CN114686254A - Method for regenerating oxygen-containing compound adsorbent - Google Patents
Method for regenerating oxygen-containing compound adsorbent Download PDFInfo
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- CN114686254A CN114686254A CN202011643620.9A CN202011643620A CN114686254A CN 114686254 A CN114686254 A CN 114686254A CN 202011643620 A CN202011643620 A CN 202011643620A CN 114686254 A CN114686254 A CN 114686254A
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- 238000000034 method Methods 0.000 title claims abstract description 54
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 18
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- 230000001172 regenerating effect Effects 0.000 title claims abstract description 17
- 238000011069 regeneration method Methods 0.000 claims description 89
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 32
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 23
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 claims description 16
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims description 9
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Classifications
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0262—Compounds of O, S, Se, Te
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
- B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
- B01J20/3483—Regenerating or reactivating by thermal treatment not covered by groups B01J20/3441 - B01J20/3475, e.g. by heating or cooling
-
- 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
-
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1022—Fischer-Tropsch products
-
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
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- Chemical & Material Sciences (AREA)
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- Oil, Petroleum & Natural Gas (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A method of regenerating an oxygenate adsorbent comprising: the temperature of the oxygen-containing compound adsorbent is programmed to 50-150 ℃; adding a C6-C12 alkane and contacting the C6-C12 alkane with the oxygenate adsorbent sufficient to regenerate the oxygenate adsorbent. The method of the invention can regenerate the adsorbent for many times, prolong the service life of the adsorbent and reduce the production cost.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a regeneration method of an oxygen-containing compound adsorbent.
Background
At present, the adsorption and the cyclic utilization of the oxygen-containing compounds in the Fischer-Tropsch oil by using a molecular sieve adsorbent are key technologies for realizing the industrial amplification of the removal of the oxygen-containing compounds and the separation of alkane and alkene.
CN110420628A discloses a zeolite molecular sieve regeneration device and a regeneration method, the zeolite molecular sieve saturated by absorbing VOC is placed in a microwave digestion tank, a temperature controller is started and the temperature is set, a microwave generator is started to heat the zeolite molecular sieve, and the time is recorded; and (4) closing the microwave generator at intervals of 1min, taking out the zeolite molecular sieve and weighing until the weight of the zeolite molecular sieve is not changed any more, and finishing regeneration.
CN 108855021A discloses a 13X molecular sieve activation regeneration method, which comprises the following steps: (1) soaking in a mixed solvent: soaking the molecular sieve by using a mixed solvent; (2) finishing with a compound salt solution: under an acidic condition, sequentially soaking the molecular sieve obtained in the step (1) by using a solution containing an Al ion source and a solution containing a Na ion source, uniformly stirring, and standing; (3) washing with water: washing the molecular sieve trimmed by the composite salt solution with deionized water until the water washing solution becomes neutral; (4) and (3) drying: removing the organic solvent and water by using the molecular sieve after washing; (5) inert gas gradient elution: under the protection of inert gas, raising the temperature in stages, and eluting; (6) low-oxygen atmosphere oxidation: heating to a certain temperature, and introducing low-oxygen atmosphere for oxidation; (7) and (5) performing hot purging by using inert gas.
CN11013558A discloses an adsorbent regeneration method based on a cyclic heating mode, which is characterized in that an adsorption tower, a blower, a gas storage tank and a heat exchanger are constructed into a closed circulating body after the adsorption process of the adsorption tower is completed; repeatedly circulating the gas in the circulating body by using the blower, and heating the circulating gas to a set temperature when the circulating gas passes through the heat exchanger; detecting the pressure and the temperature of the circulating gas, stopping the blower after the pressure and the temperature of the circulating gas reach a set pressure, and starting a vacuum pump to extract desorption gas from the circulating body to a negative pressure; repeating the steps until the adsorbent does not release the desorption gas any more; and supplementing a certain amount of dry cold air to the circulating body, circularly cooling the adsorbent, vacuumizing, and repeating until the adsorption and desorption process is completed.
CN105944674A discloses a method for regenerating a poisoned carbon molecular sieve, which comprises the following steps: s100: acid washing: placing the poisoned carbon molecular sieve in a hydrochloric acid solution for fully soaking; s200: washing with water: rinsing the poisoned carbon molecular sieve subjected to acid washing with clear water for 2-3 times; s300: solvent cleaning: and (3) placing the poisoned carbon molecular sieve after washing in an organic solvent for fully soaking: s400: hole adjustment: and (3) placing the poisoned carbon molecular sieve in a nitrogen environment, and adjusting the holes at 600-750 ℃.
