CN114441369A - Device and method for quantitatively detecting acidity of material surface - Google Patents
Device and method for quantitatively detecting acidity of material surface Download PDFInfo
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- CN114441369A CN114441369A CN202011195996.8A CN202011195996A CN114441369A CN 114441369 A CN114441369 A CN 114441369A CN 202011195996 A CN202011195996 A CN 202011195996A CN 114441369 A CN114441369 A CN 114441369A
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- 239000000463 material Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000002253 acid Substances 0.000 claims abstract description 20
- 238000005259 measurement Methods 0.000 claims abstract description 17
- 239000000523 sample Substances 0.000 claims description 82
- 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 22
- 238000006073 displacement reaction Methods 0.000 claims description 18
- 238000001179 sorption measurement Methods 0.000 claims description 17
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 12
- 238000000746 purification Methods 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001514 detection method Methods 0.000 claims description 7
- 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
- 238000003556 assay Methods 0.000 claims description 2
- 238000001816 cooling Methods 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
- 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
- 230000003760 hair shine Effects 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B11/00—Measuring arrangements characterised by the use of optical techniques
- G01B11/02—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
- G01B11/04—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness specially adapted for measuring length or width of objects while moving
- G01B11/043—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness specially adapted for measuring length or width of objects while moving for measuring length
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- General Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
A device and method for quantitative determination of material surface acidity, comprising a hollow measuring tube, a spring suspended on the top of the measuring tube is arranged in the measuring tube, and a sample basket is connected below the spring; a reflector is arranged between the spring and the sample basket, a light source and a detector are arranged outside the measuring tube corresponding to the position of the reflector, and when the position and the length of the reflector and the detector enable the reflector to move up and down along with the spring, light emitted by the light source can irradiate the reflector and be reflected to the detector to be captured, and is externally connected with a program control system and a temperature control system; the invention determines the spring deformation caused by the weight change of the sample by a laser reflection distance measurement mode, and determines the surface acid amount and distribution of the measured material. 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 detecting 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, and the weight change of the catalyst is measured in real time by using a spring scale, so that the acid strength distribution and the acid 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 determination of the acidity of the catalytic material and improve the accuracy and the repeatability of an acidity determination result, a device and a method for determining the acidity of the catalytic material are needed to be established, so that the acidity information of the surface of the material can be conveniently, quickly and accurately determined, and the determination accuracy and the repeatability are improved.
Disclosure of Invention
The invention provides a device and a method for quantitatively detecting the acidity of a material surface, aiming at solving the problems of large volume, complex operation and large error of a measurement result of a material surface acidity measurement device in the prior art.
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 detecting 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, a reflecting mirror is arranged between the spring and the sample basket, a light source and a detector are arranged outside the measuring tube corresponding to the position of the reflecting mirror, and when the positions and the lengths of the reflecting mirror and the detector enable the reflecting mirror to move up and down along with the spring, light emitted by the light source can irradiate the reflecting mirror and be reflected to the detector to be captured; 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.
Further, the light source is a laser light source; the detector is an array detector.
Further, the light source, the reflector and the detector are in a vertical plane, and the surface of the detector is larger than the diameter of a light spot reflected when the reflector moves.
Furthermore, the material of the corresponding measuring tube part on the light path formed by the light source, the reflector and the detector is a light-transmitting material.
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 detection of material surface acidity by using the device, which comprises the following steps:
starting a light source and a program control system, recording the initial position of reflected light detected by a detector, when a sample to be detected is placed in a sample basket, the vacuum degree is adjusted through a vacuum system, the temperature is adjusted through a heating device, an adsorption probe molecular tube is opened to enable the sample to adsorb molecular probes under different conditions, a spring deforms due to the change of the weight of the sample, the position of a reflector changes, the position of the reflected light detected by the detector changes accordingly, the program control system records the displacement change information of the reflected light under different conditions, the length change of the spring under different conditions corresponds to the length change of the spring under different conditions, and then the displacement change information is associated with the weight and the weight change of the sample, so that quantitative acidity information is obtained.
