CN110180321B - A kind of adsorption process method using multiple adsorbents in series - Google Patents
A kind of adsorption process method using multiple adsorbents in series Download PDFInfo
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- CN110180321B CN110180321B CN201910449299.1A CN201910449299A CN110180321B CN 110180321 B CN110180321 B CN 110180321B CN 201910449299 A CN201910449299 A CN 201910449299A CN 110180321 B CN110180321 B CN 110180321B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
- B01D53/0407—Constructional details of adsorbing systems
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
- B01D53/047—Pressure swing adsorption
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
- B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
- B01D53/047—Pressure swing adsorption
- B01D53/0476—Vacuum pressure swing adsorption
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Abstract
本发明公开了一种多种吸附剂串联使用的吸附工艺方法，将两种或两种以上的吸附剂串联使用，串联使用的吸附剂中至少有一种为吸附质的优惠型吸附剂，至少有一种为吸附质的非优惠型吸附剂。对同一种吸附质而言，浓度锋面在非优惠型吸附剂填充范围内逐渐分散，但优惠型吸附剂可将分散的浓度锋面进行压缩。与单一吸附剂装填相比，吸附剂串联的方式解决了优惠型吸附剂脱附速率低、脱附残留大的缺点和非优惠型吸附剂床层利用率低、穿透时间短的问题。将本发明应用于固定床变压吸附与冷凝结合连续回收挥发性有机物的装置中，在保证排放尾气不含挥发性有机物，且实现挥发性有机物100％回收的前提下，与单一吸附剂装填相比，实现装置能耗显著降低。
The invention discloses an adsorption process method in which multiple adsorbents are used in series. Two or more adsorbents are used in series. At least one of the adsorbents used in series is a preferential adsorbent for adsorbents, and at least one adsorbent is a preferential adsorbent. A non-preferential adsorbent that is an adsorbate. For the same adsorbate, the concentration front gradually disperses in the filling range of the non-preferential adsorbent, but the preferential adsorbent can compress the dispersed concentration front. Compared with single adsorbent loading, the series connection of adsorbents solves the disadvantages of low desorption rate and large desorption residues of preferential adsorbents and the problems of low bed utilization rate and short breakthrough time of non-preferential adsorbents. The invention is applied to a device for continuously recovering volatile organic compounds by combining fixed-bed pressure swing adsorption and condensation, and on the premise that the exhaust gas does not contain volatile organic compounds and realizes 100% recovery of volatile organic compounds, it can be combined with a single adsorbent filling phase. The energy consumption of the device is significantly reduced.
Description
Technical Field
The invention belongs to the field of gas-solid phase adsorption, relates to an adsorbent, and particularly relates to an adsorption process method for serial use of multiple adsorbents.
Background
Adsorption is a common treatment method for separating mixtures, and gas phase adsorption is often combined with condensation or rectification and other processes to realize separation and recovery of adsorbates. The choice of adsorbent plays a crucial role in the design of the adsorption scheme. According to previous studies, physical adsorption of gas in porous media occurs in two forms, adsorption of gas on the surfaces of the pores and capillary condensation. The surface adsorption is that the adsorbate is fixed on the surface of the adsorbent pore channel by the action force between the adsorbate and the adsorbent, and the capillary condensation is that the equilibrium vapor pressure of small drops in the capillary is larger than that of large plane liquid due to the action of surface tension. The ideal adsorbent should have the advantages of large adsorption capacity, fast adsorption and desorption rate, excellent cycle performance, low desorption residue, low price, low thermal effect and the like, but the actual adsorbent is often difficult to meet all conditions.
Preferential type adsorbent: the adsorbent has strong van der waals force to the adsorbate. The adsorption usually occurs in a surface adsorption form or a pore channel filling form in pores, the strong adsorption potential of the adsorbent ensures that the adsorbent has higher adsorption capacity at low adsorbate concentration, and the isotherm is preferential, so that the adsorbent is called as an exterior preferential adsorbent. The strong adsorption potential makes the adsorbent possess quick adsorption rate, and the concentration frontal surface in the adsorption zone is steeper, and the adsorbent high-usage when breaching through. But the large adsorption potential often limits the desorption rate, so that the desorption gas has low purity, long desorption time and high energy consumption of the device. Some adsorbents such as activated carbon also have irreversible adsorbate residues that affect the recycling performance of the adsorbent. Therefore, preferential adsorbents have limited their application in industrial adsorption due to factors of desorption performance and recycling performance.
