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CN111208034A - A kind of method for measuring the solubility of paraffin in organic solvent - Google Patents

A kind of method for measuring the solubility of paraffin in organic solvent Download PDF

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Publication number
CN111208034A
CN111208034A CN201811390600.8A CN201811390600A CN111208034A CN 111208034 A CN111208034 A CN 111208034A CN 201811390600 A CN201811390600 A CN 201811390600A CN 111208034 A CN111208034 A CN 111208034A
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paraffin
solubility
organic solvent
undissolved
mass
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罗源军
刘波
张鸣
陈立义
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Zhonghao Chenguang Research Institute of Chemical Industry Co Ltd
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Zhonghao Chenguang Research Institute of Chemical Industry Co Ltd
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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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  • Health & Medical Sciences (AREA)
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Abstract

本发明涉及一种测定石蜡在有机溶剂中溶解度的方法，包括如下步骤：将过量的石蜡溶解于有机溶剂中，分离出未溶解的石蜡，根据未溶解和已溶解的石蜡的质量进行计算，得石蜡在所述有机溶剂中的溶解度。本发明采用的方法一方面对溶解达到平衡的速度没有限制，而且代表着物质达到真实溶解平衡的数据，适合推广使用。另一方面本发明提供的测定方法所需仪器简单，成本较低，可操作性强，能够准确的测定石蜡在各种有机溶剂中的溶解度。The invention relates to a method for determining the solubility of paraffin in an organic solvent. Solubility of paraffin in the organic solvent. On the one hand, the method adopted in the present invention has no limit on the speed of the dissolution reaching equilibrium, and represents the data that the material reaches the real dissolution equilibrium, which is suitable for popularization and use. On the other hand, the measuring method provided by the present invention requires simple instruments, low cost and strong operability, and can accurately measure the solubility of paraffin in various organic solvents.

