CN116990346B - Method for measuring acidity coefficient of rock wool based on differential scanning calorimetry - Google Patents
Method for measuring acidity coefficient of rock wool based on differential scanning calorimetry Download PDFInfo
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- 239000011490 mineral wool Substances 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000000113 differential scanning calorimetry Methods 0.000 title claims abstract description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 303
- 239000000523 sample Substances 0.000 claims abstract description 158
- 238000001228 spectrum Methods 0.000 claims abstract description 27
- 239000000126 substance Substances 0.000 claims abstract description 24
- 238000012360 testing method Methods 0.000 claims abstract description 20
- 239000012496 blank sample Substances 0.000 claims abstract description 17
- 238000010586 diagram Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 30
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 25
- 235000012239 silicon dioxide Nutrition 0.000 claims description 19
- 239000000377 silicon dioxide Substances 0.000 claims description 15
- 238000012545 processing Methods 0.000 claims description 8
- 230000003595 spectral effect Effects 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 4
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 8
- 238000001757 thermogravimetry curve Methods 0.000 description 18
- 238000001514 detection method Methods 0.000 description 9
- 230000008569 process Effects 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 238000000265 homogenisation Methods 0.000 description 4
- 238000010561 standard procedure Methods 0.000 description 4
- 238000010998 test method Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 229920000742 Cotton Polymers 0.000 description 2
- 239000002841 Lewis acid Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 150000007517 lewis acids Chemical class 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000010309 melting process Methods 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000007848 Bronsted acid Substances 0.000 description 1
- 238000010669 acid-base reaction Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000007515 arrhenius acids Chemical class 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000011152 fibreglass Substances 0.000 description 1
- 239000012784 inorganic fiber Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000002411 thermogravimetry Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/20—Investigating or analyzing materials by the use of thermal means by investigating the development of heat, i.e. calorimetry, e.g. by measuring specific heat, by measuring thermal conductivity
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- 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)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
Abstract
The invention provides a method for measuring acidity coefficient of rock wool based on differential scanning calorimetry, which comprises the following steps: s1: preparing sodium hydroxide standard substance samples and sodium hydroxide blank samples with different proportions; s2: measuring integral heat flow values of a differential heat-thermal gravimetric chart and a sample differential heat-thermal gravimetric chart of a sodium hydroxide standard sample and a sodium hydroxide blank sample, and drawing a concentration-integral heat flow difference standard working curve; s3: preparing a sample to be detected and sodium hydroxide into the sample to be detected, measuring a differential thermal-thermogravimetric spectrum diagram of the sample to be detected, and calculating an integral thermal current value of the sample to be detected; s4: mixing a sample to be detected, sodium hydroxide and a standard substance, preparing an internal standard sample, measuring a differential heat-heat weight spectrogram of the internal standard sample, and calculating an integral heat flow value of the internal standard sample; s5: and calculating the acidity coefficient of the sample to be measured. Compared with the traditional capacity analysis method, the method has the advantages of higher accuracy, low cost, greatly reduced workload and greatly shortened test period.
Description
Technical Field
The invention belongs to the technical field of rock wool acidity coefficient measurement, and particularly relates to a method for measuring rock wool acidity coefficient based on a differential scanning calorimetry.
Background
Rock wool is used as a heat insulating material and is widely applied to various heat insulating occasions. The rock wool is an artificial inorganic fiber prepared from basalt, and has the excellent performances of light weight, small heat conductivity, incombustibility and the like. The rock wool is produced into rock wool products such as rock wool boards, rock wool felts, rock wool belts and the like through the technological processes of high-temperature melting, cotton spraying, cotton collecting, sizing, press forming, directional cutting and the like.
The acidity coefficient is an important index for measuring the chemical durability of rock wool, and is the ratio of the sum of the contents of silicon dioxide and aluminum oxide to the sum of the contents of calcium oxide and magnesium oxide in fiber components. The national standard requires that the acidity coefficient of rock wool used for the building outer wall is more than or equal to 1.8, and the basic physical and chemical stability requirements of the outer wall heat preservation system on the rock wool product can be met only when the acidity coefficient of the rock wool product is more than or equal to 1.8.
