CN107340214B - System for detecting adsorption capacity of molecular sieve under high pressure condition and detection method thereof - Google Patents
System for detecting adsorption capacity of molecular sieve under high pressure condition and detection method thereof Download PDFInfo
- Publication number
- CN107340214B CN107340214B CN201611102790.XA CN201611102790A CN107340214B CN 107340214 B CN107340214 B CN 107340214B CN 201611102790 A CN201611102790 A CN 201611102790A CN 107340214 B CN107340214 B CN 107340214B
- Authority
- CN
- China
- Prior art keywords
- molecular sieve
- impurity
- tank
- pressure
- impurities
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 107
- 239000002808 molecular sieve Substances 0.000 title claims abstract description 95
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 238000001514 detection method Methods 0.000 title claims abstract description 20
- 239000012535 impurity Substances 0.000 claims abstract description 141
- 239000007788 liquid Substances 0.000 claims abstract description 44
- 238000003860 storage Methods 0.000 claims abstract description 44
- 238000002347 injection Methods 0.000 claims abstract description 36
- 239000007924 injection Substances 0.000 claims abstract description 36
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000005303 weighing Methods 0.000 claims description 14
- 239000007789 gas Substances 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 150000001299 aldehydes Chemical class 0.000 claims description 2
- 239000008098 formaldehyde solution Substances 0.000 claims description 2
- 150000002576 ketones Chemical class 0.000 claims description 2
- 230000009467 reduction Effects 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 238000012360 testing method Methods 0.000 abstract description 17
- 238000010998 test method Methods 0.000 abstract description 2
- WQOXQRCZOLPYPM-UHFFFAOYSA-N dimethyl disulfide Chemical compound CSSC WQOXQRCZOLPYPM-UHFFFAOYSA-N 0.000 description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 239000003463 adsorbent Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 6
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 6
- 239000003915 liquefied petroleum gas Substances 0.000 description 5
- 230000003068 static effect Effects 0.000 description 5
- 238000000926 separation method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- -1 ethylene, propylene Chemical group 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/08—Investigating permeability, pore-volume, or surface area of porous materials
- G01N2015/0866—Sorption
Landscapes
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention relates to a system for detecting molecular sieve adsorption capacity under high pressure and a detection method thereof, wherein the system comprises a high-pressure liquid storage tank, an impurity injection unit, a molecular sieve adsorption tank and a detection instrument which are sequentially communicated with an outlet of the high-pressure liquid storage tank, an inlet of the high-pressure liquid storage tank is communicated with an external high-pressure medium conveying pipeline, a first flow control valve and a second flow control valve are respectively arranged between the high-pressure liquid storage tank and the impurity injection unit and between the impurity injection unit and the molecular sieve adsorption tank, a pressure reducing valve is also arranged between the molecular sieve adsorption tank and the detection instrument, and the molecular sieve adsorption tank is connected with an external vacuum pump; the impurity injection unit includes at least one impurity tank. Compared with the prior art, the method can test the adsorption capacity of the molecular sieve material to different impurities under high pressure, the test method is easy to adjust the adsorption temperature, the impurity type and the impurity concentration, and the test of the co-adsorption capacity of various impurities can be realized.
Description
Technical Field
The invention belongs to the technical field of chemical detection, and relates to a system and a method for detecting the adsorption capacity of a molecular sieve under a high-pressure condition.
Background
The molecular sieve material has uniform aperture and extremely high specific surface area, can realize selective adsorption on various molecules, and has extremely high separation precision and separation rate, reversible adsorption process and wide application field as an adsorbent. The molecular sieve is often used for removing impurities in a high-pressure medium, and the presence of the impurities can influence the subsequent processes, such as dehydration, dealcoholization, desulfurization and the like of various hydrocarbons, so as to meet the purity requirements of different processes on materials. The good adsorption performance of the molecular sieve adsorbent is a basic condition of an adsorption separation process, the adsorption efficiency and the purity of the material at the outlet of the adsorber are determined, and the adsorbent with excellent adsorption performance can be selected to reduce the using amount of the adsorbent or improve the adsorption treatment capacity.