Non-preferential adsorbents: the relatively weak adsorption potential results in a low equilibrium adsorption capacity of the adsorbent at low adsorbate concentrations and capillary condensation at medium and high adsorbate concentrations, which are also referred to as capillary condensation adsorbents. The adsorbent has small adsorption potential and low capillary condensation rate, so that the slope of the concentration front in the adsorption zone is gradually reduced along with the movement of the adsorption zone in the adsorption process, the utilization rate of the adsorbent is low, and the penetration time is short. But the smaller adsorption potential and fast capillary gasification cause the adsorbent to exhibit a faster desorption rate during desorption. The desorption gas has high concentration, short desorption time, less residue and good recycling performance.
The absorption penetration time, the desorption gas concentration, the desorption time and the residual quantity of adsorbate are important indexes for measuring the absorption performance. The energy consumption of the process of recovering the adsorbate by the adsorption process is an important factor for determining whether the adsorbent can be industrially applied. Disclosure of Invention
Aiming at the problems in the application of the two types of adsorbents and the characteristics of the two types of adsorbents, the invention develops an adsorption process method adopting two or more than two types of adsorbents in series, and replaces the traditional filling mode of a single adsorbent. In the adsorption process, the preferential adsorbent can compress the concentration front dispersed in a non-preferential adsorbent filling area, and compared with an adsorption device filled with a single preferential adsorbent, the utilization rate of the adsorbent in the series adsorbent process is higher, and the penetration time is longer. Meanwhile, the influence of a small amount of loaded preferential adsorbent on the desorption performance is small.
The invention provides an adsorption process method with a plurality of adsorbents connected in series, which is used for replacing a filling mode of a single adsorbent. The process is illustrated as follows:
an adsorption process for serially using more than two adsorbents features that two or more than two adsorbents are serially used, and at least one of the serially used adsorbents is preferential adsorbent and at least one is non-preferential adsorbent.
In addition, the series connection is used by filling two or more adsorbents into one adsorption device or adopting a plurality of adsorption devices in series connection, and each adsorption device is filled with one or more adsorbents.
Moreover, the adsorbent is a carbon material adsorbent or a silicon-containing material adsorbent or a carbon-silicon composite material adsorbent.
Moreover, the carbon material adsorbent is activated carbon, a biomass carbon material, a carbon nanotube and activated carbon fiber.
Moreover, the adsorbent containing the silicon material is silica gel, silicon dioxide, molecular sieve, resin, zeolite and MOFs.
And the packing volume ratio of the adsorbent is between 0.01 and 100.
Furthermore, the adsorption operation pressure is between 100kPa and 100MPa, and the adsorption operation temperature is between 0K and 400K.
The adsorption device is a fixed bed, the adsorbate is VOCs, and the filling ratio of preferential adsorbents to non-preferential adsorbents is 1: 4-4: 1.
The adsorbate is a gas phase inorganic substance or a gas phase organic substance.
The invention has the following advantages:
compared with the filling of a single preferential adsorbent, the invention improves the desorption performance of the adsorption process, improves the purity of adsorbates in desorption gas, reduces the desorption time, reduces the desorption residual quantity and improves the recycling performance of the adsorption process.
Compared with the filling of a single non-preferential adsorbent, the invention improves the slope of the concentration frontal surface in the adsorption process and improves the utilization rate and the penetration time of the adsorbent.
3, by optimizing the filling volumes of different adsorbents, the energy consumption of the device is obviously reduced compared with the filling of a single adsorbent under the condition of ensuring the complete separation of mixed gas phases.
Drawings
FIG. 1 is a schematic diagram of an apparatus for recovering ortho-xylene from an offgas by combining fixed bed pressure swing adsorption and condensation in an embodiment.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments, which are illustrative only and not limiting, and the scope of the present invention is not limited thereby.
The application of the invention in a VOCs recovery device combining fixed bed pressure swing adsorption and condensation illustrates the superiority of the invention in reducing energy consumption.
