TABLE 1
As can be seen from table 1, the regeneration method of the present application can completely regenerate and activate the adsorbent, and the activity of the regenerated and activated adsorbent is high.
Effect example 2
This effect example tests the stability of the adsorbent regeneration effect.
The test method is as follows:
the Fresh adsorbent is marked as Fresh, and the solid adsorbent is silica gel and is used for adsorbing and removing oxygen-containing compounds from isoparaffin. The content of oxygenates was 0.271wt% based on the compositional analysis of the isoparaffin provided. The adsorption evaluation conditions were: at 0.2MPa and 50 ℃ for 1h -1 The mass space velocity of (3) and the loading amount of the adsorbent is 80mL; after 60 times of the volume of the adsorbent is treated, the adsorbent is saturated, the adsorbent needs to be regenerated after being deactivated, and the deactivated adsorbent is marked as A-1. For the deactivated adsorbent noted A-1, regeneration was performed using the regeneration method of example 1 to obtain regenerated adsorbent RB-1; repeating the adsorption-regeneration steps for 5 times; the regeneration effect of the regenerated adsorbent obtained is shown in table 2.
TABLE 2
| Adsorbent and process for producing the same | Oxide adsorption content/wt% |
| Fresh | 16.260 |
| 1 regeneration | 16.135 |
| 2 regeneration | 16.130 |
| 3 times of regeneration | 16.126 |
| 4 regeneration times | 16.109 |
| 5 regenerations | 16.012 |
As can be seen from Table 2, the adsorbent still has high activity after 5 times of regeneration, which shows that the method of the present invention can improve the stability of the regeneration activation of the adsorbent.
Finally, it should be noted that the above embodiments are intended to illustrate the technical solutions of the present invention and not to limit the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (9)
1. A regeneration method of an adsorbent for removing oxygen-containing compounds in isoparaffin is characterized by comprising the following steps:
purging: purging the solid adsorbent to be regenerated with at least one dry inert gas;
regeneration: after purging is finished, introducing a regenerant for regeneration, wherein the volume ratio of the regenerant to the solid adsorbent is (5);
and (3) drying: and after the regeneration is finished, drying the solid adsorbent.
2. The regeneration method of claim 1, wherein the parameters of the purge are: the purging temperature is 50-80 ℃, and the purging time is 4-8 h.
3. The regeneration process of claim 1, wherein the inert gas has a volumetric space velocity of 100 to 400h -1 。
4. Regeneration method according to claim 1, characterised in that the parameters of the regeneration are: the regeneration temperature is 80-120 ℃, and the regeneration pressure is 0.2-0.3 MPa.
5. The regeneration process of claim 1 wherein the mass space velocity of the regenerant is from 1.0 to 5.0h -1 。
6. The regeneration method according to claim 1, characterized in that the drying parameters are: the drying temperature is 150-200 ℃, and the drying pressure is 0.5-1.0 MPa.
7. The regeneration method of claim 1, wherein the inert gas is one of nitrogen, argon, and helium.
8. The regeneration process of claim 1, wherein the solid adsorbent is at least one of silica gel, activated alumina, molecular sieves.
9. The regeneration process of claim 1, wherein the regeneration process is carried out in situ in an adsorption column for removing oxygenates from isoparaffins.
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| CN202211296744.3A CN115491223A (en) | 2022-10-21 | 2022-10-21 | Regeneration method of adsorbent for removing oxygen-containing compounds in isoparaffin |
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