Description

Method for measuring solubility of paraffin in organic solvent
Technical Field
The invention relates to the technical field of solubility test, in particular to a method for measuring the solubility of paraffin in an organic solvent.
Background
The paraffin is one of main products in the petroleum refining process, mainly comprises normal paraffin, is colorless or light yellow solid at normal temperature, generally has 16-32 carbon atoms and 300-540 molecular weight, has a fraction range of 350-500 ℃, and has a density of 0.880-0.915 kg/L. The main quality indexes of the paraffin are melting point and oil content, wherein the former represents temperature resistance, and the latter represents purity. Each wax is divided into different varieties according to melting points, such as the brands of 52, 54, 56, 58 and the like. According to different processing and refining degrees, the method can be divided into three types of fully refined paraffin, semi-refined paraffin and crude paraffin. The oil content of the fully refined paraffin is less than 0.8 percent, and the oil content of the semi-refined paraffin is less than 1.8 percent. Among them, the 58 # fully refined paraffin wax plays an important role as a stabilizer in the polytetrafluoroethylene dispersion resin industry, and in the dispersion polymerization thereof, the paraffin wax as a dispersion stabilizer of the reaction system is substantially inactive and is in a liquid state under the reaction conditions. The function of the emulsion breaking inhibitor is to reduce the adhesion phenomenon of the fluororesin on the inner wall of the polymerization kettle and the stirring paddle on one hand, and reduce the probability of forming large particles due to collision among fluororesin particles on the other hand, so that the polymerization system is more stable, the generation of aggregates is prevented, and the emulsion breaking phenomenon is prevented to a certain extent. The dosage of the paraffin has important influence on the dispersion polymerization of PTFE and the performance of products, the resin bonding phenomenon is obviously reduced along with the increase of the dosage of the paraffin, the tensile strength and the elongation at break are improved, but the polymerization reaction rate is reduced. In actual production, the amount used is preferably 0.1% to 12% based on the mass of water used. However, in the processes of liquid separation and coagulation after the reaction, a part of PTFE dispersion resin and the rest of paraffin are often tightly wrapped in the intermediate transition layer, and the PTFE dispersion resin cannot be recovered by the traditional 'water boiling process'. According to the characteristics of paraffin, the extraction effect of the organic solvent is obviously better than that of the traditional 'water boiling process' by utilizing the principle of 'similar and compatible'. However, the theoretical prediction and various estimation methods of the solid solubility are not mature and complete enough at present, so that the determination of the solid solubility is still based on experimental research tests. At present, the solubility determination methods commonly used in laboratories, such as chromatography, potentiometric titration and spectrophotometry, are often impossible to perform due to the high melting point and chemical inertness of paraffin.
At present, no relevant literature reports about a method for measuring the solubility of paraffin in an organic solvent at home and abroad, and a similar Chinese patent (publication number: CN102262031A) discloses a method for measuring the practical solubility of calcium sulfate for papermaking fillers.
Disclosure of Invention
In order to determine the solubility of paraffin in different organic solvents, the invention provides a simple and rapid method for determining the solubility of paraffin in organic solvents, which comprises the following steps: and dissolving excessive paraffin in an organic solvent, separating undissolved paraffin, and calculating according to the mass of the undissolved paraffin and the dissolved paraffin to obtain the solubility of the paraffin in the organic solvent.
Preferably, the volume of the organic solvent is 50-100 mL, the dissolving grade of the common paraffin in the organic solvent is between slightly soluble and easily soluble, the corresponding solvent amount is 10-1000 mL, and under the condition of not influencing the experimental result, 50-100 mL is convenient for laboratory operation and subsequent waste liquid treatment.
Preferably, the organic solvent is placed in a narrow-mouth bottle. Placing the paraffin in a narrow-mouth bottle can promote full dissolution of the paraffin by shaking. In the operation process, the narrow-mouth bottle is a conical bottle or a triangular bottle.
Preferably, the fineness of the paraffin is 100 meshes or more than 100 meshes. The paraffin wax of the above-mentioned fineness is more likely to be sufficiently dissolved in an organic solvent.
Preferably, the paraffin is added into the solvent for 2-5 times, and after each addition, the narrow-mouth bottle is oscillated to promote the dissolution of the paraffin. Through the operation, the paraffin is more favorably and fully dissolved.
Preferably, the solution system is kept still for 22-26 hours before the undissolved paraffin is separated.
Preferably, the undissolved paraffin is separated off by filtration.
As a preferred method, the method of the present invention comprises the steps of:
1) preparation before measurement: putting the cleaned beaker and quantitative filter paper in a drying oven at 105-110 ℃ for drying for 20-40 min, taking out the beaker and putting the beaker and the quantitative filter paper in a drier for cooling for 20-40 min, weighing the beaker and the quantitative filter paper againFeeding the beaker and quantitative filter paper into the oven with the same temperature, drying for 20-40 min, cooling and weighing, repeating the steps until the weight difference between the two times is less than 0.0004g, and recording the mass m1；
2) And (3) testing: pulverizing solid paraffin to fineness greater than or equal to 100 mesh for use, and accurately weighing the powder3Putting paraffin into a dry conical flask, adding a solvent with the volume of v into the conical flask, fully shaking and shaking at 25 +/-2 ℃ until the paraffin is fully dissolved, standing for 22-26 h, filtering with the quantitative filter paper in the step 1), putting the quantitative filter paper with filter residues into the beaker in the step 1), transferring the beaker into a drying oven with the temperature of 105-110 ℃ for drying for 3-5 h, putting the beaker into a drier for cooling for 20-40 min, weighing, continuing to dry for half an hour, weighing again after cooling, repeating the steps until the weight is constant, and recording the mass m2；