CN110935281A discloses an adsorbing and regenerating device and method for a solid adsorbent adsorbing volatile organic compounds, the device and method are to adsorb waste gas containing volatile organic compounds by using the solid adsorbent, and to regenerate the solid adsorbent saturated in adsorption after heating the waste gas containing volatile organic compounds, so as to obtain waste gas with increased concentration of volatile organic compounds, and to absorb the waste gas with increased concentration of volatile organic compounds by using an absorbent having absorbing ability for volatile organic compounds after cooling, so as to obtain waste gas with decreased concentration of volatile organic compounds, which is used as regeneration gas for recycling. And continuously cooling the solid adsorbent with high regeneration qualified temperature by using waste gas containing volatile organic compounds, stopping cooling when the temperature of the solid adsorbent is reduced to a certain temperature, and re-adsorbing by using the solid adsorbent.
CN107376883A discloses an activated carbon regeneration method with saturated adsorption, comprising the following steps: putting an alkaline solvent or an alkaline regeneration solvent and activated carbon with saturated adsorption into a container with a heating device and a stirring device for mixing to obtain an alkaline mixture; carrying out solid-liquid separation on the obtained alkaline mixture to obtain activated carbon to be treated, and recycling an alkaline regenerated solvent generated in the solid-liquid separation process; putting the obtained activated carbon to be treated and an acidic solvent or an acidic regenerated solvent into a container with a heater and a stirrer for mixing to obtain an acidic mixture; carrying out solid-liquid separation on the obtained acidic mixture to obtain activated carbon to be washed, and recycling an acidic regenerated solvent generated in the solid-liquid separation process; and washing the obtained activated carbon to be washed by water to obtain regenerated activated carbon, reusing the regenerated activated carbon for treating the wastewater containing the benzoic acid, and adding acid into the acidic water generated in the washing process for recycling.
For the regeneration process of the oxygen-containing compound molecular sieve adsorbent in the Fischer-Tropsch oil, the existing regeneration process has the following problems: 1. the regeneration cycle evaluation performance is poor; 2. the process is complex and the energy consumption is high.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for regenerating an oxygen-containing compound adsorbent, which can improve the regeneration efficiency of the oxygen-containing compound adsorbent.
The invention adopts the following technical scheme:
a method of regenerating an oxygenate adsorbent, comprising:
the temperature of the oxygen-containing compound adsorbent is programmed to 50-150 ℃;
adding a C6-C12 alkane and contacting the C6-C12 alkane with the oxygenate adsorbent sufficient to regenerate the oxygenate adsorbent.
In some embodiments, the regeneration process is performed in situ in a fixed bed reactor containing an oxygenate adsorbent.
In some embodiments, the C6-C12 alkane is introduced into the C6-C12 alkane from the bottom of the fixed bed reactor and contacts the adsorbent bed.
In some embodiments, the temperature ramp rate of the temperature program is 0.5-3 deg.C/min (e.g., 1.0 deg.C/min, 1.5 deg.C/min, 2.0 deg.C/min, or 2.5 deg.C/min).
In some embodiments, the C6-C12 alkane is reacted with the oxygenate adsorbent for a period of 100-500min (e.g., 200min, 300min, or 400 min).
In some embodiments, as the alkane carbon number employed in the regeneration process decreases, the pressure employed increases and the temperature employed decreases.
In some embodiments, the alkane used in the regeneration process is dodecane, the pressure used is atmospheric, and the temperature used is 80-150 ℃.
In some embodiments, the alkane used in the regeneration process is n-hexane or n-octane, the pressure used is 3.5 to 4.5MPa, and the temperature used is 50 to 70 ℃.
In some embodiments, the regeneration method further comprises: before adding C6-C12 alkane, removing carbonyl-containing impurities in the C6-C12 alkane.
In some embodiments, carbonyl-containing impurities are removed using a molecular sieve adsorbent.
Compared with the prior art, the regeneration method of the oxygen-containing compound adsorbent adopts a fixed bed dynamic adsorption separation technology, can be carried out in situ in a fixed bed reactor, and has the advantages of high regeneration efficiency, simple operation, economy and environmental protection; the method of the invention can regenerate the adsorbent for many times, prolong the service life of the adsorbent and reduce the production cost.