The adsorption performance of a molecular sieve material is generally evaluated by adsorption capacity, and in the currently relevant national and industrial standards of molecular sieves, the adsorption capacity is used for evaluating the relevant adsorption performance of the molecular sieve, such as static water adsorption capacity, static methanol adsorption capacity and the like. The water adsorption capacity is generally in the air under constant humidity, so that the molecular sieve material adsorbs water until the water is balanced, and the molecular sieve adsorption capacity is obtained by calculation after the water is balanced. The method for testing the water adsorption in the national standard GB/T6287 molecular sieve static water adsorption determination method comprises the following steps: and (2) stabilizing the humidity in the closed container to be 75% by using a saturated sodium chloride solution at the temperature of 35 ℃, weighing a certain amount of molecular sieve in the container, and calculating the static water adsorption capacity of the molecular sieve by a weighing method after 24 hours. The method for testing the water adsorption capacity of the US standard MIL-D-3464 comprises the following steps: at 25 ℃, the dry gas passes through concentrated sulfuric acid aqueous solution with fixed concentration, so that the water content of the outlet gas is stable; and introducing the constant-humidity gas into the molecular sieve material, and calculating by a weighing method to obtain the water adsorption capacity of the molecular sieve material. The methanol adsorption capacity is measured by a Macbain device, a method for measuring the static adsorption capacity of the methanol is specified in the Roads standard HG/T2524 < 4A molecular sieve >, during the test, a sample is arranged in a carrying basket hung on a quartz spring, the sample is heated and regenerated under the vacuum condition, then the uniformly diffused adsorption gas is adsorbed under certain pressure, after the adsorption balance, the elongation of the quartz spring in the device before and after the adsorption is measured by a height gauge, so that the mass change proportion of the molecular sieve is calculated, and the adsorption capacity (specific gravity) is obtained.
The adsorption tests reflect the adsorption capacity of the molecular sieve material, but when the molecular sieve material is frequently applied to high-pressure media such as ethylene, propylene, hydrogen, liquefied petroleum gas and the like, the adsorption capacity of the molecular sieve is greatly different under the influence of pressure and the adsorption media. Meanwhile, the method is only suitable for testing of single impurities, and can not be used for testing of multiple impurities simultaneously, in actual use, the adsorbent is usually required to remove multiple impurities, and due to the fact that the adsorption process is competitive adsorption, the multiple impurities can affect each other during co-adsorption, and have different adsorption amounts.
In the technical literature, the device is tested by using a dynamic method, the adsorption quantity of gas-phase impurities can be tested by using a double-gas-path flow method, and the adsorption test of impurities which are in a liquid phase at normal temperature and normal pressure is generally carried out by using a high-pressure medium with standard concentration of impurities. The configuration of the high-pressure medium with the standard concentration is time-consuming and high in manufacturing cost, and various standard media are required to be configured for different impurity concentrations, so that the testing device is complex and the testing process is complicated.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a system for detecting the adsorption capacity of the molecular sieve under the high-pressure condition, which does not need to be provided with a high-pressure medium with standard impurity concentration, has short detection time, high controllability and high detection precision.
It is another object of the present invention to provide a method for testing the system for testing the adsorption capacity of a molecular sieve under high pressure conditions.
The purpose of the invention can be realized by the following technical scheme:
a system for detecting molecular sieve adsorption capacity under high pressure condition, this system include high-pressure liquid storage pot, impurity injection unit, molecular sieve adsorption tank and the detecting instrument that is linked together with the export of high-pressure liquid storage pot in proper order, the import of high-pressure liquid storage pot be linked together with outside high-pressure medium conveying pipeline, high-pressure liquid storage pot and impurity injection unit between impurity injection unit and the molecular sieve adsorption tank between be equipped with first flow control valve, second flow control valve respectively, molecular sieve adsorption tank and detecting instrument between still be equipped with the relief pressure valve, and the molecular sieve adsorption tank be connected with outside vacuum pump.
The impurity injection unit includes at least one impurity tank.
When the impurity injection unit is provided with a plurality of impurity tanks, the impurity tanks are sequentially connected in series.
And a third flow control valve is arranged between each impurity tank.
The impurity tank inside be equipped with the heater, the outside is equipped with the filling opening with microsyringe looks adaptation.
The inlet and the outlet of the impurity tank are positioned on the same side, and the inlet pipe at the inlet is communicated with the bottom of the impurity tank and communicated with the outlet, so that the residue of impurity components can be avoided.