3) And (3) calculating the solubility: the solubility was: x ═ m3-(m2-m1)]/ν×103。
The invention has the following beneficial effects:
1) the method adopted by the invention has no limit on the speed of reaching the equilibrium of dissolution, represents the data of the real dissolution equilibrium of the substance and is suitable for popularization and application.
2) The measuring method provided by the invention has the advantages of simple required instrument, low cost and strong operability, and can accurately measure the solubility of paraffin in various organic solvents.
The method has better guiding significance in the engineering practice of extracting the waxy PTFE waste residue by the organic solvent and recycling the paraffin with high added value.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
1) Preparation before measurement: putting the cleaned 50mL beaker and quantitative filter paper in a drying oven at 105-110 ℃ for drying for 30min, taking out the beaker, putting the beaker in a drier for cooling for 30min, weighing, putting the 50mL beaker and the quantitative filter paper into the drying oven at the same temperature for drying for 30min, cooling and weighing, and repeating the steps until the weight of the beaker and the quantitative filter paper reaches twiceUntil the difference is less than 0.0004g, the mass m is recorded1＝42.754g。
2) Measurement: the solid paraffin is crushed into the fineness of more than or equal to 100 meshes by a laboratory crusher (FW-200, Beijing Zhongxing Weiwei instruments Co., Ltd.) for standby. Accurately weighing powdered paraffin m3Putting 9.990g of the extract into a 125mL conical flask, adding 50mL of corresponding solvent, fully shaking and shaking at 25 +/-2 ℃ for 30min, standing for 24h, filtering by using slow quantitative filter paper, putting the quantitative filter paper with filter residue into a 50mL beaker with constant weight, transferring the beaker into an oven at 105-110 ℃ for drying for 4h, putting the beaker into a drier for cooling for 30min, weighing, continuing to dry for half an hour, weighing again, repeating the process until the weight is constant, and recording the mass m until the weight is constant2The calculated solubility of paraffin wax in chloroform was found to be 175.2 g/L43.982 g.
Example 2
This example relates to a method for determining the solubility of paraffin in organic solvents, the procedure of the test of this example being identical to that of example 1, except that the organic solvent used is dichloromethane, and m is obtained1＝39.080g，m2＝48.269g，m3The calculated solubility of paraffin wax in methylene chloride was found to be 20.4 g/L10.212 g.
Example 3
This example relates to a method for determining the solubility of paraffin in organic solvents, the procedure of the test of this example being identical to example 1, except that the organic solvent used is carbon tetrachloride, and m is obtained1＝43.245g，m2＝45.022g，m310.741g, the calculated solubility of paraffin wax in carbon tetrachloride was 179.252 g/L.
Example 4
This example relates to a method for determining the solubility of paraffin in organic solvents, the procedure of the test of this example being identical to example 1, except that the organic solvent used is n-hexane, m is obtained1＝39.263g，m2＝43.205g，m310.080g, the calculated solubility of paraffin wax in n-hexane was 122.8 g/L.
Example 5
This example relates to a method for determining the solubility of paraffin in organic solvents, the procedure of the test of this example being identical to that of example 1, except that the organic solvent used is cyclohexane, and m is obtained1＝35.262g，m2＝36.118g，m3The calculated solubility of paraffin wax in cyclohexane was found to be 175.7 g/L9.640 g.
Example 6
This example relates to a method for determining the solubility of paraffin in organic solvents, the procedure of the test of this example being identical to that of example 1, except that the organic solvent used is acetonitrile, m being obtained1＝39.633g，m2＝49.205g，m3The calculated solubility of paraffin wax in acetonitrile was found to be 19.0 g/L10.521 g.
Example 7
This example relates to a method for determining the solubility of paraffin in organic solvents, the procedure of the test of this example being identical to that of example 1, except that the organic solvent used is acetone, and m is obtained1＝35.335g，m2＝44.820g，m3The calculated solubility of paraffin wax in acetone was found to be 18.7 g/L10.422 g.
Example 8
This example relates to a method for determining the solubility of paraffin in organic solvents, the procedure of the test of this example being identical to that of example 1, except that the organic solvent used is methanol, and m is obtained1＝38.991g，m2＝47.948g，m3The calculated solubility of paraffin wax in methanol was found to be 26.9 g/L10.310 g.
Example 9
This example relates to a method for determining the solubility of paraffin in organic solvents, the procedure of the test of this example being identical to that of example 1, except that the organic solvent used is tetrahydrofuran, and m is obtained1＝31.410g，m2＝39.597g，m3The calculated solubility of paraffin wax in tetrahydrofuran was 10.813g, which was 52.5 g/L.
Example 10
The embodiment relates to a method for dissolving paraffin in organic solventMethod for determining the solubility in a solvent, the procedure for testing this example being identical to that of example 1, except that the organic solvent used is ethyl acetate, m obtained1＝43.379g，m2＝52.223g，m3The calculated solubility of paraffin wax in ethyl acetate was found to be 23.7 g/L10.030 g.
Example 11
This example relates to a method for determining the solubility of paraffin in organic solvents, the procedure of the test of this example being identical to that of example 1, except that the organic solvent used is ethanol, and m is obtained1＝39.515g，m2＝49.690g，m3The calculated solubility of paraffin wax in ethanol was 14.3 g/L10.891 g.
Example 12
This example relates to a method for determining the solubility of paraffin in organic solvents, the procedure of the test of this example being identical to that of example 1, except that the organic solvent used is benzene, and m is obtained1＝40.535g，m2＝44.045g，m3The calculated solubility of paraffin wax in benzene was 147.4 g/L10.880 g.
Example 13
This example relates to a method for determining the solubility of paraffin in organic solvents, the procedure of the test of this example being identical to that of example 1, except that the organic solvent used is isopropanol, and m is obtained1＝39.713g，m2＝45.727g，m3The calculated solubility of paraffin wax in isopropanol was 10.092g, which was 81.5 g/L.
Although the invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it will be apparent to those skilled in the art that many modifications and improvements can be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.