Further, as a more specific embodiment, the specific steps of the assay are as follows:
(1) starting a light source and a program control system, and recording the initial position of reflected light detected by a detector;
(2) putting a sample to be measured with a certain weight into the sample basket, wherein the spring is lengthened, the position of the reflector is changed, the position of reflected light detected by the detector is changed along with the change of the spring, and the program control system records the displacement change of the reflected light, corresponds to the change of the length of the spring and is then related to 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 position change information of the reflected light detected by a detector 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 correlation information of displacement change of reflected light and sample weight change under different temperatures and pressures so as to obtain quantitative acidity information of the sample to be detected under different measurement conditions;
(4) after the measurement of all temperature points is finished, the conversion relation between the length of the spring and the weight of the sample is obtained according to the displacement change of the reflected light, 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 to perform programmed heating and vacuum treatment after adsorption equilibrium, the sample mass after adsorbing probe molecules also changes continuously due to the continuous change of temperature, which causes the deformation of the spring and the change of the position of the reflector, and the program control system detects and records the displacement information of the reflected light through the detector; 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 corresponding temperature, and then recording displacement information of reflected light 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 measures the length change of the spring by using a laser reflection distance measuring mode, 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, becomes a conventional analytical instrument which can be directly placed on a test bed, provides help for the development of new catalytic materials, and has good application prospect and commercial value.
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 laser light source 3, a reflector 4, an array detector 5, a heating furnace 6, a sample basket 7, a sample to be measured 8, a thermocouple 9, a pyridine tube 10, a vacuum system 11, a program control system 12 and a temperature control system 13.
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 7 is connected below the spring 2, and the sample basket 7 is made of quartz glass; install a speculum 4 between spring 2 and the sample basket 7, be provided with laser light source 3 and array detector 5 outside surveying buret 1 that corresponds with speculum 4 position, when speculum 4 and array detector 5's position and length made speculum 4 reciprocate along with the spring, the light homoenergetic that laser light source 3 transmitted shines on speculum 4 and reflects array detector 5 and is caught, array detector 5 surface is greater than the facula diameter, laser light source 3, speculum 4 and array detector 5 are in a vertical plane, and the material of surveying buret 1 part that the light path that the three formed corresponds is the printing opacity material. The array detector 5 is externally connected with a program control system 12 and can record the movement information of reflected light on the array detector 5; the heating furnace 6 is arranged at the periphery of the sample basket 7, the heating furnace 6 is arranged outside the measuring tube 1, and the measuring tube 1 between the heating furnace 6 and the sample basket 7 is made of quartz glass; a thermocouple 9 is arranged beside the sample basket 7, the heating furnace 6 and the thermocouple 9 are both connected with a temperature control system 13 outside the measuring tube 1, and the temperature control system 13 is connected with a program control system 12; the measuring tube 1 is also connected with a pyridine tube 10 and a vacuum system 11, the vacuum system 11 is a mode of combining 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 laser light source 3 and the program control system 12, and recording the initial position of the reflected light detected by the array detector 5, wherein the initial position corresponds to the length of the initial spring 2;
(2) a sample 8 to be measured with a certain weight is put into the sample basket 7, the spring 2 is lengthened, the position of the reflector 4 is changed, the position of reflected light detected by the array detector 5 is changed therewith, and the program control system 12 records the displacement change of the reflected light, corresponds to the length change of the spring 2 and is then related to the weight change of the sample;
(3) the vacuum degree is adjusted through a vacuum system 11, the temperature is adjusted through a thermocouple 9, high-temperature and high-vacuum purification treatment is carried out on the sample, the temperature is reduced to room temperature after the purification is finished, and a program control system 12 automatically records the displacement change of reflected light; opening the pyridine tube 10 to enable the sample to adsorb the molecular probe, closing the pyridine tube 10 after adsorption balance, starting program heating and vacuum treatment, and obtaining correlation information of displacement change of reflected light and sample weight change under a certain temperature and pressure, so as to obtain 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 the measurement of all temperature points is finished, the conversion relation between the length of the spring 2 and the weight of the sample is obtained according to the displacement change of the reflected light, and the acid amount and the acid strength distribution of the sample at different temperatures can be obtained.
