CN114199712A - Method for measuring oil absorption value of silicon dioxide - Google Patents

Method for measuring oil absorption value of silicon dioxide Download PDF

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CN114199712A
CN114199712A CN202111425875.2A CN202111425875A CN114199712A CN 114199712 A CN114199712 A CN 114199712A CN 202111425875 A CN202111425875 A CN 202111425875A CN 114199712 A CN114199712 A CN 114199712A
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oil
absorption value
oil absorption
silicon dioxide
measuring
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邹坚涛
张云龙
郑松玲
王宪伟
杨标源
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Jinsanjiang Zhaoqing Silicon Material Co ltd
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Jinsanjiang Zhaoqing Silicon Material Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N5/00Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
    • G01N5/02Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by absorbing or adsorbing components of a material and determining change of weight of the adsorbent, e.g. determining moisture content

Abstract

The invention belongs to the technical field of oil absorption value detection, and particularly relates to a method for measuring the oil absorption value of silicon dioxide, which comprises the following steps: 1) measuring the apparent density and pore volume of a typical silica sample; 2) measuring the oil absorption value of a typical silicon dioxide sample by a manual method; 3) fitting k and phi values according to the apparent density, pore volume and oil absorption value formulas of typical silica samples to obtain a calculation formula of the oil absorption value of the silica; 4) and measuring the apparent density and pore volume of the silicon dioxide sample to be measured, and calculating the oil absorption value of the silicon dioxide sample to be measured according to the calculation formula of the oil absorption value of the silicon dioxide. The measuring method can be convenient for manufacturers, customers and the like to unify the measuring method, is convenient for controlling and judging the product quality, can calculate the oil absorption value only by additionally testing the apparent density and the BET single-point adsorption total pore volume, and has the advantages of simple operation, small error, stable result and great labor cost saving in the measuring process.

Description

Method for measuring oil absorption value of silicon dioxide
Technical Field
The invention belongs to the technical field of oil absorption value detection, and particularly relates to a method for measuring an oil absorption value of silicon dioxide powder.
Background
The silicon dioxide has stable physical and chemical properties, good thixotropy and wear resistance, good compatibility with toothpaste raw materials and optimal compatibility, can effectively solve the problem of toothpaste slag falling during tooth brushing due to the good thixotropy, and reduces the degree of wear to teeth due to the matching of the coefficient of the wear resistance of the silicon dioxide and the teeth, so that the silicon dioxide can be widely applied to toothpaste formulas as an abrasive and a thickening agent. With the cross permeation and fusion development of the nanotechnology in the white carbon black industry, special functional and special nano silicon dioxide is developed rapidly. According to different physical and chemical characteristics of the silicon dioxide, the silicon dioxide can be used as a reinforcing filler of light-colored rubber, an opening agent of plastic, a flatting agent for paint, a resin compounding agent, a chemical absorbent, a building filler, a coating agent for special paper and the like, and is applied to various fields of the chemical industry. In addition, silica is used as a reinforcing agent, a filler and a modifier in various fields such as an ink field, etc. because of its stable physicochemical properties, acid and alkali resistance, high temperature resistance and no environmental pollution.
When silica is used as a rubber filler, the degree of aggregation affects the performance properties of the vulcanizate. To characterize the degree of silica aggregation and agglomeration, an oil absorption value is often used. Under the specified experimental conditions, the amount of oil absorbed by 100g of silica is its oil absorption value. The oil absorption value is an important index for representing the aggregation degree, structure and other characteristics of the silicon dioxide and is often used as a decisive index for judging whether the product is good or bad and whether the product is qualified or not. As the nano silicon dioxide applied to powder, the size of the oil absorption value is a key index for determining the wetting and dispersion of the nano silicon dioxide and a matrix material, the oil absorption value is also referred to as the performance index of the silicon dioxide for toothpaste, and customers can specify the oil absorption value range of the silicon dioxide aiming at the toothpaste formula so as to control the stability of the formula.