The impurities comprise one or more of water, alcohol, ether, aldehyde, ketone or aqueous solution, and the aqueous solution comprises one or more of aqueous hydrogen sulfide solution, aqueous sulfur dioxide solution, aqueous hydrochloric acid solution, aqueous formaldehyde solution, aqueous lower alcohol solution or ammonia water.
The detection instrument comprises one or more of a Karl Fischer micro-moisture meter, a dew point meter, a gas chromatograph, a gas chromatography-mass spectrometer or a microcoulomb instrument, and the detection equipment is selected according to the impurity type.
The detection method of the system for detecting the adsorption capacity of the molecular sieve under the high pressure condition specifically comprises the following steps:
(1) cleaning and drying a high-pressure liquid storage tank, an impurity injection unit and a molecular sieve adsorption tank for later use;
(2) vacuumizing the high-pressure liquid storage tank, weighing, injecting a high-pressure medium into the high-pressure liquid storage tank through an external high-pressure medium conveying pipeline, closing a valve after the high-pressure medium is filled, weighing the high-pressure liquid storage tank, and calculating to obtain the total amount of the high-pressure medium;
(3) slowly transferring a certain amount of impurities by using a microsyringe, and adding the impurities into the impurity injection unit to obtain the total amount of the impurities;
(4) transferring a certain amount of molecular sieve to be detected, adding the molecular sieve into a molecular sieve adsorption tank, vacuumizing, and weighing to obtain the total amount of the molecular sieve;
(5) communicating the high-pressure liquid storage tank, the impurity injection unit and the molecular sieve adsorption tank through pipelines;
(6) heating the impurity injection unit to heat and vaporize the impurities, and then opening the second flow control valve and the first flow control valve to make the impurities and the high-pressure medium flow into the molecular sieve adsorption tank together;
(7) placing the system in a constant temperature environment, keeping the system sealed for a certain time, opening a pressure reducing valve after materials in the system reach a balanced state, and detecting the concentration of impurities in the outlet materials after the materials flow out through pressure reduction;
(8) calculating the total amount of the non-adsorbed impurities according to the total amount of the high-pressure medium in the step (2) and the impurity concentration detected in the step (7);
(9) calculating the content of the adsorbed impurities according to the difference value between the total amount of the non-adsorbed impurities calculated in the step (8) and the total amount of the impurities in the step (3);
(10) and (4) calculating the ratio of the content of the adsorbed impurities obtained in the step (9) to the total amount of the molecular sieve in the step (4), namely the adsorption capacity of the molecular sieve.
And (4) adjusting the heating temperature in the step (6) to be 50-200 ℃ according to different impurities.
The constant temperature of the constant temperature environment in the step (7) is 25-60 ℃, and the sealing time is more than or equal to 24 hours.
In the invention, each tank body is a pressure container which can bear pressure more than or equal to 10 Mpa. The high-pressure liquid storage tank, the impurity tank and the molecular sieve adsorption tank can be selected according to different materials and impurity concentrations to meet test requirements. The impurities are in liquid phase at normal temperature and normal pressure, and can be completely vaporized after being heated.
Compared with the prior art, the invention has the following characteristics:
1) the adsorption capacity of the molecular sieve under high pressure can be tested, the adsorption temperature, the high pressure medium, the impurity types and the impurity content are changed, and the adsorption capacities of the adsorbents to the impurities under different adsorption pressures and different adsorption temperatures can be tested;
2) the detection is more flexible, and the test of the co-adsorption capacity of various impurities can be realized by increasing the number of the impurity tanks;
3) the impurities are vaporized and then are introduced into the molecular sieve adsorption tank, so that the impurities can be uniformly dispersed in the system, and the test error is avoided;
4) the method has the advantages of no need of configuring a high-pressure medium with standard impurity concentration, low manufacturing cost, short required time, high controllability of the test process, easy realization, and the test method is closer to the actual situation of industrial application, provides a new method for evaluating the molecular sieve, and provides technical data for industrial design and application.