The existing rock wool acidity coefficient analysis and detection method adopts the measurement methods of silicon dioxide, aluminum oxide, calcium oxide and magnesium oxide which are respectively given in GB/T1549-2008 fiber glass chemical analysis method, and adopts the classical capacity analysis method. The capacity method is to measure the contents of four oxides in the sample to be measured and calculate the acidity coefficient. Although the method belongs to a classical method, the method has the defects of complicated sample pretreatment steps, large analysis and test workload, long test period and the like.
Disclosure of Invention
In view of the above, the invention aims to provide a method for measuring the acidity coefficient of rock wool based on a differential scanning calorimetry method, which aims to solve the problems of complex pretreatment steps, large analysis and test workload and long test period.
In order to achieve the above purpose, the technical scheme of the invention is realized as follows:
a method for measuring acidity coefficient of rock wool based on differential scanning calorimetry comprises the following steps:
s1: preparing sodium hydroxide standard substance samples and sodium hydroxide blank samples with different proportions;
s2: measuring integral heat flow values of a differential heat-thermal gravimetric chart and a sample differential heat-thermal gravimetric chart of a sodium hydroxide standard sample and a sodium hydroxide blank sample, and drawing a concentration-integral heat flow difference standard working curve;
s3: preparing a sample to be detected and sodium hydroxide into the sample to be detected, measuring a differential thermal-thermogravimetric spectrum diagram of the sample to be detected, and calculating an integral thermal current value of the sample to be detected;
s4: mixing a sample to be detected, sodium hydroxide and a standard substance, preparing an internal standard sample, measuring a differential heat-heat weight spectrogram of the internal standard sample, and calculating an integral heat flow value of the internal standard sample;
s5: calculating an integral heat flow difference of the sample to be measured and the internal standard sample, and calculating an acidity coefficient of the sample to be measured;
the standard of the sodium hydroxide standard sample is the same as that in step S3, and the standard is silica or alumina.
Further, in step S1, at least 5 sodium hydroxide standard samples of standards in different proportions are prepared, and the preparation of the sodium hydroxide standard samples includes: grinding and mixing the standard substance and sodium hydroxide uniformly;
further, the mixture was ground and mixed uniformly in a ratio of 10, 20, 30, 40, 50 parts by weight of standard per 100 parts by weight of sodium hydroxide.
Further, step S2 uses a differential scanning calorimeter to measure the integrated heat flow values of a differential thermal-thermogram and a differential thermal-thermogram of a sodium hydroxide standard sample, a sodium hydroxide blank sample,
the integrated heat flow difference refers to the difference between the integrated heat flow value of each concentration sample and the integrated heat flow value of the sodium hydroxide blank sample.
Further, in step S3, the sample to be measured and sodium hydroxide are prepared according to a mass ratio of 50:100, a differential thermal-thermogravimetric spectrum diagram of the sample to be measured is measured by adopting instrument parameters identical to a standard working curve, and an integral thermal value of the sample to be measured is calculated by using a data processing platform of the instrument.
Further, both of step S2 and step S3 use a differential scanning calorimeter, and the test conditions of the differential scanning calorimeter are set as follows: heating rate: 10 ℃ per minute, measuring temperature range: room temperature to 1000 ℃.
Further, the standard in step S4: and (3) testing a sample: the weight ratio of the sodium hydroxide is 10:50:100.
Further, the integral heat flow difference of the sample to be measured and the internal standard sample is calculated respectively, the difference between the integral heat flow value Qx of the sample to be measured and the integral heat flow value Q0 of the sodium hydroxide blank sample is expressed as delta Qx, the difference between the integral heat flow value Qnx of the internal standard sample and the integral heat flow value Q0 of the sodium hydroxide blank sample is expressed as delta Qnx, delta Qnx is substituted into a standard working curve obtained in the step S2 corresponding to the doped internal standard substance to obtain a concentration value Cnx corresponding to the delta Qnx, the obtained Cnx value is subtracted by 10, namely the concentration value of the doped internal standard substance is subtracted to obtain a standard regression concentration value of the sample to be measured, the standard regression heat flow difference of the sample to be measured is read at a point corresponding to Cnx 'on the standard working curve and is expressed as delta Qnx'; substituting the above values into the formula:
the acidity coefficient x of the sample to be measured can be obtained.
