CN114441366A - Device and method for quantitatively determining surface acidity of material - Google Patents
Device and method for quantitatively determining surface acidity of material Download PDFInfo
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- CN114441366A CN114441366A CN202011195959.7A CN202011195959A CN114441366A CN 114441366 A CN114441366 A CN 114441366A CN 202011195959 A CN202011195959 A CN 202011195959A CN 114441366 A CN114441366 A CN 114441366A
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- 239000000463 material Substances 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 25
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002253 acid Substances 0.000 claims abstract description 21
- 238000005259 measurement Methods 0.000 claims abstract description 14
- 239000000523 sample Substances 0.000 claims description 80
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000001179 sorption measurement Methods 0.000 claims description 18
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 12
- 230000000875 corresponding effect Effects 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000000746 purification Methods 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000003068 molecular probe Substances 0.000 claims description 5
- 238000009489 vacuum treatment Methods 0.000 claims description 5
- 229910000889 permalloy Inorganic materials 0.000 claims description 3
- 238000003556 assay Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 230000002596 correlated effect Effects 0.000 claims description 2
- 238000002336 sorption--desorption measurement Methods 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 description 11
- 230000002378 acidificating effect Effects 0.000 description 4
- 238000003795 desorption Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- -1 carbonium ions Chemical class 0.000 description 2
- 238000004517 catalytic hydrocracking Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000011973 solid acid Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/02—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness
- G01B7/04—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness specially adapted for measuring length or width of objects while moving
- G01B7/042—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness specially adapted for measuring length or width of objects while moving for measuring length
- G01B7/046—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring length, width or thickness specially adapted for measuring length or width of objects while moving for measuring length using magnetic means
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
A device and method for quantitative determination of material surface acidity, including a hollow measuring tube, set up a spring hung on the top in the measuring tube, connect a sample basket under the spring, mount an iron core between sample basket and the spring, install the toroidal differential transformer on the measuring tube outer wall corresponding to said iron core level, the said differential transformer connects the program control system externally, and can output the voltage signal change that the iron core causes while moving up and down to the program control system; the invention determines the amount and distribution of acid on the surface of the material by measuring the spring deformation caused by the change of the weight of the sample through a differential transformer. The device has wide application range and high result accuracy, automatically completes the measurement in the measurement process, reduces manual operation, and is easy and convenient to implement.
Description
Technical Field
The invention relates to the technical field of material characterization, in particular to a device and a method for quantitatively determining surface acidity of a material.
Background
The acidic sites of materials such as solid acid catalysts are generally regarded as active sites on the surface of oxide catalysts, hydrocarbon molecules and the acidic sites on the surface interact to form carbonium ions, namely intermediate products of the reaction in catalytic cracking, isomerization, polymerization and other reactions, and the carbonium ions can successfully explain the reaction of hydrocarbons on the acidic surface theoretically, and provide strong evidence for the existence of the acidic sites. In order to characterize the properties of the material, the acid strength and the amount of acid at the surface acid sites need to be determined.
Pyridine was the first probe molecule proposed for determining the acidity of the catalyst surface. In the experimental process, pyridine is adsorbed on the purified catalyst in a saturated mode, then high-vacuum desorption is carried out under different temperature conditions, the weight change of the catalyst is measured in real time by using a spring scale, and the acid strength distribution and the calculated amount of the catalyst can be obtained.
The existing method for measuring the infrared acid is a gravimetric method, namely a spring balance is adopted to measure the acidity of the catalyst, but the device has large volume and complicated operation, most importantly, a height measuring instrument with high price is used, and the error caused by measurement is large because manual observation and conversion are needed. In order to facilitate the measurement of the acidity of the catalytic material and improve the accuracy and the repeatability of an acidity measurement result, a device and a method for measuring the acidity of the catalytic material are urgently needed to be established, so that the acidity information on the surface of the material can be conveniently, quickly and accurately measured, and the measurement accuracy and the repeatability are improved.
Disclosure of Invention
In order to solve the problems of large volume, complex operation and large measurement result error of a material surface acidity measurement device in the prior art, the invention provides a device and a method for quantitatively measuring the material surface acidity.
The technical purpose of the invention is realized by the following technical scheme:
the technical purpose of the first aspect of the invention is to provide a device for quantitatively determining the acidity of the surface of a material, which comprises a hollow measuring tube, wherein a spring hung at the top is arranged in the measuring tube, a sample basket is connected below the spring, an iron core is arranged between the spring and the sample basket, an annular differential transformer is arranged on the outer wall of the measuring tube horizontally corresponding to the iron core, the differential transformer is externally connected with a program control system, and the change of a voltage signal caused when the iron core moves up and down can be output to the program control system; the periphery of the sample basket is provided with a heating device, the heating device is arranged outside the measuring tube, a temperature detection device is arranged beside the sample basket, the heating device and the temperature detection device are both connected with a temperature control system outside the measuring tube, and the temperature control system is connected with a program control system; the measuring tube is also connected with an adsorption probe molecular tube and a vacuum system.