Drawings
FIG. 1 is a schematic diagram of the system for measuring the adsorption capacity of a molecular sieve in example 1 under high pressure conditions;
the notation in the figure is:
1-high pressure liquid storage tank, 2-first impurity tank, 3-second impurity tank, 4-molecular sieve adsorption tank, 5-first flow control valve, 6-second flow control valve, 7-third flow control valve and 8-pressure reducing valve.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1:
as shown in fig. 1, a high-pressure liquid storage tank 1, a first impurity tank 2, a second impurity tank 3 and a molecular sieve adsorption tank 4 are cleaned, dried and vacuumized for later use. The high pressure liquid storage tank 1 is evacuated, weighed and recorded. The high-pressure liquid storage tank is connected to a liquefied petroleum gas filling system, and the liquefied petroleum gas is filled into the high-pressure liquid storage tank 1 by opening a valve. After filling, the valve is closed, the high-pressure liquid storage tank 1 is weighed, and the mass of filled liquefied petroleum gas is 2430g through calculation. Slowly transferring 2.5g of water by using a microsyringe and adding the water into the first impurity tank 2; slowly transferring 0.8g of dimethyl disulfide into a second impurity tank 3 by using a microsyringe, weighing 10.0g of fresh 13X molecular sieve sample, adding the fresh 13X molecular sieve sample into a molecular sieve adsorption tank 4, and vacuumizing; connecting a high-pressure liquid storage tank 1, a first impurity tank 2, a second impurity tank 3 and a molecular sieve adsorption tank 4 through pipelines; turning on a heater in the impurity tank, heating to 110 ℃, respectively heating and vaporizing the moisture and the dimethyl disulfide in the first impurity tank 2 and the second impurity tank 3, turning on a third flow control valve 7 and a second flow control valve 6 to make the vaporized impurities flow into a molecular sieve adsorption tank 4, and turning off the heater; opening a first flow control valve 5 to enable the liquefied petroleum gas to flow into a molecular sieve adsorption tank 4; placing the system in a constant temperature environment of 30 ℃, keeping the system sealed for 48 hours, reducing the pressure through a pressure reducing valve 8, and detecting through a Karl Fischer micro-moisture meter to obtain the water content of an outlet material of 322 ppm; detecting by a gas chromatograph to obtain 275ppm of outlet dimethyl disulfide; according to the total amount of materials, calculating to obtain the content of unadsorbed water to be 0.782g and the content of dimethyl disulfide to be 0.668 g; the adsorbed water content was 1.718g, and the adsorbed dimethyldisulfide was 0.132 g; the adsorption capacity of the 13X molecular sieve for water under the conditions was calculated to be 17.71% and the adsorption capacity for dimethyldisulfide was calculated to be 1.32%.
Example 2:
and cleaning, drying and vacuumizing the high-pressure liquid storage tank 1, the first impurity tank 2 and the molecular sieve adsorption tank 4 for later use. The high pressure liquid storage tank 1 is evacuated, weighed and recorded. The high-pressure propylene filling system is connected with the high-pressure propylene filling system, and the high-pressure liquid storage tank 1 is filled with propylene by opening a valve. After filling, the valve is closed, the high-pressure liquid storage tank 1 is weighed, and the mass of filled propylene is calculated to be 2590 g. Slowly transferring 2g of water by using a microsyringe and adding the water into the first impurity tank 2; weighing 12.0g of fresh 3A molecular sieve sample, adding the sample into a molecular sieve adsorption tank 4, and vacuumizing; connecting a high-pressure liquid storage tank 1, a first impurity tank 2 and a molecular sieve adsorption tank 4 through pipelines; opening a heater of the first impurity tank 2, heating to 100 ℃, heating and vaporizing the water in the first impurity tank 2, opening a second flow control valve 6, making the vapor heated and vaporized flow into a molecular sieve adsorption tank 4, and closing the heater; opening a first flow control valve 5 to enable propylene to flow into a molecular sieve adsorption tank 4; placing the system in a constant temperature environment of 25 ℃, keeping the system sealed for 24 hours, reducing the pressure through a pressure reducing valve 8, and detecting through a Karl Fischer micro-moisture meter to obtain the water content of the outlet material of 214 ppm; according to the total amount of propylene materials, the content of non-adsorbed impurities is calculated to be 0.554 g; the total amount of adsorbed impurities was 1.446 g; the adsorption capacity of the 3A molecular sieve is calculated to be 12.05%.
