CN111208034A - Method for measuring solubility of paraffin in organic solvent - Google Patents
Method for measuring solubility of paraffin in organic solvent Download PDFInfo
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- 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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- 239000012188 paraffin wax Substances 0.000 title claims abstract description 91
- 238000000034 method Methods 0.000 title claims abstract description 56
- 239000003960 organic solvent Substances 0.000 title claims abstract description 47
- 238000004090 dissolution Methods 0.000 claims abstract description 7
- 238000012360 testing method Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 11
- 239000002904 solvent Substances 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000005259 measurement Methods 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 3
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000006116 polymerization reaction Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 238000012674 dispersion polymerization Methods 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 238000003918 potentiometric titration Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
Classifications
-
- 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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- 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)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to a method for measuring the solubility of paraffin in an organic solvent, 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. The method adopted by the invention has no limit on the speed of reaching the equilibrium by dissolution on one hand, represents the data of the real dissolution equilibrium of the substance and is suitable for popularization and application. On the other hand, the measuring method provided by the invention has the advantages of simple required instrument, lower cost and strong operability, and can accurately measure the solubility of paraffin in various organic solvents.
Description
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. A method for determining the solubility of paraffin in an organic solvent, comprising the steps of:
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.
2. The method according to claim 1, wherein the volume of the organic solvent is 50 to 100 ml.
3. The method according to claim 1 or 2, wherein the organic solvent is placed in a narrow-mouth bottle.
4. The method according to any one of claims 1 to 3, wherein the fineness of the paraffin is 100 mesh or more than 100 mesh.
5. The method according to any one of claims 1 to 4, wherein the paraffin is added to the solvent 2 to 5 times, and after each addition, the narrow-necked flask is shaken to promote the dissolution of the paraffin.
6. The method according to any one of claims 1 to 5, wherein the solution system is allowed to stand for 22 to 26 hours before the undissolved paraffin is separated.
7. A method according to claims 1 to 6, characterized in that the mass of undissolved paraffin is 10 to 90% of the total mass of paraffin.
8. A method according to any one of claims 1 to 7, characterized in that the undissolved paraffin is separated by filtration.
9. A method according to any one of claims 1 to 8, comprising the steps of:
1) preparation before measurement: putting the cleaned beaker and quantitative filter paper into 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 into a dryer for cooling for 20-4 minWeighing after 0min, feeding the beaker and quantitative filter paper into the oven with the same temperature for 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。
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| CN201811390600.8A CN111208034A (en) | 2018-11-21 | 2018-11-21 | Method for measuring solubility of paraffin in organic solvent |
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| CN201811390600.8A CN111208034A (en) | 2018-11-21 | 2018-11-21 | Method for measuring solubility of paraffin in organic solvent |
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| CN204101401U (en) * | 2014-09-26 | 2015-01-14 | 中国石油化工股份有限公司 | A kind of asphaltene dissolution degree determinator |
| JP5709826B2 (en) * | 2005-12-16 | 2015-04-30 | レオ ラボラトリーズ リミテッド | Therapeutic composition |
| CN207600883U (en) * | 2017-10-09 | 2018-07-10 | 昆明理工大学 | A kind of measurement device of volatile organic matter apparent solubility |
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2018
- 2018-11-21 CN CN201811390600.8A patent/CN111208034A/en active Pending
Patent Citations (7)
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| JP5709826B2 (en) * | 2005-12-16 | 2015-04-30 | レオ ラボラトリーズ リミテッド | Therapeutic composition |
| CN102234525A (en) * | 2010-05-07 | 2011-11-09 | 北京安耐吉能源工程技术有限公司 | Method for reducing water content in hydrocarbon oil |
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| CN101949913A (en) * | 2010-09-03 | 2011-01-19 | 中国石油化工股份有限公司 | Device and method for testing solubility of insoluble substance |
| CN103951672A (en) * | 2014-04-08 | 2014-07-30 | 天津大学 | Method for extracting wedelolactone and method for determining solubility of wedelolactone |
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Application publication date: 20200529 |