Furthermore, the standard substance is selected from spectral pure Al 2 O 3 Or spectrally pure SiO 2 The sodium hydroxide is pure NaOH.
Acid-base reactions are a type of chemical reactions that are prevalent in a variety of applications. According to the acid-base theory, the acid present in the aqueous solution is called "arrhenius acid", the acid under the non-aqueous system is called "bronsted acid", and the acid present along with the phase transition process is called "lewis acid". The results of repeated experiments show that the silicon dioxide and the aluminum oxide in the rock wool sample under the action of sodium hydroxide have the characteristic of typical Lewis acid, a remarkable exothermic effect is generated along with the process of being heated and melted together with the sodium hydroxide, and the exothermic effect and the proportion of silicon and aluminum oxide in the sample show a direct positive correlation, namely, the higher the proportion of silicon and aluminum oxide in the sample is, the larger the exothermic effect generated along with the melting process is. Based on the principle, the invention designs a corresponding method, and the acidity coefficient of the rock wool sample is obtained by measuring the calorific value of the rock wool sample in the process of heating and melting under the action of sodium hydroxide and combining with the comparison of the working curve of the standard substance.
Compared with the prior art, the method for measuring the acidity coefficient of the rock wool based on the differential scanning calorimetry has the following advantages:
the invention relates to a differential scanning calorimetry-based rock wool acidity coefficient determination method, which is to use an instrument analysis method to replace the traditional capacity analysis method for determining sample components. The acidity coefficient of the rock wool sample to be measured is obtained by measuring the exothermic effect generated by the rock wool sample and sodium hydroxide in the heating and melting process and comparing the exothermic effect with the working curve of the standard substance, and compared with the traditional capacity analysis method, the accuracy is higher, the cost is low, the workload is greatly reduced, and the test period is greatly shortened.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention. In the drawings:
FIG. 1 is a schematic representation of the differential thermal-thermogravimetric spectrum of silica and sodium hydroxide of the present invention with a portion of 10 added;
FIG. 2 is a schematic representation of the differential thermal-thermogravimetric spectrum of silica and sodium hydroxide of the present invention with a portion of 20 added;
FIG. 3 is a schematic representation of the differential thermal-thermogravimetric spectrum of silica and sodium hydroxide of the present invention with a portion of 30 added;
FIG. 4 is a schematic representation of the differential thermal-thermogravimetric spectrum of silica and sodium hydroxide with 40 parts added according to the present invention;
FIG. 5 is a schematic representation of the differential thermal-thermogravimetric spectrum of silica and sodium hydroxide with 50 parts added according to the present invention;
FIG. 6 is a schematic representation of the differential thermal-thermogravimetric spectrum of a sodium hydroxide blank sample of the present invention;
FIG. 7 is a graph showing the standard working curve of the concentration-integrated heat flow difference for a standard sample of spectrally pure silica;
FIG. 8 is a schematic representation of the differential thermal-thermogravimetric spectrum of aluminum oxide and sodium hydroxide of the present invention added in 10 parts;
FIG. 9 is a schematic representation of the differential thermal-thermogravimetric spectrum of aluminum oxide and sodium hydroxide of the present invention added in 20 parts;
FIG. 10 is a schematic representation of the differential thermal-thermogravimetric spectrum of aluminum oxide and sodium hydroxide of the present invention added in 30 parts;
FIG. 11 is a schematic representation of the differential thermal-thermogravimetric spectrum of aluminum oxide and sodium hydroxide of the present invention added in 40 parts;
FIG. 12 is a schematic representation of the differential thermal-thermogravimetric spectrum of aluminum oxide and sodium hydroxide of the present invention added in 50 parts;