Example 3
The system for detecting the molecular sieve adsorption capacity under the high-pressure condition comprises a high-pressure liquid storage tank 1, an impurity injection unit, a molecular sieve adsorption tank 4 and a detection instrument, wherein the impurity injection unit is sequentially communicated with an outlet of the high-pressure liquid storage tank 1, an inlet of the high-pressure liquid storage tank 1 is communicated with an external high-pressure medium conveying pipeline, a first flow control valve 5 and a second flow control valve 6 are respectively arranged between the high-pressure liquid storage tank 1 and the impurity injection unit and between the impurity injection unit and the molecular sieve adsorption tank 4, a pressure reducing valve 8 is further arranged between the molecular sieve adsorption tank 4 and the detection instrument, and the molecular sieve adsorption tank 4 is connected with an external vacuum.
In this embodiment, the impurity injection unit is composed of 3 impurity tanks connected in series in sequence, and a third flow control valve 7 is provided between each impurity tank. The impurity tank is internally provided with a heater, and the outside of the impurity tank is provided with an injection port matched with the microsyringe. The inlet and the outlet of the impurity tank are positioned on the same side, and the inlet pipe at the inlet is communicated with the bottom of the impurity tank and communicated with the outlet.
The detection method of the system of the embodiment specifically comprises the following steps:
(1) cleaning and drying the high-pressure liquid storage tank 1, the impurity injection unit and the molecular sieve adsorption tank 4 for later use;
(2) vacuumizing the high-pressure liquid storage tank 1, weighing, injecting a high-pressure medium into the high-pressure liquid storage tank 1 through an external high-pressure medium conveying pipeline, closing a valve after the high-pressure medium is filled, weighing the high-pressure liquid storage tank 1, and calculating to obtain the total amount of the high-pressure medium;
(3) slowly transferring a certain amount of impurities by using a microsyringe, and adding the impurities into the impurity injection unit to obtain the total amount of the impurities;
(4) transferring a certain amount of molecular sieve to be detected, adding the molecular sieve into a molecular sieve adsorption tank 4, vacuumizing, and weighing to obtain the total amount of the molecular sieve;
(5) the high-pressure liquid storage tank 1, the impurity injection unit and the molecular sieve adsorption tank 4 are communicated through pipelines;
(6) heating the impurity injection unit to heat and vaporize the impurities, and then sequentially opening a second flow control valve 6 and a first flow control valve 5 to make the impurities and the high-pressure medium flow into the molecular sieve adsorption tank 4 together;
(7) placing the system in a constant temperature environment, keeping the system sealed for a certain time, opening the pressure reducing valve 8 after the materials in the system reach a balanced state, and detecting the concentration of impurities in the outlet materials after the materials flow out under reduced pressure;
(8) calculating the total amount of the non-adsorbed impurities according to the total amount of the high-pressure medium in the step (2) and the impurity concentration detected in the step (7);
(9) calculating the content of the adsorbed impurities according to the difference value between the total amount of the non-adsorbed impurities calculated in the step (8) and the total amount of the impurities in the step (3);
(10) and (4) calculating the ratio of the content of the adsorbed impurities obtained in the step (9) to the total amount of the molecular sieve in the step (4), namely the adsorption capacity of the molecular sieve.
In this embodiment, the high-pressure medium is compressed nitrogen.
In this embodiment, the impurities are water, ethanol, and formalin, and the heating temperature of the impurity injection unit is 105 ℃.
In this embodiment, the detection instrument is a karl fischer micro-moisture meter or a gas chromatograph.
In this example, the constant temperature of the constant temperature environment in step (7) was 60 ℃, and the time for keeping the enclosure was 24 hours.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (7)
1. The system for detecting the adsorption capacity of the molecular sieve under the high-pressure condition is characterized by comprising a high-pressure liquid storage tank, an impurity injection unit, a molecular sieve adsorption tank and a detection instrument, wherein the impurity injection unit, the molecular sieve adsorption tank and the detection instrument are sequentially communicated with an outlet of the high-pressure liquid storage tank, an inlet of the high-pressure liquid storage tank is communicated with an external high-pressure medium conveying pipeline, a first flow control valve and a second flow control valve are respectively arranged between the high-pressure liquid storage tank and the impurity injection unit and between the impurity injection unit and the molecular sieve adsorption tank, a pressure reducing valve is also arranged between the molecular sieve adsorption tank and the detection instrument, the molecular sieve adsorption tank is connected with an external vacuum pump,
the impurity injection unit comprises at least one impurity tank, a heater is arranged in the impurity tank, an injection port matched with the microsyringe is arranged outside the impurity tank, impurities are injected through the injection port, the impurities comprise one or more of water, alcohol, ether, aldehyde, ketone or aqueous solution, and the aqueous solution comprises one or more of aqueous hydrogen sulfide solution, aqueous sulfur dioxide solution, aqueous hydrochloric acid solution, aqueous formaldehyde solution, aqueous low-carbon alcohol solution or aqueous ammonia.