Claims (9)

1.一种测定石蜡在有机溶剂中溶解度的方法，其特征在于，包括如下步骤：1. a method for measuring the solubility of paraffin in an organic solvent, is characterized in that, comprises the steps: 将过量的石蜡溶解于有机溶剂中，分离出未溶解的石蜡，根据未溶解和已溶解的石蜡的质量进行计算，得石蜡在所述有机溶剂中的溶解度。Dissolving the excess paraffin in the organic solvent, separating the undissolved paraffin, and calculating according to the mass of the undissolved and dissolved paraffin, the solubility of the paraffin in the organic solvent is obtained. 2.根据权利要求1所述的方法，其特征在于，所述有机溶剂的体积为50～100ml。2 . The method according to claim 1 , wherein the volume of the organic solvent is 50-100 ml. 3 . 3.根据权利要求1或2所述的方法，其特征在于，所述有机溶剂置于细口瓶中。3. The method according to claim 1 or 2, wherein the organic solvent is placed in a narrow-mouthed bottle. 4.根据权利要求1～3任一项所述的方法，其特征在于，所述石蜡的细度为100目或大于100目。4 . The method according to claim 1 , wherein the fineness of the paraffin wax is 100 mesh or more than 100 mesh. 5 . 5.根据权利要求1～4任一项所述的方法，其特征在于，将所述石蜡分2～5次添加到所述溶剂中，每次添加完毕后，振荡所述细口瓶，促进石蜡的溶解。5. The method according to any one of claims 1 to 4, wherein the paraffin is added to the solvent in 2 to 5 times, and after each addition, the narrow-mouthed bottle is shaken to promote Paraffin dissolution. 6.根据权利要求1～5任一项所述的方法，其特征在于，分离所述未溶解的石蜡前，将溶液体系静置22～26h。The method according to any one of claims 1 to 5, characterized in that, before separating the undissolved paraffin, the solution system is allowed to stand for 22 to 26 hours. 7.根据权利要求1～6所述的方法，其特征在于，未溶解的石蜡的质量为石蜡总质量的10～90％。7 . The method according to claim 1 , wherein the mass of the undissolved paraffin wax is 10-90% of the total mass of the paraffin wax. 8 . 8.根据权利要求1～7任一项所述的方法，其特征在于，通过过滤分离出未溶解的石蜡。8. The method according to any one of claims 1 to 7, wherein undissolved paraffin is separated by filtration. 9.根据权利要求1～8任一项所述的方法，其特征在于，包括如下步骤：9. The method according to any one of claims 1 to 8, characterized in that, comprising the steps of: 1)测前准备：将洗净的烧杯与定量滤纸放在105～110℃烘箱中烘干20～40min，取出后置于干燥器中冷却20～40min后称重，再次将所述烧杯及定量滤纸送入上述同温度烘箱烘20～40min，再冷却称重，如此重复到两次重量之差小于0.0004g为止，记下质量m1；1) Preparation before measurement: put the washed beaker and quantitative filter paper in an oven at 105 to 110 °C for 20 to 40 minutes, take them out, cool them in a dryer for 20 to 40 minutes, and weigh them. The filter paper is sent into the above-mentioned oven at the same temperature for 20-40 minutes, and then cooled and weighed. Repeat this until the difference between the two weights is less than 0.0004g, and record the mass m 1 ; 2)测试：将固体石蜡粉碎至细度大于或等于100目待用，准确称取研成粉末状的质量为m3石蜡的置于干燥的锥形瓶中，向其中加入体积为ν的溶剂，在25±2℃下充分摇匀震荡至石蜡充分溶解，静置22～26h，用步骤1)所述的定量滤纸过滤，将附有滤渣的定量滤纸放入步骤1)所述的烧杯中，移入105～110℃烘箱内烘干3～5h，放入干燥器中冷却20～40min后称重，继续烘半小时，冷却后再次程重，如此反复直至恒重为止，记下质量m2；2) Test: pulverize the solid paraffin to a fineness greater than or equal to 100 meshes for use, accurately weigh and grind the powdered paraffin with a mass of m3 and place it in a dry Erlenmeyer flask, and add a solvent with a volume of v to it. , shake well at 25±2°C until the paraffin is fully dissolved, let stand for 22-26 hours, filter with the quantitative filter paper described in step 1), and put the quantitative filter paper with filter residue into the beaker described in step 1). , move it into a 105-110 ℃ oven to dry for 3-5 hours, put it in a desiccator to cool for 20-40 minutes, weigh it, continue to bake for half an hour, and re - weight it after cooling. ; 3)溶解度计算：溶解度为：X＝[m3-(m2-m1)]/ν×103。3) Solubility calculation: The solubility is: X=[m 3 -(m 2 -m 1 )]/ν×10 3 .
CN201811390600.8A 2018-11-21 2018-11-21 A kind of method for measuring the solubility of paraffin in organic solvent Pending CN111208034A (en)

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CN115326631A (en) * 2022-08-23 2022-11-11 西北大学 Method for realizing rapid measurement of solute solubility by adding anti-solvent

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Application publication date: 20200529