Drawings
The drawings are only for purposes of illustrating and explaining the present invention and are not to be construed as limiting the scope of the present invention. Wherein:
FIG. 1 is a temperature programmed process for a regeneration temperature of 80 ℃ in an embodiment of the present invention;
FIG. 2 is a temperature programmed process for a regeneration temperature of 100 ℃ in an embodiment of the present invention;
FIG. 3 is a temperature programmed process for a regeneration temperature of 120 ℃ in an embodiment of the present invention;
FIG. 4 is a temperature programmed process for a regeneration temperature of 150 ℃ in an embodiment of the present invention;
FIG. 5 is a temperature programmed process for a regeneration temperature of 50 ℃ in an embodiment of the present invention;
FIG. 6 is a temperature programmed process for a regeneration temperature of 60 ℃ in an embodiment of the present invention;
FIG. 7 is a temperature programmed process for a regeneration temperature of 70 ℃ in an embodiment of the present invention;
FIG. 8 is a temperature programmed process for a regeneration temperature of 70 ℃ in an embodiment of the present invention;
FIG. 9 is a temperature programmed process for a regeneration temperature of 120 ℃ in a comparative example of the present invention.
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
In the description of the present invention, reference to "one embodiment" means that a particular feature, structure, or parameter, step, or the like described in the embodiment is included in at least one embodiment according to the present invention. Thus, appearances of the phrases such as "in one embodiment," "in one embodiment," and the like in this specification are not necessarily all referring to the same embodiment, nor are other phrases such as "in another embodiment," "in a different embodiment," and the like. Those of skill in the art will understand that the particular features, structures or parameters, steps, etc., disclosed in one or more embodiments of the present description may be combined in any suitable manner.
Aiming at the defects in the prior art, the invention provides the method for regenerating the oxygen-containing compound adsorbent, which has the advantages of low cost, reasonability, practicability and easy industrialization. The oxygenate adsorbent in the present invention means a molecular sieve for adsorbing oxygenates, for example, a 3A, 4A, 5A, 10X, 13X type molecular sieve. The invention uses C6-C12 alkane (such as n-hexane, n-heptane, n-octane, n-nonane, n-decane, dodecane and the like) to regenerate and utilize the molecular sieve adsorbent poisoned by adsorption.
In the following examples, the adsorbent is used to adsorb the oxygen-containing compounds in the C11-C16 cut oil and regenerate the saturated adsorbent, wherein the oxygen-containing compounds in the C11-C16 cut oil include one or more of alcohols, aldehydes, acids, ketones, and esters.
The method for removing the carbonyl from the C6-C12 alkane used in the regeneration process by utilizing a dynamic adsorption mode comprises the following steps:
1. filling an adsorbent: filling a new activated adsorbent 13X molecular sieve in an adsorption tube with the inner diameter of 45mm and the length of 67.8X 2cm, and filling quartz wool up and down with the adsorbent filling amount of 2156 ml;
2. liquid feeding: C6-C12 alkane is fed for dynamic adsorption experiment;
3. sampling: sampling under the condition that no leakage is confirmed;
4. and (3) carbonyl analysis: and (4) analyzing the content of the carbonyl in the sample solution, and finding a penetration point to obtain the carbonyl-free alkane.
Examples 1-4 below use dodecane as the regeneration medium, with regeneration temperatures selected from 80 ℃ to 150 ℃.