In the flow scheme shown in FIG. 1, the main equipment includes fixed beds 2-1 and 2-2 packed in stages of alternately switched adsorbents, gas chromatographs 3-1 and 3-2, a vacuum pump 4, a condenser 5, needle valves 7-1 and 7-2, solenoid valves 8-1, 8-2, 8-3, 8-4, 8-5, 8-6, 8-7 and 8-8, and vacuum pressure gauges 9-1 and 9-2. 1 represents mixed exhaust gas, 6 represents a nitrogen source, 10 represents purified exhaust gas, and 11 represents condensed VOCs liquid.
For example, the fixed bed 2-1 is used for carrying out adsorption operation, and the operation process of the device is as follows:
an adsorption step: solenoid valves 8-1 and 8-4 are open. The mixed waste gas 1 of VOCs and nitrogen enters a fixed bed 2-1 through an electromagnetic valve 8-1, the VOCs are adsorbed by an adsorbent in the fixed bed 2-1, the nitrogen which is not easy to be adsorbed passes through an adsorbent bed layer and is used as purified tail gas to pass through an electromagnetic valve 8-4, and the purified tail gas enters a gas chromatograph 3-1 to measure the concentration of the VOCs. The remaining cleaned tail gas 10 is discharged along the pipeline. When the concentration of VOCs in the purified tail gas is detected to be more than 0ppm by the gas chromatography 3-1, the adsorption step is stopped, and the electromagnetic valves 8-1 and 8-4 are closed.
When the fixed bed 2-1 starts the adsorption step, the fixed bed 2-2 stops adsorption and starts the regeneration operation, the fixed bed regeneration operation is divided into three steps, namely a vacuumizing step, a vacuum desorption step and a pressure increasing step:
and (3) vacuumizing: and opening the electromagnetic valve 8-8, opening the needle valve 7-1 and opening the vacuum pump 4 to vacuumize the fixed bed 2-2, wherein VOCs on the adsorbent are desorbed along with the reduction of pressure and flow through the electromagnetic valve 8-8, the needle valve 7-1 and the vacuum pump 4. After the concentration is detected by the gas chromatography 3-2, in the condenser 5, VOCs gas is condensed into liquid phase, the condensed VOCs liquid 11 flows through the pipeline for collection, and the uncondensed VOCs waste gas is mixed with the VOCs waste gas 1 of the pipeline and enters the fixed bed 2-1 for adsorption. When the pressure of the vacuum pressure gauge 9-2 shows a decrease to the desorption pressure set value, the evacuation step is stopped. The fixed bed 2-2 enters a vacuum desorption step.
Vacuum desorption step: the needle valve 7-2 is opened and the electromagnetic valve 8-6 is opened. The nitrogen gas source 6 supplies nitrogen gas with a purity of 99.9% which is adjusted to a stripping gas flow rate set value by the needle valve 7-2, and the index of the vacuum pressure gauge 9-2 is maintained constant at a desorption pressure set value by adjusting the needle valve 7-1. And nitrogen flows through the fixed bed 2-2, VOCs on the adsorbent is desorbed under the dual actions of vacuum and steam stripping, the desorption gas and the desorption gas in the vacuumizing step undergo the same flow, most of the condensed VOCs are collected and recovered, and a small part of the uncondensed VOCs waste gas enters the fixed bed 2-1 for re-adsorption. And when the desorption concentration detected by the gas chromatography 3-2 is less than the concentration of the VOCs waste gas 1 in the pipeline, stopping the vacuum desorption step. The fixed bed 2-2 enters a pressure increasing step.
A step of boosting: closing the electromagnetic valve 8-8, continuously flowing nitrogen into the fixed bed 2-2 from the lower outlet, gradually increasing the pressure, closing the electromagnetic valve 8-6 when the vacuum pressure is indicated as the vacuum degree of 0KPa, and ending the pressure increasing step.