In the prior art, there are two methods for measuring the oil absorption value: manual and instrumental methods. Manual methods require manual operations, and result deviation is often large due to differences between people and between laboratories. When measured with an instrument, the results obtained with the same silica may also vary widely due to differences in the performance of the instrument. In combination with practice, the machine measurements are not as stable as manual methods. The result errors of manual and instrumental measurement are large, which brings troubles to the control of the performance and the judgment of the quality of the silicon dioxide product and even generates disputes.
Disclosure of Invention
The invention aims to provide the oil absorption value measuring method which is small in system error, high in stability and convenient to operate.
In order to achieve the purpose, the invention adopts the following technical scheme:
the first purpose of the invention is to provide a method for measuring the oil absorption value of silicon dioxide, which comprises the following steps:
1) measurement of apparent Density ρ of a typical silica sampleApparent appearanceAnd pore volume VPore volume
2) Measuring the oil absorption value of a typical silicon dioxide sample by a manual method;
3) apparent density according to typical silica sample ρApparent appearancePore volume VPore volumeAnd oil absorption value formula
Fitting k and phi values to obtain a calculation formula of the silica oil absorption value:
Figure BDA0003378404460000021
wherein the content of the first and second substances,
VpowderIs the skeletal volume of the silica powder;
ρoilAs the density of the oil used;
moilThe quality of the oil used;
ρpowderIs the skeleton density of the silicon dioxide powder;
ρapparent appearanceIs the apparent density;
Vpore volumeIs the volume of a single-point adsorption total pore measured by a static nitrogen adsorption instrument;
the size of k is only related to the type and temperature of oil, and k varies within a certain range and can be appointed within the range;
the size of phi is only related to the type and temperature of oil, and phi varies within a certain range and can be appointed within the range;
4) measuring apparent density rho of silicon dioxide sample to be measuredApparent appearancePore volume VPore volumeAnd calculating the oil absorption value of the silicon dioxide sample to be detected according to the calculation formula of the oil absorption value of the silicon dioxide.
Preferably, the number of the typical silica samples is ≧ 6.
Preferably, said step 1) measures the apparent density ρ of the silicaApparent appearanceThe method comprises the following specific steps:
weighing 3g of sample, accurately measuring to 0.01g, placing in a centrifuge tube, placing in an electric centrifuge, starting at 2000r/min for 20min, taking out, placing in a square sample presser, flattening, and accurately measuring to 0.1mL according to the volume.
Preferably, said step 2) measures the pore volume V of the silicaPore volumeComprising measuring the pore volume V of the silica with a static nitrogen adsorber of the model JW-BK12Pore volumeAnd calculating by adopting a BJH pore size distribution test method.
Preferably, in the step 3), the oil absorption value of a typical silica sample is measured by a manual method, the oil is castor oil, and the specific steps include:
taking 1-2g of silicon dioxide sample, suggesting that 2g of friction type silicon dioxide is needed, 1g of thickening type silicon dioxide is needed, and the oil absorption value experiment requires that the consumed oil is more than 1 g. Placing a silicon dioxide sample on a glass plate, weighing castor oil and a dropper to 0.01g, sucking the castor oil by the dropper, adding the castor oil into a sample drop by drop, thoroughly kneading the silicon dioxide sample by a tongue depressor after adding each drop, finishing the test when the silicon dioxide sample is kneaded into a very viscous dough which is not fragile and not easy to separate, and weighing the weight of the consumed castor oil by using a differential method.
Preferably, the method for judging whether the k and the phi values fitted according to the oil absorption value formula in the step 3) are proper comprises the following specific steps: and calculating the percentage error between the formula calculation value and the manually measured oil absorption value according to the fitted k and phi, and judging that the values of the k and the phi are reasonable when the percentage error is less than 5 percent.
Therefore, the values of k and phi are agreed between manufacturers and clients according to the result solved in the step 3), and the agreed k and phi are obtained; more, in the same industry, the same k and phi can be agreed under certain experimental conditions, so that the uniqueness of a calculation formula is ensured; in particular, when castor oil is used, k is typically in the range of 0.50 to 0.60 and phi is in the range of 0.46 to 0.55.
Preferably, the oil used is required not to wet the silica during the measurement, otherwise the formula does not apply.
Preferably, the oil used is one of linseed oil, castor oil, dioctyl adipate and dibutyl phthalate.