Furthermore, the differential transformer is composed of 2-3 groups of electromagnetic coils.
Further, the iron core is made of permalloy.
Further, the measuring tube between the heating device and the sample basket is made of quartz glass, and the sample basket is made of quartz glass.
Further, the heating device is a heating furnace; the temperature detection device is a thermocouple.
Furthermore, the adsorption probe molecule tube is a pyridine tube.
Furthermore, the vacuum system is a mode of combining a molecular turbine pump and a mechanical pump, and the vacuum degree of the system reaches 10-4Pa。
The technical purpose of the second aspect of the invention is to provide a method for quantitative determination of material surface acidity by using the device, which comprises the following steps:
starting a program control system, recording a voltage output value of the differential transformer in an initial state, when a sample to be detected is put into a sample basket, the vacuum degree is adjusted through a vacuum system, the temperature is adjusted through a heating device, and an adsorption probe molecular tube is opened to enable the sample to adsorb a molecular probe under different conditions, the spring deforms due to the change of the weight of the sample, an iron core moves along with the deformation of the spring, the voltage of the differential transformer changes, the change information is output to the program control system, the change of the voltage output information of the differential transformer under different conditions corresponds to the length change of the spring under different conditions, and then the change of the weight and the weight of the sample are correlated, so that quantitative acid information is obtained.
Further, as a more specific embodiment, the specific steps of the assay are as follows:
(1) starting a program control system and recording the voltage output value of the differential transformer in an initial state;
(2) putting a sample to be measured with a certain weight into the sample basket, lengthening the spring, moving the iron core along with the spring to cause the voltage of the differential transformer to change, outputting the change information to a program control system, and correlating the change of the length of the spring with the change of the weight of the sample;
(3) adjusting the vacuum degree through a vacuum system, adjusting the temperature through a heating device, performing high-temperature and high-vacuum purification treatment on the sample, cooling to room temperature after the purification is completed, and automatically recording the voltage change of the differential transformer through a program control system; opening an adsorption probe molecular tube to enable a sample to adsorb a molecular probe, closing the probe molecular adsorption tube after adsorption balance, starting program heating and vacuum treatment, and obtaining voltage information change output by a differential transformer under different temperatures and pressures so as to obtain quantitative acidity information of the sample to be detected under different measurement conditions;
(4) after all temperature points are measured, the conversion relation between the length of the spring and the weight of the sample is obtained according to the voltage change information of the differential transformer, and the acid amount and the acid strength distribution of the sample at different temperatures can be obtained.
In the above measurement method, it should be understood by those skilled in the art that, in step (3), during the process of starting program temperature rise and vacuum treatment after adsorption equilibrium, the mass of the sample after adsorption of probe molecules is continuously changed due to continuous temperature change, which causes spring deformation, and the program control system obtains spring deformation information by recording the voltage change information of the differential transformer; and (3) maintaining the programmed temperature at a plurality of preset temperature points for a period of time respectively to enable the sample to reach an adsorption-desorption equilibrium state at the corresponding temperature, and then recording the voltage change information of the differential transformer at the corresponding temperature points respectively.