Example 1
(1) Spreading 13X type molecular sieve adsorbent in a special burning spoon of muffle furnace (ensuring that the particle layer is thin), wherein the roasting amount is about 70g each time, the shape of the adsorbent is spherical, and the particle size is 0.85. Roasting the adsorbent at 700 ℃ for 6 hours, naturally cooling the adsorbent to 150 ℃ in a muffle furnace, taking out the adsorbent and placing the adsorbent in a dryer for later use. (the muffle furnace temperature rise rate is 2 ℃/min, and the lower rate is set to prevent the change of the adsorbent structure);
(2) the loading height of the adsorbent was determined by the constant temperature zone (h ═ 13.7cm) of the high temperature furnace, and the loading amount of the fixed bed adsorption tube was 45.32g and the loading volume was 70.81 ml. Quartz wool is filled in the upper and lower openings of the adsorbent bed layer;
(3) the primary water is used as a calibration medium, and the calibration system is located in a closed space. (calibration error caused by loss of weight of the placed first-grade water) experiment keeping airspeed v equal to 0.996h-1The volume flow rate of the C11-C16 cutting oil is calculated according to the filling volume of bed particles and is 0.27 ml/min. The calibration time of the feeding pump is 2 hours, the weight gain of the first-stage water is recorded every ten minutes, and 12 groups of weight data are fitted to determine the accurate flow of the feeding pump. Calibrated accurate flow V1＝0.272ml/min；
(4) C11-C16 cutting oil is pumped in at a flow rate of 2.48ml/min for 59min (based on the liquid outlet time of the adsorption tower), and saturated adsorption (carried out at normal temperature and normal pressure) is completed. The adsorption experiments were performed with a C11-C16 cut oil removal system calibrated for primary water. C11-C16 cutting oil enters a bed layer from the lower part of a fixed bed adsorption tower, oxygen-containing compounds in the C11-C16 cutting oil are adsorbed by the adsorption bed layer and collected from the top of the adsorption tower, carbonyl analysis is carried out on sampling liquid at the same time interval so as to determine the adsorption condition of the adsorption bed layer, and an adsorption curve is drawn by taking time as an abscissa and the number of carbonyl groups as an ordinate so as to determine the adsorption capacity corresponding to a breakthrough point of an adsorbent;
(5) as shown in fig. 1, the fixed bed regenerator was set to perform temperature programming at a rate of temperature rise: 0.9 ℃/min, heating to 80 ℃, introducing dodecane from the bottom of the fixed bed reactor, contacting with the adsorbent bed layer, regenerating at normal pressure, wherein the dodecane has the action time of 285min, and the programmed heating process is 60min, and then closing the device to recover to normal temperature, namely the regeneration is finished. Dodecane is collected in liquid form at the top of the adsorption column.
The cycle evaluation experiment specifically comprises: the regeneration is carried out for 52 times of adsorption-regeneration cycles, and the regeneration efficiency is still 91.3 percent. From the above results, the adsorption effect of the regenerated adsorbent is not obviously different from that of the fresh adsorbent, which shows that the method of the invention can regenerate the adsorbent for many times, prolong the service life of the adsorbent and reduce the production cost.
Example 2
In this example, the particle size of the 13X type molecular sieve adsorbent was 1.15mm, and the steps (1) to (4) were the same as in example 1.
In step (5), as shown in fig. 2, a fixed bed regenerator was set to perform temperature programming at a rate of temperature increase: heating to 100 deg.C at 1.25 deg.C/min, introducing dodecane from the bottom of the fixed bed reactor, contacting with the adsorbent bed layer, regenerating at normal pressure with dodecane flow of 4.04ml/min, wherein dodecane action time is 285min, and heating for 60min, and closing the device to recover to normal temperature. Dodecane is collected in liquid form at the top of the adsorption column.
The cycle evaluation experiment specifically comprises: the regeneration is carried out for 52 times of adsorption-regeneration cycles, and the regeneration efficiency is still 96.3 percent. From the above results, the adsorption effect of the regenerated adsorbent is not obviously different from that of the fresh adsorbent, which shows that the method of the invention can regenerate the adsorbent for many times, prolong the service life of the adsorbent and reduce the production cost.
Example 3
In this example, the particle size of the 13X type molecular sieve adsorbent was 1mm, and the steps (1) to (4) were the same as in example 1.
In step (5), as shown in fig. 3, a fixed bed regenerator was set to perform temperature programming at a rate of temperature increase: heating to 120 ℃ at the temperature of 1.58 ℃/min, introducing dodecane from the bottom of the fixed bed reactor, contacting with the adsorbent bed layer, regenerating at normal pressure, wherein the dodecane has the action time of 285min, and the programmed heating process is 60min, and then closing the device to recover to normal temperature, namely the regeneration is finished. Dodecane is collected in liquid form at the top of the adsorption column.
The cycle evaluation experiment specifically comprises: regeneration is carried out for 55 times of adsorption-regeneration cycles, and the regeneration rate is still kept at 96.4 percent. From the above results, the adsorption effect of the regenerated adsorbent is not obviously different from that of the fresh adsorbent, which shows that the method of the invention can regenerate the adsorbent for many times, prolong the service life of the adsorbent and reduce the production cost.
Example 4
In this example, the particle size of the 13X type molecular sieve adsorbent was 1mm, and the steps (1) to (4) were the same as in example 1.
In step (5), as shown in fig. 4, a fixed bed regenerator is set to perform temperature programming at a rate of temperature increase: 2.1 ℃/min, heating to 150 ℃, introducing dodecane from the bottom of the fixed bed reactor, contacting with the adsorbent bed layer, regenerating at normal pressure, wherein the dodecane has the action time of 285min, and the programmed heating process is 60min, and then closing the device to recover to normal temperature, namely the regeneration is finished. Dodecane is collected in liquid form at the top of the adsorption column.