FIG. 13 is a graph showing the standard working curve of the concentration-integrated heat flow difference of the present invention with a standard sample of spectrally pure aluminum oxide;
FIG. 14 is a schematic representation of a differential thermal-thermogravimetric spectrum of sample one and sodium hydroxide of the present invention;
FIG. 15 is a schematic representation of the differential thermal-thermogravimetric spectra of the spectrally pure silica, sample one and sodium hydroxide of the present invention;
FIG. 16 is a schematic representation of the differential thermal-thermogravimetric spectrum of sample two and sodium hydroxide of the present invention;
FIG. 17 is a schematic representation of the differential thermal-thermogravimetric spectrum of the spectrally pure aluminum oxide, sample two and sodium hydroxide of the present invention;
FIG. 18 is a graphic illustration of the differential thermal-thermogravimetric spectra of sample three and sodium hydroxide of the present invention;
FIG. 19 is a schematic representation of a spectroscopically pure aluminum oxide with sample three, sodium hydroxide differential thermal-thermogravimetry;
FIG. 20 is a schematic representation of a differential thermal-thermogravimetric spectrum of sample four and sodium hydroxide;
FIG. 21 is a schematic representation of the differential thermal-thermogravimetric spectrum of spectrally pure silica with sample four, sodium hydroxide.
Detailed Description
It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
The invention will be described in detail below with reference to the drawings in connection with embodiments.
1. The preparation method comprises the steps of respectively selecting spectral pure silicon dioxide and aluminum oxide, adding 10, 20, 30, 40 and 50 parts by weight of sodium hydroxide into each 100 parts by weight of sodium hydroxide, grinding and mixing uniformly. 5 samples were prepared for each standard.
2. Selecting a suitable differential scanning calorimeter, wherein the instrument parameters meet the following conditions:
thermal balance inductance: 1X 10 -6 G; temperature control precision: 0.01 ℃; working temperature range: room temperature to 1300 ℃. Setting test conditions: heating rate: 10 ℃ per minute, measuring temperature range: room temperature to 1000 ℃. Under this condition, the differential thermal thermogram of the two standard substances prepared in advance, 5 concentrations of each standard sample, and a total of 10 samples were measured one by one. And a differential thermal thermogram of a sodium hydroxide blank sample without the addition of a standard sample was measured. The integrated heat flow values giving a differential heat-heat thermogram for each sample were calculated with an instrument data processing platform.
The concentration-integrated heat flow difference standard operating curve was made for each sample for each of the two substances. The integrated heat flow difference refers to the difference between the integrated heat flow value (denoted as Q10, Q20, Q30, Q40, Q50, respectively) of each concentration sample and the integrated heat flow value (denoted as Q0) of the sodium hydroxide blank sample. According to the experimental results, the standard working curves of the two substances are approximate straight lines.
The sample to be measured and sodium hydroxide are prepared according to the sample to be measured: preparing a sample by using the mass ratio of sodium hydroxide=50:100, measuring a differential thermal-thermogravimetric spectrum diagram of the sample to be measured by using the instrument parameters which are the same as the standard working curve, and calculating an integral thermal current value (expressed as Qx) of the sample to be measured by using a data processing platform of the instrument.
One of two standard substances is selected, and is uniformly mixed with a sample to be tested and sodium hydroxide to prepare an internal standard sample, wherein the proportion of the internal standard sample is as follows: and (3) testing a sample: sodium hydroxide = 10:50:100, the differential thermal-thermogram of the internal standard sample was also measured using the same instrument parameters as the standard operating curve, and the integrated heat flow value (denoted Qnx) of the internal standard sample was calculated using the data processing platform of the instrument.