The invention has the following advantages:
(1) the device can quantitatively determine the acid amount and the acid strength distribution of various catalyst materials, has wide application range and high result accuracy and repeatability, automatically completes determination in the determination process, reduces manual operation, and is easy and convenient to implement;
(2) the device utilizes the iron core and the differential transformer to measure the length change of the spring, does not need an expensive height measuring instrument, and has the advantages of small volume, convenient operation and the like;
(3) the acidity measuring device can be completely packaged in an instrument shell to form a conventional analytical instrument which can be directly placed on a test bed, and help is provided for development of new catalytic materials.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
FIG. 1 is a schematic view of an apparatus for quantitative determination of surface acidity of a material according to the present invention;
the device comprises a measuring tube 1, a spring 2, a differential transformer 3, an iron core 4, a heating furnace 5, a sample basket 6, a sample 7, a thermocouple 8, a pyridine tube 9, a vacuum system 10, a program control system 11 and a temperature control system 12.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
Example 1
The embodiment discloses a device for quantitatively determining the acidity of a material surface, which is shown in figure 1:
the device comprises a hollow measuring tube 1, wherein a spring 2 hung at the top is arranged in the measuring tube 1, a sample basket 6 is connected below the spring 2, and the sample basket 6 is made of quartz glass; between the spring 2 and the sample basket 6Installing an iron core 4, wherein the iron core 4 is made of permalloy, an annular differential transformer 3 is installed on the outer wall of a measuring tube horizontally corresponding to the iron core 4, the differential transformer 3 is composed of 2-3 groups of electromagnetic coils, the differential transformer 3 is externally connected with a program control system 11, and voltage signal change caused when the iron core 4 moves up and down can be output to the program control system 11; the periphery of the sample basket 6 is provided with a heating furnace 5, the heating furnace 5 is arranged outside the measuring tube 1, and the measuring tube 1 between the heating furnace 5 and the sample basket 6 is made of quartz glass; a thermocouple 8 is arranged beside the sample basket 6, the heating furnace 5 and the thermocouple 8 are both connected with a temperature control system 12 outside the measuring tube 1, and the temperature control system 12 is connected with a program control system 11; the measuring tube 1 is also connected with a pyridine tube 9 and a vacuum system 10, the vacuum system 10 is a combination mode of a molecular turbine pump and a mechanical pump, and the vacuum degree of the system can reach 10-4Pa。
Example 2
This example discloses a method for quantitative determination of the acidity of a material surface using the apparatus of example 1:
(1) starting the program control system 11, and recording the voltage output value of the differential transformer 3 in the initial state;
(2) a sample 7 to be measured with a certain weight is put into the sample basket 6, the spring 2 is lengthened, the iron core 4 moves along with the sample basket, the voltage of the differential transformer 3 is changed, the change information is output to the program control system 11, and the change information corresponds to the change of the length of the spring 2 and is related to the change of the sample weight;
(3) the vacuum degree is adjusted by a vacuum system 10, the temperature is adjusted by a thermocouple 8, the sample 7 is purified at high temperature and high vacuum, the temperature is reduced to room temperature after purification is finished, and a program control system 11 automatically records the voltage change of the differential transformer 3; opening a pyridine tube 9 to enable a sample 7 to adsorb the molecular probe, closing the pyridine tube 9 after adsorption balance, starting program heating and vacuum treatment, and obtaining voltage change information output by the differential transformer 3 under certain temperature and pressure and correlation information of sample weight change, thereby obtaining quantitative acidity information of the sample to be measured under the measurement condition; then changing the temperature and pressure, the same method can obtain the measured data under different measuring conditions;
(4) after all temperature points are measured, the conversion relation between the length of the spring 2 and the weight of the sample is obtained according to the voltage change information, and the acid amount and the acid strength distribution of the sample at different temperatures can be obtained.
Example 3
This example discloses the process of quantitatively determining the surface acidity of a particular catalyst material using the apparatus and method of examples 1 and 2:
(1) starting a program control system 11, recording the voltage output value of the differential transformer 3 in the initial state, and corresponding to the state of the initial spring 2;
(2) adding 0.2g of a hydrocracking catalyst sample 7 to be tested into a sample basket 6, starting a vacuum system 10 and a temperature control system 12, and measuring the voltage output change of the differential transformer 3 when the weight change of the sample 7 to be tested is measured in real time by the cooperation of the spring 2, the iron core 4 and the differential transformer 3, wherein the voltage output change corresponds to the change of the spring 2. After the sample 7 to be detected is subjected to high-temperature and high-vacuum purification treatment (4 hours), the pyridine pipe 9 is opened, the pyridine is adsorbed to the sample 7 to be detected in a steam form, the programmed heating and high-vacuum purification treatment processes are started after the adsorption is balanced, the desorption temperatures are respectively 160 ℃, 250 ℃, 350 ℃ and 450 ℃, the constant-temperature desorption is carried out for 1 hour in each stage, pyridine molecules are continuously desorbed, and the weight change of the sample is measured in real time. The device is automatically tested during the whole testing process, and the vacuum system 10 and the temperature control system 12 are closed. And after the desorption process is finished, converting the acid amount and the acid strength distribution of the sample to be detected according to the weight change of the sample to be detected 7 before and after the pyridine is adsorbed. The results of the measurements were 5 times each and are shown in Table 1. Wherein the acid strength unit is mmol/g.
The acid strength of the same hydrocracking catalyst is measured by a traditional method, and the measurement is carried out for 5 times respectively, and errors are compared. The results are shown in Table 2, where the acid strength is in mmol/g.
Table 1.
Table 2.