The invention also provides an application of the measuring method in the detection of the oil absorption value of the powder.
Compared with the prior art, the invention has the following beneficial effects:
(1) the method creatively deduces the formula of the oil absorption value of the powder such as the silicon dioxide, so that the measurement process of the oil absorption value of the powder such as the silicon dioxide is simple, the oil absorption value can be calculated only by measuring the BET nitrogen adsorption data and the apparent density of the silicon dioxide, the repeated work of manually measuring the oil absorption value by operators is avoided, and the huge labor cost is saved.
(2) The measuring method of the invention is convenient for manufacturers, clients and other parties to unify the measuring method, and is convenient for controlling and judging the product quality.
(3) The measuring method of the invention has the advantages of convenient operation, small error and stable result. In the measuring process, errors mainly come from systematic errors and random errors of apparent density measurement and pore volume measurement, and excessive human factor errors are avoided.
Drawings
FIG. 1 is a schematic diagram of an idealized model of an oil slug;
FIG. 2 is ρOil blockAnd rhoApparent appearanceA linear fit graph between;
FIG. 3 is a graph of a linear fit of the k and φ values of example 2;
FIG. 4 is a graph of a linear fit of the k and φ values of example 3.
Detailed Description
The present invention will be described in further detail with reference to the following examples. It should not be understood that the scope of the above-described subject matter of the present invention is limited to the following examples.
Example 1 derivation of oil absorption formula
The silica powder was purchased from silicon materials of jinsanjiang (zhaoqing) gmbh and includes silica samples of thickening type silica (type a, type B), synthetic type (type C), and friction type silica (type D, type E, type F).
When the oil absorption value is measured by a manual method, the material obtained at the end point is an oil block. An ideal model of the oil cake was constructed, a schematic of the model being shown in fig. 1. Because the oil and powder particles in the oil block are uniformly distributed; therefore, during manual measurement of the oil absorption value, the powder volume is compressed during the spatula process. Thus, volume ρ of oil cakeOil blockSatisfies the following conditions:
ρoil block=kρPerformance ofOilFormula (1)
Wherein in the formula (1), ρOil blockIs the oil bulk density, ρApparent appearanceIs apparent density, ρOilTaking 0.95g/mL of castor oil as the density of the oil; the magnitude of k depends only on the type of oil and the temperature, and varies within a certain range. Measurement of oil bulk Density ρOil blockAnd apparent density ρApparent appearanceDensity of oil cake ρOil blockAnd apparent density ρApparent appearanceThe measurement results of (a) are shown in table 1.
The measured oil bulk density ρOil blockThe method specifically comprises the following steps: 1) weighing the mass of the oil cake by using an analytical balance; 2) wrapping the sealing oil block with a film (with negligible volume); 3) measuring the volume of the oil block by using a drainage method;
4) calculating the density of the oil block;
the measured apparent density ρApparent appearanceThe method comprises the following specific steps: weighing 3g of sample, accurately weighing to 0.01g, placing in a centrifuge tube, and placing in an electric centrifugeIn the heart machine, the rotation speed is 2000r/min, the heart machine is started for 20min, and the heart machine is taken out and put into a square sample presser to be flattened to be accurate to 0.1mL according to the volume.
TABLE 1 oil bulk Density and apparent Density data sheet
Model number Apparent density/(g/mL) Oil block density/(mL/g)
A 0.16 1.0396
B 0.19 1.0570
C 0.23 1.0782
D 0.38 1.1591
E 0.41 1.1764
F 0.60 1.2822
The results of linear fitting using Excel are shown in FIG. 2, yielding R20.9999, an intercept of 0.95, and precisely a density value of 0.95g/mL for castor oil, illustrate the rationality of the formula (1) according to the invention.
Because, in the process of testing by a static nitrogen adsorption instrument, oil hardly enters into the nano holes of the hydrophilic powder; in the oil cake, only a part of the volume between the powder particles is occupied by oil, and therefore, the formula can be derived:
Vair (a)=VPore volume+φVParticle voidsFormula (2)
In the formula (2), the phi is only related to the type and temperature of oil and varies within a certain range; total pore volume V of single-point adsorption of the powderPore volumeThe method is characterized in that a JW-BK112 static nitrogen adsorption instrument is adopted for determination, and a BJH method is adopted for calculation; the JW-BK112 static nitrogen adsorption instrument is purchased from Beijing Jingwei Gaokao technical Co.