Generally, the regeneration operation of the fixed bed requires a shorter time than the adsorption operation. When the fixed bed 2-1 completes the adsorption operation, the fixed bed 2-1 is switched to the evacuation step of the regeneration operation, and the electromagnetic valve 8-7 is opened. At the same time, the fixed bed 2-2 is shifted to the adsorption step, and the electromagnetic valves 8-2 and 8-3 are opened. When the index of the vacuum pressure gauge 9-1 is lower than the set value of the desorption pressure, the fixed bed 2-1 enters a vacuum desorption step, and the electromagnetic valve 8-5 is opened. When the concentration of the desorption gas is lower than the concentration of VOCs waste gas 1 in the pipeline in the detection of 3-2 by the gas chromatography, the fixed bed 2-1 enters a pressure boosting step, and the electromagnetic valve 8-7 is closed. When the index of the vacuum pressure gauge 9-1 is 0KPa, the pressure increasing step of the fixed bed 2-1 is finished, and the electromagnetic valve 8-5 is closed. When the concentration of o-xylene in the purified tail gas is more than 0ppm as determined by gas chromatography 3-1, the adsorption step of the fixed bed 2-2 is stopped, and the electromagnetic valves 8-2 and 8-3 are closed. One adsorption regeneration cycle is completed and the next cycle is performed. The adsorption steps of the fixed beds 2-1 and 2-2 and the regeneration operation are alternately switched, and the switch of the electromagnetic valve is logically controlled by a PLC.
Example 1
The experiment was carried out at ambient temperature.
The adsorbent is selected from spherical preferential activated carbon and spherical non-preferential activated carbon.
The experimental results using a single preferential activated carbon and a single non-preferential activated carbon were used as controls, and the sum of the volumes of the two activated carbons in the adsorbent cascade was equal to the fill volume of the single activated carbon experiment. And obtaining the optimal filling ratio of the two activated carbons under the experimental conditions by comparing the energy consumption values of the two activated carbons for treating the unit amount of waste gas under different filling ratios.
O-xylene as VOCs at a concentration of 4000ppm and a flow of 300m3The temperature is normal temperature.
The set value of desorption pressure in the regeneration operation was vacuum degree 95 KPa.
The condenser cools the desorbed gas with 10-degree condensate water.
Table 1 shows the average value of five periodic cycles of the comparison of the process parameters of different loading proportions of non-preferential activated carbon and preferential activated carbon in the pressure swing adsorption and condensation combined recovery of o-xylene
Example 2
The experiment was carried out at ambient temperature.
The adsorbent is selected from spherical preferential silica gel and spherical non-preferential silica gel.
The experimental results using a single preferential silica gel and a single non-preferential silica gel were used as controls, and the sum of the two silica gel volumes in the adsorbent series arrangement was equal to the fill volume of the single silica gel experiment. And obtaining the optimal filling proportion of the two silica gels under the experimental condition by comparing the energy consumption values of the two silica gels for treating the unit amount of waste gas under different filling proportions.
O-xylene as VOCs at a concentration of 4000ppm and a flow of 300m3The temperature is normal temperature.
The set value of desorption pressure in the regeneration operation was vacuum degree 95 KPa.
The condenser cools the desorbed gas with 10-degree condensate water.
Table 2 comparison of series loading and single component loading of non-preferential silica gel and preferential silica gel at different loading ratios and five-cycle cyclic averaging of process parameters of recycling o-xylene by combining pressure swing adsorption and condensation
Example 3
The experiment was carried out at ambient temperature.
The adsorbent is selected from spherical preferential resin and spherical non-preferential resin.
The results of the experiments using a single preferential resin and a single non-preferential resin were used as controls, and the sum of the two resin volumes in the adsorbent cascade was equal to the fill volume of the single resin experiment. And obtaining the optimal filling ratio of the two resins under the experimental conditions by comparing the energy consumption values of the two resins for treating the unit waste gas amount under different filling ratios.
O-xylene as VOCs at a concentration of 4000ppm and a flow of 300m3The temperature is normal temperature.
The set value of desorption pressure in the regeneration operation was vacuum degree 95 KPa.
The condenser cools the desorbed gas with 10-degree condensate water.
Table 3 comparison of series filling and single component filling of different filling ratios of non-preferential resin and preferential resin in the process of recovering o-xylene by combining pressure swing adsorption and condensation and taking an average value through five-period circulation
Example 4
The experiment was carried out at ambient temperature.
The adsorbent is selected from spherical preferential zeolite and spherical non-preferential zeolite.
The results of the experiments using a single preferential zeolite and a single non-preferential zeolite were used as controls, and the sum of the volumes of the two zeolites in the adsorbent series was equal to the packing volume of the single zeolite experiment. And obtaining the optimal filling ratio of the two zeolites under experimental conditions by comparing the energy consumption values of the two zeolites for treating unit waste gas amount under different filling ratios.
O-xylene as VOCs at a concentration of 4000ppm and a flow of 300m3The temperature is normal temperature.