The integral heat flow difference of the sample to be detected and the internal standard added sample is calculated respectively, namely, the difference values of Qx, qnx and Q0 are calculated respectively and are respectively expressed as delta Qx and delta Qnx. Substituting Δ Qnx into the standard operating curve corresponding to the doped internal standard yields a concentration value Cnx corresponding to the Δqx value. Subtracting 10 from the Cnx value, namely subtracting the concentration value of the doped internal standard substance, to obtain a standard regression concentration value of the sample to be detected, which is represented as Cnx'. And reading the standard regression integral heat flow difference of the sample to be measured at a point corresponding to Cnx 'on the standard working curve, wherein the standard regression integral heat flow difference is shown as delta Qnx'. Substituting the above values into the formula:
the acidity coefficient x of the sample to be measured can be obtained.
Establishment of a standard working curve:
spectrally pure SiO 2 Establishing a standard working curve with NaOH;
the samples of different concentrations were prepared by selecting the spectral pure silica, preferably pure sodium hydroxide, according to the following mass ratios. Sodium hydroxide: silica is 100:10, 100:20, 100:30, 100:40, 100:50, respectively; the samples with the above proportion are ground and mixed uniformly, are put into a plastic sealing pocket and are put into a glass dryer.
The SDT Q600 differential scanning calorimeter is selected, and the instrument parameters can meet the following conditions:
thermal balance inductance: 1X 10 -6 G; temp. -controlling essenceDegree: 0.01 ℃; working temperature range: room temperature to 1300 ℃. The test conditions were set as follows: heating rate: 10 ℃ per minute, measuring temperature range: room temperature to 1000 ℃. Under this condition, the samples of 5 concentrations prepared in the previous step were measured one by one to obtain five differential thermal-thermograms of the samples, respectively shown in fig. 1 to 5, and under the same conditions, differential thermal-thermograms of the sodium hydroxide of superior purity were measured, as shown in fig. 6. Based on the measured results, the integrated heat flow differences corresponding to the samples with different concentrations are shown in table 1.
TABLE 1 test results with spectrally pure silica as standard
And (3) plotting by taking the integral heat flow difference corresponding to each concentration value as an abscissa and the addition part of the standard sample as an ordinate, so as to obtain a concentration-integral heat flow difference standard working curve of the spectrum pure silicon dioxide serving as a standard sample, as shown in fig. 7.
Spectrally pure Al 2 O 3 Establishing a standard working curve with NaOH;
spectrally pure Al is selected 2 O 3 Samples of different concentrations were prepared from the pure NaOH in the following mass ratios.
NaOH：Al 2 O 3 100:10, 100:20, 100:30, 100:40, 100:50, respectively; the samples with the above proportion are ground and mixed uniformly, are put into a plastic sealing pocket and are put into a glass dryer.
The SDT Q600 differential scanning calorimeter is selected, and the instrument parameters can meet the following conditions: thermal balance inductance: 1X 10 -6 G; temperature control precision: 0.01 ℃; working temperature range: room temperature to 1300 ℃; the test conditions were set as follows: heating rate: 10 ℃ per minute, measuring temperature range: room temperature to 1000 ℃. The previously formulated 5 concentration samples were measured one by one under this condition to give five samples of differential thermal-thermograms, listed in figures 8-12, respectively.
Under the same conditions, the differential heat-thermal gravimetric spectrum of the sodium hydroxide with high purity is measured, as shown in fig. 6, and the integral heat flow differences corresponding to samples with different concentrations are listed according to the actual measurement results, as shown in table 2.
TABLE 2 test results of spectrally pure aluminum oxide as standard
And (3) plotting by taking the integral heat flow difference corresponding to each concentration value as an abscissa and the addition part of the standard sample as an ordinate to obtain a concentration-integral heat flow difference standard working curve of the spectrum pure aluminum oxide serving as a standard sample, as shown in fig. 13.
Example 1:
and (3) finishing pretreatment such as degumming, homogenization, shrinkage and the like of a rock wool sample I according to standard requirements, and performing sample I according to mass ratio: sodium hydroxide=50:100 sample one and high-grade pure sodium hydroxide were mixed uniformly and the differential thermal-thermogram was determined and the results are shown in fig. 14.
FIG. 14 is data processed to give an integrated thermal tolerance of 10430J/g, denoted Qx1.
Sample one was prepared as an internal standard added sample. The same batch of samples as the first sample is subjected to the same and processing process, and the silicon dioxide is spectrally pure according to the mass ratio: sample one: sodium hydroxide=10:50:100 the internal standard (spectrally pure silica), sample one and high-grade pure sodium hydroxide were weighed and mixed well, and the differential thermal-thermogram was determined and the results are shown in fig. 15.
The data in FIG. 15 is processed to give an integrated thermal tolerance of 9573J/g, designated Qnx.
Difference values are respectively obtained between Qx1 and Qnx1 and Q0, and accordingly ΔQx1=6341J/g and Δ Qnx 1=7198J/g are obtained; substituting the standard working curve of concentration-integrated heat flow difference for the standard sample with spectrally pure silica (fig. 7) gives the corresponding standard concentration Cnx of 46.64, subtracting the internal standard concentration value 10, and obtaining Cnx ' = 36.64, and thus reading Cnx ' the integrated heat flow difference Δ Qnx1' =10602J/g on the standard working curve of concentration-integrated heat flow difference for the standard sample with spectrally pure silica. Substituting the values into the following formula to obtain the acidity coefficient x1 of the sample I.
The detection result is compared with a standard method, and GB/T5480-2017 mineral wool and product test method thereof are adopted to detect the acidity coefficient of the sample I, wherein the detection result is 2.52 and is within the allowable error range.
Example 2
And (3) finishing pretreatment such as degumming, homogenization, shrinkage and the like of a rock wool sample II according to standard requirements, and performing pretreatment such as sample II according to mass ratio: sodium hydroxide=50:100 sample one and high-grade pure sodium hydroxide were mixed uniformly, and the differential heat-thermogram was measured, and the result is shown in fig. 16.
FIG. 16 is data processed to give an integrated thermal tolerance of 10044J/g, designated Qx2.
Sample two was prepared as an internal standard added sample. The same batch of samples are the same as the second sample, and the same and treatment process is carried out on the same batch of samples, wherein the samples are spectrally pure aluminum oxide according to the mass ratio: sample two: sodium hydroxide=10:50:100 the internal standard (spectrally pure aluminum oxide), sample two and high-grade pure sodium hydroxide were weighed and mixed well, and the differential thermal thermogram was determined and the results are shown in fig. 17.
The data in FIG. 17 were processed to give an integrated thermal tolerance of 8854J/g, designated Qxn.
Difference values were obtained between Qx2 and Qxn2 and Q0, respectively, to obtain Δqx2=6341J/g and Δ Qnx 2=7971J/g. Substituting Δ Qnx2 into the concentration-integrated heat flow difference standard working curve (fig. 13) with the spectral pure aluminum oxide as the standard sample, obtaining the corresponding standard concentration of Cnx2 'as 45.75, subtracting the internal standard concentration value of 10, obtaining Cnx' =35.75, and reading the integrated heat flow difference Δ Qnx2 '=6445J/g on the concentration-integrated heat flow difference standard working curve with the spectral pure aluminum oxide corresponding to Cnx' as the standard sample. Substituting the values into the following formula to obtain the acidity coefficient x2 of the sample II.
Comparing the detection result with a standard method, and detecting the acidity coefficient of the sample II by using GB/T5480-2017 mineral wool and a product test method thereof, wherein the detection result is 2.36 and is within an allowable error range.
Example 3
And (3) finishing pretreatment such as degumming, homogenization, shrinkage and the like of a rock wool sample III according to standard requirements, and performing pretreatment according to the mass ratio of the sample III: sodium hydroxide=50:100 sample one and high-grade pure sodium hydroxide were mixed uniformly, and the differential thermal-thermogram was measured, and the result is shown in fig. 18.
The integrated heat flow difference is 10158J/g, denoted as Qx3, obtained by data processing in FIG. 18.
Sample three was prepared as an internal standard added sample. The same batch of samples are the same as the sample III, and the spectrally pure aluminum oxide is prepared according to the mass ratio through the same pretreatment process: sample three: sodium hydroxide=10:50:100 the internal standard (spectrally pure aluminum oxide), sample three and high-grade pure sodium hydroxide were weighed and mixed uniformly, and the differential thermal-thermogram was determined and the results are shown in fig. 19.
The data in FIG. 19 were processed to give an integrated heat flow difference of 8944J/g, designated Qnx.
Difference values are obtained between Qx3 and Qnx3 and Q0, respectively, to obtain Δqx3=6613J/g and Δ Qnx3' =7827J/g. Substituting Δqx3 into the concentration-integrated heat flow difference standard working curve (fig. 13) with the spectral pure aluminum oxide as the standard sample, obtaining the corresponding standard concentration Cnx of 44.79 and subtracting the internal standard concentration value 10 to obtain Cnx '= 34.79, and reading the integrated heat flow difference Δ Qnx3' =6296J/g on the concentration-integrated heat flow difference standard working curve with the spectral pure aluminum oxide corresponding to Cnx3 as the standard sample. Substituting the values into the following formula to obtain the acidity coefficient x3 of the sample three.
Comparing the detection result with a standard method, and detecting the acidity coefficient of a sample III by using GB/T5480-2017 mineral wool and a product test method thereof, wherein the detection result is 2.24 and is within an allowable error range.
Example 4
And (3) finishing pretreatment such as degumming, homogenization, shrinkage and the like of a rock wool sample IV according to standard requirements, and performing pretreatment such as sample IV according to mass ratio: sodium hydroxide=50:100 samples four and high grade pure sodium hydroxide were mixed well and the differential thermal-thermogram was determined and the results are shown in fig. 20.
FIG. 20 is data processed to give an integrated thermal tolerance of 10858J/g, denoted Qx4.
Sample four was prepared as an internal standard added sample. The same batch of samples is the same as the sample IV, and the same and processing process is carried out on the same samples, namely the spectrally pure silicon dioxide according to the mass ratio: sample four: sodium hydroxide=10:50:100 the internal standard (spectrally pure silica), sample four and high-grade pure sodium hydroxide were weighed and mixed well, and the differential thermal-thermogram was determined and the results are shown in fig. 21.
The data in FIG. 21 were processed to give an integrated thermal tolerance of 9829J/g, designated Qnx.
Difference between Qx4 and Qnx4 and Q0 is obtained, and Δ Qnx4 =5913J/g, and Δ Qnx4 =6942J/g is obtained. Substituting Δ Qnx4 into the concentration-integrated heat flow difference standard operating curve (fig. 7) with spectrally pure silica as standard sample, obtaining the corresponding standard concentration Cnx of 43.94, subtracting the internal standard concentration value of 10, obtaining Cnx ' =33.94, and reading Cnx ' the integrated heat flow difference Δ Qnx4' =5887J/g on the concentration-integrated heat flow difference standard operating curve with spectrally pure silica as standard sample. Substituting the values into the following formula to obtain the acidity coefficient x4 of the sample four.
Comparing the detection result with a standard method, and detecting the acidity coefficient of a sample four by using GB/T5480-2017 mineral wool and a product test method thereof, wherein the detection result is 1.96 and is within an allowable error range.
The use time of the prior art is as follows: all specified test items were completed with a minimum time consumption of 36 hours. In this embodiment, the test of two differential thermal-thermograms of one sample to be tested is completed, and the time required for the test is 3.5 hours, so that the test time is greatly shortened.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (7)
1. A method for measuring acidity coefficient of rock wool based on differential scanning calorimetry is characterized in that: the method comprises the following steps:
s1: preparing sodium hydroxide standard substance samples and sodium hydroxide blank samples with different proportions;
s2: measuring integral heat flow values of a differential heat-thermal gravimetric chart and a sample differential heat-thermal gravimetric chart of a sodium hydroxide standard sample and a sodium hydroxide blank sample, and drawing a concentration-integral heat flow difference standard working curve;
s3: preparing a sample to be detected and sodium hydroxide into the sample to be detected, measuring a differential thermal-thermogravimetric spectrum diagram of the sample to be detected, and calculating an integral thermal current value of the sample to be detected;
s4: mixing a sample to be detected, sodium hydroxide and a standard substance, preparing an internal standard sample, measuring a differential heat-heat weight spectrogram of the internal standard sample, and calculating an integral heat flow value of the internal standard sample;
s5: calculating an integral heat flow difference of the sample to be measured and the internal standard sample, and calculating an acidity coefficient of the sample to be measured;
the standard of the sodium hydroxide standard sample is the same as the standard in the step S3, and the standard is silicon dioxide or aluminum oxide;
in the step S3, preparing a sample to be tested and sodium hydroxide according to the mass ratio of 50:100;
standard in step S4: and (3) testing a sample: the weight ratio of the sodium hydroxide is 10:50:100;
calculating the integral heat flow difference of the sample to be detected and the internal standard sample, wherein the difference value between the integral heat flow value Qx of the sample to be detected and the integral heat flow value Q0 of the sodium hydroxide blank sample is represented as delta Qx, the difference value between the integral heat flow value Qnx of the internal standard sample and the integral heat flow value Q0 of the sodium hydroxide blank sample is represented as delta Qnx, delta Qnx is substituted into a standard working curve obtained in the step S2 corresponding to the doped internal standard substance to obtain a concentration value Cnx corresponding to the delta Qnx, the obtained Cnx value is subtracted by 10, namely the concentration value of the doped internal standard substance is subtracted to obtain a standard regression concentration value of the sample to be detected, the point corresponding to Cnx 'is obtained on the standard working curve, and the standard regression integral heat flow difference of the sample to be detected is read and is represented as delta Qnx'; substituting the above values into the formula:
the acidity coefficient x of the sample to be measured can be obtained.
2. The method for determining the acidity coefficient of rock wool based on differential scanning calorimetry according to claim 1, wherein: step S1, preparing sodium hydroxide standard samples of at least 5 standards in different proportions, wherein the preparation of the sodium hydroxide standard samples comprises the following steps: the standard substance is ground and mixed with sodium hydroxide uniformly.
3. The method for determining the acidity coefficient of rock wool based on differential scanning calorimetry according to claim 2, wherein: the mixture is ground and mixed uniformly according to the proportion of adding 10, 20, 30, 40 and 50 parts by weight of standard substances into every 100 parts by weight of sodium hydroxide.
4. The method for determining the acidity coefficient of rock wool based on differential scanning calorimetry according to claim 1, wherein: step S2, measuring the integrated heat flow values of a differential heat-heat spectrogram and a differential heat-heat spectrogram of a sodium hydroxide standard sample and a sodium hydroxide blank sample by using a differential scanning calorimeter;
the integrated heat flow difference refers to the difference between the integrated heat flow value of each concentration sample and the integrated heat flow value of the sodium hydroxide blank sample.
5. The method for determining the acidity coefficient of rock wool based on differential scanning calorimetry according to claim 1, wherein: and measuring a differential thermal-thermogravimetric spectrum diagram of the sample to be measured by adopting instrument parameters which are the same as the standard working curve, and calculating by using a data processing platform of the instrument to obtain an integral thermal current value of the sample to be measured.
6. The method for determining the acidity coefficient of rock wool based on differential scanning calorimetry according to claim 1, wherein: step S2 and step S3 each use a differential scanning calorimeter, and the test conditions of the differential scanning calorimeter are set as follows: heating rate: 10 ℃ per minute, measuring temperature range: room temperature to 1000 ℃.
7. The method for determining the acidity coefficient of rock wool based on differential scanning calorimetry according to claim 1, wherein: the standard substance is selected from spectral pure Al 2 O 3 Or spectrally pure SiO 2 The sodium hydroxide is pure NaOH.
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