In the oil cake material, the following formula (3) is satisfied, and in the formula (3), VOilVolume of oil, VPowderIs the skeletal volume (true volume), V, of the silicon dioxide powderAir (a)Is the volume of air in the oil cake.
VOil+VPowder+VAir (a)=VOil blockFormula (3)
At ambient conditions, the mass of air is about 1.2mg/mL, and therefore, the density of the oil cake can be deduced as:
Figure BDA0003378404460000071
further, the deformation may result in:
Figure BDA0003378404460000072
in the formula (5), ρPowderThe skeletal density (true density) of a powder can be obtained from the physical properties of the powder, and is well knownThe density of the silica powder was taken to be 2.2 g/mL.
From equation (2), V can be derivedParticle voidsThe calculation of (a) is disclosed as:
Figure BDA0003378404460000073
wherein in the formula (6), ρGranulesRefers to the average apparent density of individual particles in the powder, and is calculated by the formula:
Figure BDA0003378404460000074
the following formula (1), (2), (5), (6) and (7) can be combined:
Figure BDA0003378404460000081
and because of VOil=mOilOilNamely:
Figure BDA0003378404460000082
when castor oil was used, ρ is obtained by using 100g of silica powder and 2.2g/mL of known silica powderOilTaking 0.95g/mL to obtain:
Figure BDA0003378404460000083
in the formula (10), mOilThe unit of (2) is g/100g, the density unit is g/mL, VPore volumeTake mL/g.
Therefore, the formula of the oil absorption value of the powder such as silicon dioxide is creatively deduced, the measurement process of the oil absorption value of the powder such as silicon dioxide is simple, the oil absorption value can be calculated only by measuring the BET nitrogen adsorption data and the apparent density of the silicon dioxide, the repeated work of manually measuring the oil absorption value by operators is avoided, and the huge labor cost is saved.
Example 2 measurement method of silica oil absorption value
The silicon dioxide powder has a total pore volume V of single-point adsorptionPore volumeThe method is characterized in that a JW-BK112 static nitrogen adsorption instrument is adopted for determination, and a BJH method is adopted for calculation;
the apparent density ρ of the measurement silicaApparent appearanceThe method comprises the following specific steps: weighing 3g of sample, accurately measuring the sample to 0.01g, placing the sample in a centrifugal tube, placing the centrifugal tube in an electric centrifuge, starting the centrifuge for 20min at the rotating speed of 2000r/min, taking out the sample, placing the sample in a square sample presser for flattening, and accurately measuring the sample to 0.1mL according to the volume of the sample;
the JW-BK112 static nitrogen adsorption instrument is purchased from Beijing Jingwei Gaokao Bokojic technology Co., Ltd; the silica sample powder was purchased from jin san jiang silicon materials ltd, including thickening silica (type a, type B), synthetic silica (type C), friction silica (type D, type E, type F).
1) Measurement of apparent Density ρ of silica for a typical silica sampleApparent appearanceAnd pore volume VPore volumeThe results of the data are shown in table 2;
2) measuring the oil absorption values of 6 typical silica samples by a manual method;
the oil absorption value test results are shown in the following table 2 and are obtained by manual test, and the test method is as follows: taking 1-2g of silicon dioxide sample, 2g of friction type silicon dioxide, 1g of thickening type silicon dioxide and more than 1g of oil consumption required by oil absorption value experiment. Placing a silicon dioxide sample on a glass plate, weighing castor oil and a dropper to 0.01g, sucking the castor oil by the dropper, adding the castor oil into a sample drop by drop, thoroughly kneading the silicon dioxide sample by a tongue depressor after adding each drop, finishing the test when the silicon dioxide sample is kneaded into a very viscous dough which is not fragile and not easy to separate, and weighing the weight of the consumed castor oil by using a differential method.