The set value of desorption pressure in the regeneration operation was vacuum degree 95 KPa.
The condenser cools the desorbed gas with 10-degree condensate water.
TABLE 4 comparison of different loading ratios of non-preferential zeolite and preferential zeolite for series loading and single-component loading in pressure swing adsorption and condensation combined process parameters for recovering o-xylene, and taking average value for five cycles
The comparative experiment shows that: the longer desorption time of the preferential adsorbent and the shorter penetration time of the non-preferential adsorbent can cause the energy consumption of the VOCs recovery process to be higher than that of a recovery device with two adsorbents connected in series. By adopting the comparison of the device energy consumption of preferential adsorbents and non-preferential adsorbents in different filling ratios, the adsorbent series process is found to be capable of effectively reducing the energy consumption of the adsorption process, and the adsorbent series process has a good application prospect.
Example 5
The experiment was carried out at ambient temperature.
The adsorbent is selected from spherical preferential silica and spherical non-preferential silica.
The results of the experiments using a single preferential silica and a single non-preferential silica are used as controls, and the sum of the two silica volumes in the adsorbent tandem is equal to the fill volume of the single silica experiment. And obtaining the optimal filling proportion of the two silicon dioxides under the experimental condition by comparing the energy consumption values of the two silicon dioxides for treating the unit waste gas amount under different filling proportions.
O-xylene as VOCs at a concentration of 4000ppm and a flow of 300m3The temperature is normal temperature.
The set value of desorption pressure in the regeneration operation was vacuum degree 95 KPa.
The condenser cools the desorbed gas with 10-degree condensate water.
TABLE 4 comparison of the parameters of the series loading and single-component loading of non-preferential silica and preferential silica at different loading ratios for recovering ortho-xylene by pressure swing adsorption and condensation combined with five cycles of averaging
The comparative experiment shows that: the longer desorption time of the preferential adsorbent and the shorter penetration time of the non-preferential adsorbent can cause the energy consumption of the VOCs recovery process to be higher than that of a recovery device with two adsorbents connected in series. By adopting the comparison of the device energy consumption of preferential adsorbents and non-preferential adsorbents in different filling ratios, the adsorbent series process is found to be capable of effectively reducing the energy consumption of the adsorption process, and the adsorbent series process has a good application prospect.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various changes and modifications can be made without departing from the inventive concept, and these changes and modifications are all within the scope of the present invention.
Claims (9)
1. An adsorption process method for serial use of multiple adsorbents is characterized in that: more than two adsorbents are used in series, at least one of the adsorbents used in series is preferential adsorbent of adsorbate, at least one of the adsorbents used in series is non-preferential adsorbent of adsorbate, and the preferential adsorbent is used for the VOCs recovery device combining fixed bed pressure swing adsorption and condensation.
2. The adsorption process of claim 1 wherein the plurality of adsorbents are used in series, wherein: the serial use is that more than two adsorbents are filled in one adsorption device or a plurality of adsorption devices are adopted to be connected in series, and more than one adsorbent is filled in each adsorption device.
3. The adsorption process of claim 1 wherein the plurality of adsorbents are used in series, wherein: the adsorbent is a carbon material adsorbent or a silicon-containing material adsorbent.
4. The adsorption process of claim 3 wherein the plurality of adsorbents are used in series, wherein: the adsorbent is a carbon-silicon composite adsorbent.
5. The adsorption process of claim 3 wherein the plurality of adsorbents are used in series, wherein: the carbon material adsorbent is activated carbon, a biomass carbon material and a carbon nano tube.
6. The adsorption process of claim 3 wherein the plurality of adsorbents are used in series, wherein: the adsorbent containing the silicon material is silica gel, silicon dioxide, molecular sieve, resin and MOFs.
7. The adsorption process of claim 1 wherein the plurality of adsorbents are used in series, wherein: the adsorption operation pressure is between 100kPa and 100MPa, and the adsorption operation temperature is between 0K and 400K.
8. The adsorption process of claim 1 wherein the plurality of adsorbents are used in series, wherein: the adsorption device is a fixed bed, the adsorbate is VOCs, and the filling ratio of preferential adsorbents to non-preferential adsorbents is 1: 4-4: 1.
9. The adsorption process of claim 1 wherein the plurality of adsorbents are used in series, wherein: the adsorbate is a gas-phase organic matter.
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