2. The system according to claim 1, wherein the impurity injection unit comprises a plurality of impurity tanks, and the impurity tanks are connected in series.
3. The system for detecting the adsorption capacity of the molecular sieve under the high pressure condition of claim 2, wherein a third flow control valve is respectively arranged between each impurity tank.
4. The system according to claim 3, wherein the inlet and the outlet of the canister are located on the same side, and the inlet pipe at the inlet opens into the bottom of the canister and communicates with the outlet.
5. The system for detecting the adsorption capacity of a molecular sieve under high pressure according to claim 1, wherein the detection instrument comprises one or more of a karl fischer micro-moisture meter, a dew point meter, a gas chromatograph-mass spectrometer, or a microcoulomb spectrometer.
6. The method of any one of claims 1 to 5, wherein the method comprises the following steps:
(1) cleaning and drying a high-pressure liquid storage tank, an impurity injection unit and a molecular sieve adsorption tank for later use;
(2) vacuumizing the high-pressure liquid storage tank, weighing, injecting a high-pressure medium into the high-pressure liquid storage tank through an external high-pressure medium conveying pipeline, closing a valve after the high-pressure medium is filled, weighing the high-pressure liquid storage tank, and calculating to obtain the total amount of the high-pressure medium;
(3) slowly transferring a certain amount of impurities by using a microsyringe, and adding the impurities into the impurity injection unit to obtain the total amount of the impurities;
(4) transferring a certain amount of molecular sieve to be detected, adding the molecular sieve into a molecular sieve adsorption tank, vacuumizing, and weighing to obtain the total amount of the molecular sieve;
(5) communicating the high-pressure liquid storage tank, the impurity injection unit and the molecular sieve adsorption tank through pipelines;
(6) heating the impurity injection unit to heat and vaporize the impurities, and then opening the second flow control valve and the first flow control valve to make the impurities and the high-pressure medium flow into the molecular sieve adsorption tank together;
(7) placing the system in a constant temperature environment, keeping the system sealed for a certain time, opening a pressure reducing valve after materials in the system reach a balanced state, and detecting the concentration of impurities in the outlet materials after the materials flow out through pressure reduction;
(8) calculating the total amount of the non-adsorbed impurities according to the total amount of the high-pressure medium in the step (2) and the impurity concentration detected in the step (7);
(9) calculating the content of the adsorbed impurities according to the difference value between the total amount of the non-adsorbed impurities calculated in the step (8) and the total amount of the impurities in the step (3);
(10) and (4) calculating the ratio of the content of the adsorbed impurities obtained in the step (9) to the total amount of the molecular sieve in the step (4), namely the adsorption capacity of the molecular sieve.