Claims (10)
1. A device for quantitatively determining the acidity of the surface of a material is characterized by comprising a hollow measuring tube, wherein a spring hung at the top is arranged in the measuring tube, a sample basket is connected below the spring, an iron core is arranged between the spring and the sample basket, an annular differential transformer is arranged on the outer wall of the measuring tube horizontally corresponding to the iron core, and the differential transformer is externally connected with a program control system and can output voltage signal change caused by the up-and-down movement of the iron core to the program control system; the periphery of the sample basket is provided with a heating device, the heating device is arranged outside the measuring tube, a temperature detection device is arranged beside the sample basket, the heating device and the temperature detection device are both connected with a temperature control system outside the measuring tube, and the temperature control system is connected with a program control system; the measuring tube is also connected with an adsorption probe molecular tube and a vacuum system.
2. The device of claim 1, wherein the differential transformer is comprised of 2-3 sets of electromagnetic coils.
3. The apparatus of claim 1, wherein the core is of permalloy material.
4. The apparatus of claim 1, wherein the measurement tube between the heating device and the sample basket is of quartz glass material.
5. The apparatus of claim 1, wherein the heating device is a furnace; the temperature detection device is a thermocouple.
6. The device of claim 1, wherein the adsorption probe molecule tube is a pyridine tube.
7. The device according to claim 1, wherein the vacuum system is a combination of a molecular turbine pump and a mechanical pump, and the vacuum degree of the system is 10-4Pa。
8. A method for quantitative determination of the acidity of the surface of a material by using the device according to any one of claims 1 to 7, comprising the following steps:
starting a program control system, recording a voltage output value of the differential transformer in an initial state, when a sample to be detected is put into a sample basket, the vacuum degree is adjusted through a vacuum system, the temperature is adjusted through a heating device, and an adsorption probe molecular tube is opened to enable the sample to adsorb a molecular probe under different conditions, the spring deforms due to the change of the weight of the sample, an iron core moves along with the deformation of the spring, the voltage of the differential transformer changes, the change information is output to the program control system, the change of the voltage output information of the differential transformer under different conditions corresponds to the length change of the spring under different conditions, and then the change of the weight and the weight of the sample are correlated, so that quantitative acid information is obtained.
9. The method according to claim 9, wherein the specific steps of the assay are as follows:
(1) starting a program control system and recording the voltage output value of the differential transformer in an initial state;
(2) putting a sample to be measured with a certain weight into the sample basket, lengthening the spring, moving the iron core along with the spring to cause the voltage of the differential transformer to change, outputting the change information to a program control system, and correlating the change of the length of the spring with the change of the weight of the sample;
(3) adjusting the vacuum degree through a vacuum system, adjusting the temperature through a heating device, performing high-temperature and high-vacuum purification treatment on the sample, cooling to room temperature after the purification is completed, and automatically recording the voltage change of the differential transformer through a program control system; opening an adsorption probe molecular tube to enable a sample to adsorb a molecular probe, closing the probe molecular adsorption tube after adsorption balance, starting program heating and vacuum treatment, and obtaining voltage information change output by a differential transformer under different temperatures and pressures so as to obtain quantitative acidity information of the sample to be detected under different measurement conditions;
(4) after all temperature points are measured, the conversion relation between the length of the spring and the weight of the sample is obtained according to the voltage change information of the differential transformer, and the acid amount and the acid strength distribution of the sample at different temperatures can be obtained.
10. The method according to claim 9, wherein in the step (3), in the process of starting program heating and vacuum treatment after adsorption equilibrium, the mass of the sample after adsorption of probe molecules is continuously changed due to continuous temperature change to cause spring deformation, and the program control system obtains the spring deformation information by recording the voltage change information of the differential transformer; and (3) maintaining the programmed temperature at a plurality of preset temperature points for a period of time respectively to enable the sample to reach an adsorption-desorption equilibrium state at the corresponding temperature, and then recording the voltage change information of the differential transformer at the corresponding temperature points respectively.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114965927A (en) * | 2022-05-24 | 2022-08-30 | 鲁东大学 | Portable water quality observation equipment |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114965927A (en) * | 2022-05-24 | 2022-08-30 | 鲁东大学 | Portable water quality observation equipment |
| CN114965927B (en) * | 2022-05-24 | 2023-11-21 | 鲁东大学 | Portable water quality observation equipment |
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Effective date of registration: 20240108 Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Applicant after: CHINA PETROLEUM & CHEMICAL Corp. Applicant after: Sinopec (Dalian) Petrochemical Research Institute Co.,Ltd. Address before: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Applicant before: CHINA PETROLEUM & CHEMICAL Corp. Applicant before: DALIAN RESEARCH INSTITUTE OF PETROLEUM AND PETROCHEMICALS, SINOPEC Corp. |