TABLE 26 typical Property parameters of various types of silica samples
Figure BDA0003378404460000091
3) Fitting k and phi values according to the apparent density, pore volume and oil absorption value formulas of typical silica samples to obtain a calculation formula of the oil absorption value of the silica, and specifically comprising the following steps:
the parameters k, φ in the oil absorption value expression were fitted using the data in Table 2 and the formula (10) derived in example 1:
substituting the data in Table 2 into equation (10) derived in example 1, 6 equations were obtained for k and φ,
Figure BDA0003378404460000101
Figure BDA0003378404460000102
the 6 equations are used to draw the function image, as shown in fig. 3, other programming software can also be used to perform linear fitting, from the perspective of solving the equations, the best k and phi are fitted, that is, a "point (k, phi)" is found, and almost all curves can pass through, that is, the "thinnest" place of the curve bundle in the figure, and this place satisfies that k is greater than 0.50 and less than 0.55, and phi is greater than 0.50 and less than 0.55.
And setting the percentage error of fitting as Yn, wherein the calculation method of Yn comprises the following steps:
Figure BDA0003378404460000103
taking a series of points (0.51 ), (0.51, 0.52), (0.51, 0.53), (0.51, 0.54); (0.52, 0.51), (0.52 ), (0.52, 0.53),. the. (0.52, 0.54.) the calculation of Yn is performed, and the value of (k, φ) is acceptable when the calculated Yn is less than 5% for all types of powders.
When k is 0.5492 and phi is 0.52, Yn is less than 5%, and the calculation formula of the oil absorption value of the silicon dioxide is obtained:
Figure BDA0003378404460000104
the percentage error of the oil absorption value calculated by the formula and the manual test is shown in table 3.
TABLE 3 comparative data for oil absorption value calculated by silica sample formula and measured by hand
Figure BDA0003378404460000105
Figure BDA0003378404460000111
The results in Table 3 show that the relative errors are less than 5%, which indicates the reasonableness of the fitting k and phi in the formula and the reasonableness of the formula derivation process.
4) And (3) measuring the apparent density and the pore volume of the silicon dioxide sample to be tested, calculating the oil absorption value of the silicon dioxide sample to be tested according to a calculation formula (12) for calculating the oil absorption value of the silicon dioxide, and simultaneously, measuring the oil absorption value of the silicon dioxide sample to be tested by a manual method for verification, wherein the test results are shown in table 4. The a, b, c, e and f are all products of Jinsanjiang silicon materials GmbH.
TABLE 4 comparison data of oil absorption value calculated by formula and hand oil absorption value of silicon dioxide sample to be measured
Figure BDA0003378404460000112
The results in Table 4 show that the relative errors are less than 5%, and the reasonability of the agreed values of k and phi is further verified. In addition, according to the industry recommendations, when castor oil is used, k ranges from 0.50 to 0.60 and phi ranges from 0.46 to 0.55, and fitting is generally agreed to be performed within the range, and the applicability and practicability of the formula of the invention are illustrated within the range in the embodiment. Therefore, in the actual operation process, the method for measuring the oil absorption value of the silicon dioxide provided by the invention is more convenient for manufacturers, customers and other parties to unify the measuring method, and is convenient for controlling and judging the product quality; in addition, the measuring method is convenient to operate, small in error and stable in result; in the measuring process, errors mainly come from systematic errors and random errors of apparent density measurement and pore volume measurement, and excessive human factor errors are avoided.
Example 3 measurement method of oil absorption value of silica
The silicon dioxide powder has a total pore volume V of single-point adsorptionPore volumeThe method is characterized by adopting a JW-BK112 static nitrogen adsorption instrument for measurement and adopting a BJH method for calculation. The JW-BK112 static nitrogen adsorption instrument is purchased from Beijing Jingwei Gaokao Bokojic technology Co., Ltd;
the apparent density ρ of the measurement silicaApparent appearanceThe method comprises the following specific steps: weighing 3g of sample, accurately measuring the sample to 0.01g, placing the sample in a centrifugal tube, placing the centrifugal tube in an electric centrifuge, starting the centrifuge for 20min at the rotating speed of 2000r/min, taking out the sample, placing the sample in a square sample presser for flattening, and accurately measuring the sample to 0.1mL according to the volume of the sample;
the silicon dioxide sample powder is purchased from ZEODENT series products such as thickening type silicon dioxide (I type, II type), comprehensive type (III type), friction type silicon dioxide (IV type, V type, VI type) and the like of special chemical company Limited.