7. The method for detecting the system for detecting the adsorption capacity of the molecular sieve under the high pressure condition as claimed in claim 6, wherein the constant temperature of the constant temperature environment in the step (7) is 25-60 ℃, and the sealing time is not less than 24 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611102790.XA CN107340214B (en) | 2016-12-05 | 2016-12-05 | System for detecting adsorption capacity of molecular sieve under high pressure condition and detection method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611102790.XA CN107340214B (en) | 2016-12-05 | 2016-12-05 | System for detecting adsorption capacity of molecular sieve under high pressure condition and detection method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107340214A CN107340214A (en) | 2017-11-10 |
| CN107340214B true CN107340214B (en) | 2019-12-20 |
Family
ID=60222354
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611102790.XA Active CN107340214B (en) | 2016-12-05 | 2016-12-05 | System for detecting adsorption capacity of molecular sieve under high pressure condition and detection method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107340214B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110850024B (en) * | 2018-08-21 | 2021-11-09 | 中国计量科学研究院 | Water detection calibration system, detection model establishing method and water detection method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202126379U (en) * | 2011-04-20 | 2012-01-25 | 中国石油化工股份有限公司 | Device for measuring adsorption capacity of molecular sieves |
| CN102749259A (en) * | 2011-04-20 | 2012-10-24 | 中国石油化工股份有限公司 | Method for determining adsorption quantity of molecular sieve |
| CN104792908A (en) * | 2015-04-20 | 2015-07-22 | 中国石油大学(华东) | Detection device and detection method for detecting secondary migration effect of oil-gas component |
| CN105158489A (en) * | 2015-07-30 | 2015-12-16 | 中国石油大学(华东) | Supercritical-state gas adsorption desorption apparatus and application method thereof |
| CN106018166A (en) * | 2016-04-28 | 2016-10-12 | 河南理工大学 | Multicomponent gas adsorption simulation experiment method and device |
-
2016
- 2016-12-05 CN CN201611102790.XA patent/CN107340214B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN202126379U (en) * | 2011-04-20 | 2012-01-25 | 中国石油化工股份有限公司 | Device for measuring adsorption capacity of molecular sieves |
| CN102749259A (en) * | 2011-04-20 | 2012-10-24 | 中国石油化工股份有限公司 | Method for determining adsorption quantity of molecular sieve |
| CN104792908A (en) * | 2015-04-20 | 2015-07-22 | 中国石油大学(华东) | Detection device and detection method for detecting secondary migration effect of oil-gas component |
| CN105158489A (en) * | 2015-07-30 | 2015-12-16 | 中国石油大学(华东) | Supercritical-state gas adsorption desorption apparatus and application method thereof |
| CN106018166A (en) * | 2016-04-28 | 2016-10-12 | 河南理工大学 | Multicomponent gas adsorption simulation experiment method and device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107340214A (en) | 2017-11-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Furukawa et al. | Independent verification of the saturation hydrogen uptake in MOF-177 and establishment of a benchmark for hydrogen adsorption in metal–organic frameworks | |
| CN103994943B (en) | A kind of coal/shale adsorption isotherm experiment device | |
| CN206057126U (en) | A kind of shale multi component adsorption experimental provision | |
| CN102749259B (en) | The method of molecular sieve adsorption quantitative determination | |
| CN104897525A (en) | Diffusion coefficient and isothermal adsorption/desorption curve test system and method | |
| CN108226322A (en) | A kind of low temperature concentrating instrument and control method | |
| CN107340214B (en) | System for detecting adsorption capacity of molecular sieve under high pressure condition and detection method thereof | |
| CN104399353A (en) | Methane-carbon dioxide-nitrogen gas or hydrogen gas multi-component separation method and device | |
| CN114279890B (en) | System and method for measuring liquid volume under high pressure | |
| CN112284651A (en) | Method for detecting interlayer vacuum degree of low-temperature storage tank | |
| CN114797367A (en) | Device and method for testing and evaluating low-temperature adsorption performance of adsorbent | |
| CN109696380A (en) | A kind of method and device for evaluating poromerics gas separating property | |
| CN114646571A (en) | Low-temperature high-pressure adsorption measuring device and method for measuring adsorption quantity of material gas | |
| CN111948092B (en) | Shale reservoir gas content testing device and method | |
| CN101701900B (en) | Device and method for testing absorbance by electric quantity method | |
| CN109323909B (en) | Gas automatic separation system for inertness in small-gas-volume environment sample | |
| JP6618672B2 (en) | Porous substance characteristic measuring apparatus and porous substance characteristic measuring method | |
| CN201387413Y (en) | Adsorbent precision tester | |
| CN202126379U (en) | Device for measuring adsorption capacity of molecular sieves | |
| CN111077039B (en) | Device and method for measuring physical oxygen uptake, chemical oxygen uptake and true density of coal | |
| CN107543772A (en) | A kind of porous material saturated extent of adsorption determines device and method | |
| CN210803224U (en) | Volumetric method isobaric adsorption tester | |
| CN112666042A (en) | Novel experiment device for detecting performance of adsorbent | |
| CN112504904B (en) | Gas adsorption isotherm test analysis method for rock under different water-containing conditions | |
| CN116735419B (en) | System and method for measuring adsorption capacity of adsorbent at low temperature |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |