CN110763807A - Method for quickly separating water, soap and oil in emulsion and measuring oil concentration - Google Patents
Method for quickly separating water, soap and oil in emulsion and measuring oil concentration Download PDFInfo
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- 239000000839 emulsion Substances 0.000 title claims abstract description 151
- 239000003921 oil Substances 0.000 title claims abstract description 150
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000000034 method Methods 0.000 title claims abstract description 65
- 239000000344 soap Substances 0.000 title claims abstract description 62
- 238000010438 heat treatment Methods 0.000 claims abstract description 60
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 28
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims description 17
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- 239000002994 raw material Substances 0.000 abstract description 2
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- 150000002367 halogens Chemical class 0.000 description 5
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4044—Concentrating samples by chemical techniques; Digestion; Chemical decomposition
-
- G01N33/0003—
Abstract
The invention belongs to the field of chemical analysis of energy medium raw materials, and relates to a method for quickly separating water, soap and oil in emulsion and measuring the concentration of the oil. The method for quickly separating the water, the soap and the oil of the emulsion comprises the following steps: (1) adding concentrated sulfuric acid into the emulsion, uniformly mixing, and heating to 50-80 ℃; (2) adding saturated sodium chloride solution at 50-80 deg.c and heating to 80-100 deg.c; (3) and (4) separating water, soap and oil in the emulsion and then stopping heating. The method for quickly separating the water, the soap and the oil of the emulsion realizes the purpose of quickly and accurately detecting the quick separation of the water, the soap and the oil in the process of detecting the concentration of the cold-rolled emulsion oil.
Description
Technical Field
The invention belongs to the field of chemical analysis of energy medium raw materials, relates to a method for quickly separating water, soap and oil from emulsion and measuring the concentration of the oil, and particularly relates to a technology for quickly separating water, soap and oil from silicon steel cold rolling emulsion in the using process.
Background
The emulsion is a high-performance semisynthetic metal working fluid, and comprises the following main chemical components: water, rolling oil, surfactants, rust inhibiting additives, antioxidants, friction modifiers, and the like. The emulsion is used for solving the problems of chip adhesion, tool abrasion, poor workpiece surface precision, surface pollution and the like during alloy processing.
If the oil concentration in the emulsion is low, the lubricating property of the roller and the steel plate is poor, the bearing of the supporting roller is easy to burn, and the rolled steel plate is easy to rust. If the oil concentration of the emulsion is kept at a high value for a long time, although the oil concentration is beneficial to rolled steel plates, rolling mill rolls and bearings, a large amount of rolling oil is wasted, so that the production cost per ton of steel is greatly increased, and the defects of difficult cleaning, formation of surface black spots and the like at the later stage are easily caused. Therefore, the method has important significance for ensuring the quality of the steel strip and saving the production cost by accurately measuring and controlling the concentration of the emulsion within a target range.
The detection of the oil concentration of the emulsion refers to the content of rolling oil in the emulsion. There are two methods for conventional oil concentration detection: (1) detecting by a halogen moisture tester; (2) acid separation by heating in water bath. The detection method of the halogen moisture determinator comprises the steps of removing moisture in an emulsion by heating, and measuring the weight ratio of a solid substance to an original emulsion to obtain a detection result. Because impurities in the sample cannot be removed, the oil concentration value of the emulsion is seriously high, and the detection accuracy is poor. The water bath heating acid separation method is characterized in that excessive strong acid is added to demulsify, and then the emulsifier is separated into three layers of water, soap and oil by water bath heating. Wherein the oil concentration is +1/2 soap layer concentration. The method has the defects that the water bath heating temperature is not uniform, a soap layer contains a large amount of missible oil (as shown in figure 1), the deviation between a detection result and the actual oil concentration is large, and in addition, the demulsification capability of pure strong acid is poor, and the demulsification of emulsion with strong stability is incomplete.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for quickly separating water, soap and oil in emulsion and measuring the concentration of the oil.
On one hand, the method for quickly separating the water, the soap and the oil of the emulsion comprises the following steps:
(1) adding concentrated sulfuric acid into the emulsion, uniformly mixing, and heating to 50-80 ℃;
(2) adding saturated sodium chloride solution at 50-80 deg.c and heating to 80-100 deg.c;
(3) and (4) separating water, soap and oil in the emulsion and then stopping heating.
In the method for quickly separating the water, the soap and the oil from the emulsion, the heating is carried out in a thermostat.
In the method for quickly separating the water, the soap and the oil from the emulsion, the concentration of the concentrated sulfuric acid is 80-98%.
In another aspect, the method of the present invention for determining the oil concentration in an emulsion comprises the steps of:
(1) weighing a certain amount of emulsion, putting the emulsion into a concentration bottle, adding concentrated sulfuric acid, uniformly mixing, and heating to 50-80 ℃;
(2) adding a saturated sodium chloride solution at the temperature of 50-80 ℃ to ensure that the liquid surface is positioned at the narrow neck of the concentration bottle with scale marks, and heating to 80-100 ℃;
(3) separating water, soap and oil in the emulsion, stopping heating, and reading the volume of the oil;
(4) the oil concentration in the emulsion was calculated according to the following formula:
C＝Voil/VEmulsion liquid×100％
Wherein: c is the oil concentration in the emulsion,%;
Vemulsion liquidIs the volume of the emulsion, mL;
VoilVolume of oil, mL.
In the method for measuring the oil concentration in the emulsion, in the step (1), half of the quantitative emulsion is added into the concentration bottle, concentrated sulfuric acid is added and mixed uniformly, the mixture is preheated to 30-50 ℃, then the other half of the quantitative emulsion is added, and the mixture is heated to 50-80 ℃ after being mixed uniformly.
In the method for determining the oil concentration in the emulsion, the heating is carried out in a thermostat.
In the method for measuring the oil concentration in the emulsion, the concentrated sulfuric acid has a concentration of 80-98%.
In the method for measuring the oil concentration in the emulsion, in the step (1), the preheating time is 10-20min, and the heating time is 20-40 min.
In the method for measuring the oil concentration in the emulsion, in the step (1), the preheating time is 15min, and the heating time is 30 min.
The method for determining the concentration of the oil in the emulsion comprises the steps that the concentration bottle comprises a flat-bottom bottle body and a thin neck; wherein, the thin neck is carved with scale marks.
The technical scheme of the invention has the following beneficial effects:
(1) the method for quickly separating the water, the soap and the oil of the emulsion disclosed by the invention optimizes the traditional emulsion breaking method, improves the emulsion breaking effect, reduces the acid discharge amount and improves the environment of a working place, and the thermostat is adopted to replace a water bath for heating and heat preservation, so that a test sample is uniformly heated, the water, the soap and the oil are effectively separated, and the aim of quickly and accurately measuring the quick separation of the water, the soap and the oil in the process of detecting the concentration of the oil by using the cold-rolled emulsion for silicon steel is fulfilled;
(2) the method for measuring the oil concentration in the emulsion can shorten the analysis period, reduce the labor intensity, save manpower and material resources, reduce the purchase and storage cost and greatly improve the analysis efficiency, and the analysis precision and the accuracy of the method both meet the requirements of the national chemical analysis method on the analysis precision and the accuracy;
(3) the method for measuring the oil concentration in the emulsion can be applied to the accurate measurement of water, soap and oil separation in the process of measuring the oil concentration in the cold rolling emulsion for silicon steel, can be popularized to all production units using rolling oil, and has strong practical value;
(4) the field detection result shows that when the aging degree of the emulsion is higher and the impurity content is higher, the oil concentration of the emulsion measured by the method is more accurate, and the requirement of a silicon steel plant on quality detection is met.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention.
FIG. 1 is a schematic diagram showing the distribution of oil and soap in an emulsion after separation by a conventional water bath heating acid separation method;
FIG. 2 is a schematic diagram showing the distribution of oil and soap in an emulsion after separation according to the method for determining the oil concentration in an emulsion of the present invention;
FIG. 3 is a schematic diagram of a concentration bottle used in the present invention;
wherein, 1 is an oil layer, and 2 is a soap layer.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to fully understand the objects, features and effects of the invention. The process of the present invention employs conventional methods or apparatus in the art, except as described below. The following noun terms have meanings commonly understood by those skilled in the art unless otherwise specified.
When the emulsion is used for a long time and the impurity content is high, the conditions that the oil layer is few and most of the oil layer is a soap layer and water is in oil after demulsification occur, so that accurate oil concentration data of the emulsion cannot be obtained, and the oil concentration of a site cannot be accurately monitored. The invention aims to optimize a technical method for separating water, soap and oil in the oil concentration in the silicon steel cold rolling emulsion detection process, provides a simple, convenient, rapid, accurate and reliable water-oil separation technology, and can accurately detect the oil concentration of the emulsion with higher oil aging degree and higher impurity content.
Specifically, the invention discloses a method for quickly separating water, soap and oil from emulsion, which comprises the following steps:
(1) adding concentrated sulfuric acid into the emulsion, uniformly mixing, and heating to 50-80 ℃;
(2) adding saturated sodium chloride solution at 50-80 deg.c and heating to 80-100 deg.c;
(3) and (4) separating water, soap and oil in the emulsion and then stopping heating.