1) Measurement of apparent Density ρ of a typical silica sampleApparent appearanceAnd pore volume VPore volumeThe results of the data are shown in table 4;
2) measuring the oil absorption values of 6 typical silica samples by a manual method;
the oil absorption values are shown in the following table 4, and are obtained by manual testing, and the testing method is as follows: taking 1-2g of silicon dioxide sample, 2g of friction type silicon dioxide is needed, 1g of thickening type silicon dioxide is needed, and the oil absorption value experiment requires that the consumed oil is more than 1 g. Placing a silicon dioxide sample on a glass plate, weighing castor oil and a dropper to 0.01g, sucking the castor oil by the dropper, adding the castor oil into a sample drop by drop, thoroughly kneading the silicon dioxide sample by a tongue depressor after adding each drop, finishing the test when the silicon dioxide sample is kneaded into a very viscous dough which is not fragile and not easy to separate, and weighing the weight of the consumed castor oil by using a differential method.
TABLE 56 typical Property parameters of various types of silica samples
Figure BDA0003378404460000131
3) Fitting k and phi values according to the apparent density, pore volume and oil absorption value formulas of typical silica samples to obtain a calculation formula of the oil absorption value of the silica, and specifically comprising the following steps:
the parameters k, φ in the oil absorption value expression were fitted using the data in Table 5 and the formula (10) derived in example 1:
substituting the data in Table 5 into equation (10) yields 6 equations for k, φ,
Figure BDA0003378404460000132
Figure BDA0003378404460000133
the function image is plotted using these 6 equations, as shown in fig. 4.
From the angle of solving the equation, the best k and phi are fitted, namely a 'point (k, phi') is found, almost all curves can pass through, namely the thinnest part of the curve beam in the graph is satisfied, wherein k is more than 0.50 and less than or equal to 0.55, and phi is more than 0.50 and less than 0.55.
Taking a series of points (0.51 ), (0.51, 0.52), (0.51, 0.53), (0.51, 0.55); (0.52, 0.51), (0.52 ), (0.52, 0.53),. the. (0.52, 0.55.) the calculation of Yn is performed, and the value of (k, φ) is acceptable when the calculated Yn is less than 5% for all types of powders.
When k is 0.55 and phi is 0.545, Yn is less than 5%, and the calculation formula of the oil absorption value of the silicon dioxide is obtained by the following calculation:
Figure BDA0003378404460000141
the percentage error between the oil absorption value calculated by the formula and the manual test is shown in table 6.
TABLE 6 comparative data of oil absorption value calculated by silicon dioxide sample formula and oil absorption value measured by hand
Figure BDA0003378404460000142
The results in Table 6 show that the relative errors are less than 5%, which indicates the reasonableness of the fitting k and phi in the formula and the reasonableness of the formula derivation process.
4) And (3) measuring the apparent density and the pore volume of the silicon dioxide sample to be tested, calculating the oil absorption value of the silicon dioxide sample to be tested according to the calculation formula (13) for calculating the oil absorption value of the silicon dioxide, and simultaneously, measuring the oil absorption value of the silicon dioxide sample to be tested by a manual method for verification, wherein the test results are shown in table 7. The I ', II', III ', IV', V 'and VI' are all products of the winning special chemical company Limited.
TABLE 7 comparison data of oil absorption value calculated by formula and hand oil absorption value of silicon dioxide sample to be measured
Figure BDA0003378404460000151
The results in Table 7 show that the relative errors are less than 5%, and the reasonability of the agreed values of k and phi is further verified. In addition, according to the industry recommendations, when castor oil is used, k ranges from 0.50 to 0.60 and phi ranges from 0.46 to 0.55, and fitting is generally agreed to be performed within the range, and the applicability and practicability of the formula of the invention are illustrated within the range in the embodiment. Therefore, in the actual operation process, the method for measuring the oil absorption value of the silicon dioxide is convenient for manufacturers, customers and other parties to unify the measuring method, and is convenient for controlling and judging the product quality; in the measuring process, errors mainly come from systematic errors and random errors of apparent density measurement and pore volume measurement, and excessive human factor errors are avoided.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.