Example 3
This example discloses the procedure for determining the surface acidity of a particular catalyst material using the apparatus and method of examples 1 and 2:
(1) starting the laser light source 3 and the program control system 12, and recording the initial position of the reflected light detected by the array detector 5, wherein the initial position corresponds to the length of the initial spring 2;
(2) adding 0.2g of a hydrocracking catalyst sample 8 to be detected into a sample basket 7, starting a vacuum system 11 and a temperature control system 13, enabling a laser light source 3, a reflector 4, an array detector 5 and a spring 2 to start to work cooperatively, and measuring the position change of reflected light on the array detector 5 when the weight of the sample 8 to be detected changes in real time, wherein the position change corresponds to the change of the spring 2. After the sample 8 to be detected is subjected to high-temperature and high-vacuum purification treatment (4 hours), the pyridine pipe 10 is opened, pyridine is adsorbed to the sample 8 to be detected in a steam mode, the programmed temperature rise and high-vacuum purification treatment process is started after adsorption balance, desorption temperatures are respectively 160 ℃, 250 ℃, 350 ℃ and 450 ℃, desorption is carried out for 1 hour at constant temperature in each stage, pyridine molecules are continuously desorbed, and the weight change of the sample is measured in real time. The automatic measurement is completed in the whole measurement process, and the vacuum system 11 and the temperature control system 13 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 8 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, respectively, in which the acid strength is in mmol/g.
Table 1.
Table 2.
Claims (11)
1. A device for quantitatively detecting 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, a reflecting mirror is arranged between the spring and the sample basket, a light source and a detector are arranged outside the measuring tube corresponding to the position of the reflecting mirror, when the positions and the lengths of the reflecting mirror and the detector enable the reflecting mirror to move up and down along with the spring, light emitted by the light source can irradiate the reflecting mirror and be reflected to the detector to be captured, and the detector is externally connected with a program control system and can record reflected light movement information on the detector; 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 apparatus of claim 1, wherein the light source is a laser light source; the detector is an array detector.
3. The apparatus of claim 1, wherein the light source, the mirror, and the detector are in a vertical plane, and wherein the detector surface is larger than a diameter of a spot of light reflected by the mirror as it moves.
4. The apparatus of claim 1, wherein the light source, the reflector and the detector form a light path, and the corresponding measuring tube portion is made of a light-transmissive material.
5. The apparatus of claim 1, wherein the measurement tube between the heating device and the sample basket is of quartz glass material.
6. The apparatus of claim 1, wherein the heating device is a furnace; the temperature detection device is a thermocouple.
7. The device of claim 1, wherein the adsorption probe molecule tube is a pyridine tube.
8. 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。
9. The method for quantitatively detecting the acidity of the surface of the material by using the device of any one of claims 1 to 8 comprises the following steps:
starting a light source and a program control system, recording the initial position of reflected light detected by a detector, when a sample to be detected is placed in a sample basket, the vacuum degree is adjusted through a vacuum system, the temperature is adjusted through a heating device, an adsorption probe molecular tube is opened to enable the sample to adsorb a molecular probe under different conditions, a spring deforms due to the change of the weight of the sample, the position of a reflector changes, the position of the reflected light detected by the detector changes accordingly, the program control system records the displacement change information of the reflected light under different conditions, the length change of the spring under different conditions corresponds to the change of the weight of the sample, and then the displacement change information is related to the change of the weight of the sample, so that quantitative acidity information is obtained.
10. The method according to claim 8, wherein the specific steps of the assay are as follows:
(1) starting a light source and a program control system, and recording the initial position of reflected light detected by a detector;
(2) putting a sample to be measured with a certain weight into the sample basket, wherein the spring is lengthened, the position of the reflector is changed, the position of reflected light detected by the detector is changed along with the change of the spring, and the program control system records the displacement change of the reflected light, corresponds to the change of the length of the spring and is then related to 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 position change information of the reflected light detected by a detector 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 correlation information of displacement change of reflected light and sample weight change under different temperatures and pressures so as to obtain quantitative acidity information of the sample to be detected under different measurement conditions;
(4) after the measurement of all temperature points is finished, the conversion relation between the length of the spring and the weight of the sample is obtained according to the displacement change of the reflected light, and the acid amount and the acid strength distribution of the sample at different temperatures can be obtained.
11. The method according to claim 10, wherein in the step (3), during the process of starting the programmed heating and vacuum treatment after the adsorption equilibrium, the sample mass after the adsorption of the probe molecules is continuously changed due to the continuous change of the temperature, so that the spring is deformed, the position of the reflector is changed, and the program control system detects and records the displacement information of the reflected light through the detector; 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 corresponding temperature, and then recording displacement information of reflected light at the corresponding temperature points respectively.
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