The cycle evaluation experiment specifically comprises: the regeneration is carried out for 42 times of adsorption-regeneration cycles, and the regeneration rate is still maintained at 91.4 percent. From the above results, the adsorption effect of the regenerated adsorbent is not obviously different from that of the fresh adsorbent, which shows that the method of the invention can regenerate the adsorbent for many times, prolong the service life of the adsorbent and reduce the production cost.
In the following examples 5-7, n-hexane was used as a regeneration medium, the system pressure was 3.5-4.5MPa, and the regeneration temperature was selected from 50 ℃ to 70 ℃.
Example 5
In this example, the particle size of the 13X type molecular sieve adsorbent was 0.85mm, and the steps (1) to (4) were the same as in example 1.
In step (5), as shown in fig. 5, a fixed bed regenerator was set to perform temperature programming at a rate of temperature increase: 0.5 ℃/min, heating to 50 ℃, and keeping the system pressure at 3.5 MPa. Introducing n-hexane from the bottom of the fixed bed reactor, contacting with the adsorbent bed layer, wherein the flow rate of n-hexane is 3.15ml/min, regenerating under pressurization, wherein the action time of n-hexane is 120min, and the temperature programming process is 50min, then closing the device to release pressure, and recovering to normal temperature, namely finishing regeneration. The n-hexane was collected in liquid form at the top of the adsorption column.
The cycle evaluation experiment specifically comprises: regeneration is carried out for 36 times of adsorption-regeneration cycles, and the regeneration rate is still maintained at 98.4 percent. From the above results, the adsorption effect of the regenerated adsorbent is not obviously different from that of the fresh adsorbent, which shows that the method of the invention can regenerate the adsorbent for many times, prolong the service life of the adsorbent and reduce the production cost.
Example 6
In this example, the particle size of the 13X type molecular sieve adsorbent was 1.15mm, and the steps (1) to (4) were the same as in example 1.
In step (5), as shown in fig. 6, a fixed bed regenerator was set to perform temperature programming at a rate of temperature increase: 0.5 ℃/min, heating to 60 ℃, and keeping the system pressure at 4.0 MPa. Introducing n-hexane from the bottom of the fixed bed reactor, contacting with the adsorbent bed layer, wherein the flow rate of n-hexane is 3.15ml/min, regenerating under pressurization, wherein the action time of n-hexane is 120min, the temperature programming process is 70min, then closing the device to release pressure, and recovering to normal temperature, namely finishing regeneration. The n-hexane was collected in liquid form at the top of the adsorption column.
The cycle evaluation experiment specifically comprises: regeneration is carried out for 45 times of adsorption-regeneration cycles, and the regeneration rate is still maintained at 99.2 percent. From the above results, the adsorption effect of the regenerated adsorbent is not obviously different from that of the fresh adsorbent, which shows that the method of the invention can regenerate the adsorbent for many times, prolong the service life of the adsorbent and reduce the production cost.
Example 7
In this example, the particle size of the 13X type molecular sieve adsorbent was 1mm, and the steps (1) to (4) were the same as in example 1.
In step (5), as shown in fig. 7, a fixed bed regenerator was set to perform temperature programming at a rate of temperature increase: 0.5 ℃/min, the temperature is raised to 70 ℃, and the system pressure is 4.5 MPa. Introducing n-hexane from the bottom of the fixed bed reactor, contacting with the adsorbent bed layer, wherein the flow rate of n-hexane is 3.15ml/min, regenerating under pressurization, wherein the action time of n-hexane is 120min, the temperature programming process is 90min, then closing the device to release pressure, and recovering to normal temperature, namely finishing regeneration. The n-hexane was collected in liquid form at the top of the adsorption column.
The cycle evaluation experiment specifically comprises: regeneration is carried out for 49 times of adsorption-regeneration cycles, and the regeneration rate is still kept at 97.8 percent. From the above results, the adsorption effect of the regenerated adsorbent is not obviously different from that of the fresh adsorbent, which shows that the method of the invention can regenerate the adsorbent for many times, prolong the service life of the adsorbent and reduce the production cost.
Example 8
In the embodiment, n-octane is used as a regeneration medium, the system pressure is 4.0MPa, and the regeneration temperature is selected to be 70 ℃.
In this example, the particle size of the 13X type molecular sieve adsorbent was 1mm, and the steps (1) to (4) were the same as in example 1.