Claims (9)

1. A method for measuring the oil absorption value of silicon dioxide is characterized by comprising the following steps:
1) measurement of apparent Density ρ of a typical silica sampleApparent appearanceAnd pore volume VPore volume
2) Measuring the oil absorption value of a typical silicon dioxide sample by a manual method;
3) apparent density according to typical silica sample ρApparent appearancePore volume VPore volumeFitting an oil absorption value formula to obtain k and phi values to obtain a calculation formula of the oil absorption value of the silicon dioxide:
Figure FDA0003378404450000011
wherein the content of the first and second substances,
VpowderIs the skeletal volume of the silica powder;
ρoilAs the density of the oil used;
moilThe quality of the oil used;
ρpowderIs the skeleton density of the silicon dioxide powder;
ρapparent appearanceIs the apparent density;
Vpore volumeTo utilize the static stateThe volume of the single-point adsorption total pore measured by a nitrogen adsorption instrument;
the size of k is only related to the type and temperature of oil, and k varies within a certain range and can be appointed within the range;
the size of phi is only related to the type and temperature of oil, and phi varies within a certain range and can be appointed within the range;
4) measuring apparent density rho of silicon dioxide sample to be measuredApparent appearancePore volume VPore volumeAnd calculating the oil absorption value of the silicon dioxide sample to be detected according to the calculation formula of the oil absorption value of the silicon dioxide.
2. The method for measuring the oil absorption of silica according to claim 1, wherein the number of the typical silica samples is not less than 6.
3. The method for measuring the oil absorption value of silica according to claim 1, wherein the step 1) is carried out to measure the apparent density p of silicaApparent appearanceThe method comprises the following specific steps:
weighing 3g of sample, accurately measuring to 0.01g, placing in a centrifuge tube, placing in an electric centrifuge, starting at 2000r/min for 20min, taking out, placing in a square sample presser, flattening, and accurately measuring to 0.1mL according to the volume.
4. The method for measuring the oil absorption value of silica as claimed in claim 1, wherein the step 2) measures the pore volume V of the silicaPore volumeComprising measuring the pore volume V of the silica with a static nitrogen adsorber of the model JW-BK12Pore volumeAnd calculating by adopting a BJH pore size distribution test method.
5. The method for measuring the oil absorption value of the silica as claimed in claim 1, wherein the step 3) of manually measuring the oil absorption value of a typical silica sample, the oil used is castor oil, and the specific steps comprise:
taking 1-2g of silicon dioxide sample, placing the silicon dioxide sample on a glass plate, weighing castor oil and a dropper to 0.01g, then sucking the castor oil by the dropper, adding the castor oil into the sample drop by drop, thoroughly kneading the silicon dioxide sample by a tongue depressor after adding each drop, finishing the test when the silicon dioxide sample is kneaded into a very viscous dough which is not fragile and not easy to separate, and weighing the weight of the consumed castor oil by using a differential method.
6. The method for measuring the oil absorption value of the silica as claimed in claim 1, wherein the method for judging whether the k and the phi values fitted according to the oil absorption value formula in the step 3) are proper comprises the following specific steps: and calculating the percentage error between the formula calculation value and the manually measured oil absorption value according to the fitted k and phi, and judging that the values of the k and the phi are reasonable when the percentage error is less than 5 percent.
7. A method of measuring the oil absorption of silica as claimed in claim 1 wherein the oil used is required not to wet the silica during the measurement, otherwise the formula does not apply.
8. The method for measuring the oil absorption value of silica according to claim 1, wherein the oil is one of linseed oil, castor oil, dioctyl adipate and dibutyl phthalate.
9. Use of the measurement method according to any one of claims 1 to 8 in the detection of the oil absorption value of a powder.
CN202111425875.2A 2021-11-26 2021-11-26 Method for measuring oil absorption value of silicon dioxide Withdrawn CN114199712A (en)

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