In step (5), as shown in fig. 8, a fixed bed regenerator is set to perform temperature programming at a rate of temperature increase: 0.5 ℃/min, heating to 70 ℃, and keeping the system pressure at 4.0 MPa. Introducing n-octane from the bottom of the fixed bed reactor, contacting with the adsorbent bed layer, wherein the flow rate of the n-octane is 3.2ml/min, regenerating under pressurization, wherein the action time of the n-octane is 120min, carrying out temperature programming for 90min, then closing the device to release pressure, and recovering to normal temperature, namely finishing regeneration. The carbonyl-free n-octane is collected as a liquid at the top of the adsorption column.
The cycle evaluation experiment specifically comprises: regeneration is carried out for 59 times of adsorption-regeneration cycles, and the regeneration rate is still kept at 97.2 percent. From the above results, the adsorption effect of the regenerated adsorbent is not obviously different from that of the fresh adsorbent, which shows that the adsorbent of the present invention can be regenerated repeatedly, the service life of the adsorbent is prolonged, and the production cost is reduced.
Comparative example
This example uses pentadecane as the regeneration medium, the regeneration temperature being chosen at 120 ℃. In this example, the particle size of the 13X type molecular sieve adsorbent was 1mm, and the steps (1) to (4) were the same as in example 1.
In step (5), as shown in fig. 9, a fixed bed regenerator was set to perform temperature programming at a rate of temperature increase: heating to 120 deg.C at 0.5 deg.C/min. And introducing pentadecane from the bottom of the fixed bed reactor to contact with the adsorbent bed, wherein the flow rate of the pentadecane is 3.2ml/min, the action time of the pentadecane is 120min, the temperature programming process is 190min, and the normal temperature is recovered, namely the regeneration is finished. The carbonylless pentadecane is collected in liquid form at the top of the adsorption column.
The cycle evaluation experiment specifically comprises: regeneration is carried out for 16 times of adsorption-regeneration cycles, and the regeneration rate is 39.2 percent. From the above results, the adsorption effect of the regenerated adsorbent is significantly different from that of the fresh adsorbent.
The invention pretreats the adsorbent to ensure that the 13X type adsorbent has higher adsorption capacity, which is beneficial to accelerating the adsorption rate and prolonging the service life of the adsorbent; the fixed bed adsorption tower is used, the operation is simple and easy, and the process flow is simple. The adsorption is carried out at normal temperature, so that high adsorption capacity can be obtained, and meanwhile, the regeneration method is simple and feasible and has long service cycle. The invention has reasonable and practical design, reduces the cost, saves the resources, improves the economic benefit and the production efficiency, and is suitable for being widely popularized and used.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method of regenerating an oxygenate adsorbent comprising:
the temperature of the oxygen-containing compound adsorbent is programmed to 50-150 ℃;
adding a C6-C12 alkane and contacting the C6-C12 alkane with the oxygenate adsorbent sufficient to regenerate the oxygenate adsorbent.
2. The regeneration process of claim 1, wherein the regeneration process is conducted in situ in a fixed bed reactor containing an oxygenate adsorbent.
3. The regeneration process of claim 2, wherein the C6-C12 alkane is introduced into the C6-C12 alkane from the bottom of the fixed bed reactor and contacts the adsorbent bed.
4. The regeneration method of claim 1, wherein the temperature ramp rate of the programmed temperature is 0.5-3 ℃/min (e.g., 1.0 ℃/min, 1.5 ℃/min, 2.0 ℃/min, or 2.5 ℃/min).
5. The regeneration method as claimed in claim 1, wherein the reaction time of the C6-C12 alkane and the oxygen-containing compound adsorbent is 100-500min (e.g. 200min, 300min or 400 min).
6. The regeneration process of claim 1, wherein the pressure employed increases and the temperature employed decreases as the alkane carbon number employed decreases in the regeneration process.
7. The regeneration process according to claim 1, wherein the alkane used in the regeneration process is dodecane, the pressure used is atmospheric pressure, and the temperature used is 80-150 ℃.
8. The regeneration process according to claim 1, wherein the alkane used in the regeneration process is n-hexane or n-octane, the pressure used is comprised between 3.5 and 4.5MPa and the temperature used is comprised between 50 and 70 ℃.
9. The regeneration method of claim 1, wherein the regeneration method further comprises: before adding the C6-C12 alkane, carbonyl-containing impurities in the C6-C12 alkane are removed.
10. The regeneration process of claim 9, wherein the carbonyl-containing impurities are removed using a molecular sieve adsorbent.
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