The addition amount of the concentrated sulfuric acid may be adjusted according to the volume, aging degree, and the like of the emulsion, and the present invention is not limited specifically herein.
Preferably, the heating is performed in an oven, and optionally, the heating may also be performed in an oven.
According to the method for quickly separating the water, the soap and the oil from the emulsion, the constant temperature box is adopted for heating and heat preservation, so that the test sample is uniformly heated, and the water, the soap and the oil are quickly and effectively separated. Thereby solving the problems that the sample is heated unevenly when the water bath kettle is heated, part of oil phase is not separated out at the saponified part, the detection time is long, and the like.
Preferably, the concentration of the concentrated sulfuric acid is 80% -98%, and more preferably, the concentration of the concentrated sulfuric acid is 98%.
The method for quickly separating the water, the soap and the oil of the emulsified liquid optimizes the traditional emulsion breaking method, improves the emulsion breaking effect, reduces the acid discharge amount, improves the environment of a working place and realizes the purpose of quickly and accurately detecting the separation of the water, the soap and the oil in the oil concentration in the process of detecting the cold-rolled emulsified liquid for silicon steel by adopting concentrated sulfuric acid and hot saturated NaCl (as shown in figure 2).
In another aspect, the invention also provides a method for determining the oil concentration in an emulsion. The method for measuring the oil concentration in the emulsion adopts a special concentration bottle, and can quickly and accurately calculate the oil concentration in the emulsion after separating the water, the soap and the oil in the emulsion by utilizing the method for quickly separating the water, the soap and the oil in the emulsion.
Specifically, the method for determining the oil concentration in the emulsion comprises the following steps:
(1) weighing a certain amount of emulsion, putting the emulsion into a concentration bottle, adding concentrated sulfuric acid, uniformly mixing, and heating to 50-80 ℃.
The concentration bottle is a narrow-necked bottle with scales, and comprises a flat-bottomed bottle body and a narrow neck as shown in fig. 3; wherein the thin neck is also marked with scale marks.
In view of safety, the concentration bottle does not use a sealing bottle stopper when being heated in a thermostat, and the bottle opening is blocked by a breathable material such as absorbent cotton.
Preferably, the heating is performed in an incubator; alternatively, the heating may also be performed in an oven. The constant temperature box is adopted for heating and heat preservation, so that the test sample is uniformly heated, and the separation of water, soap and oil is accelerated.
Wherein the concentration of the concentrated sulfuric acid is 80% -98%, and preferably, the concentration of the concentrated sulfuric acid is 98%.
Preferably, the concentration bottle is filled with half of the quantitative emulsion, then concentrated sulfuric acid is added and mixed uniformly, the mixture is preheated to 30-50 ℃, then the other half of the quantitative emulsion is added, and the mixture is mixed uniformly again and heated to 50-80 ℃.
According to the invention, one half of quantitative emulsion and concentrated sulfuric acid are preheated to 30-50 ℃ and then the other half of the quantitative emulsion is added and heated to 50-80 ℃, so that on one hand, the strong oxidizing property of the concentrated sulfuric acid can be utilized to rapidly break the water-oil bond of part of the emulsion, thereby forming a chain reaction, greatly improving the demulsifying capability and demulsifying speed, on the other hand, the thermal spraying caused by excessive liquid poured in one time can be avoided, and the operation is safer and more reliable.
In the step (1), the preheating time is 10-20min, and the heating time is 20-40 min. Preferably, the preheating time is 15min, and the heating time is 30 min.
(2) Adding saturated sodium chloride solution at 50-80 deg.c to make the liquid level in the narrow neck of the concentration bottle with scale mark, and heating to 80-100 deg.c.
The invention can further separate the part which can not be demulsified by concentrated sulfuric acid in the emulsion into water, soap and oil by adding a saturated sodium chloride solution with the temperature of 50-80 ℃ into a concentration bottle. Therefore, the emulsion, particularly the emulsion with higher aging degree and impurity content, can be separated from water, soap and oil more thoroughly, and the accuracy of the method for determining the oil concentration in the emulsion is further ensured.
On the other hand, the oil and soap separated from the emulsion can be located at the narrow neck with the graduation lines by adding saturated sodium chloride solution, so as to be convenient for accurately reading and calculating the volume of the oil and soap.
In some embodiments, the liquid level is located around the 5mL mark on the narrow neck of the concentration vial.
(3) After separating the water, soap and oil in the emulsion, the heating was stopped and the volume of the oil was read.
(4) The oil concentration in the emulsion was calculated according to the following formula:
C＝Voil/VEmulsion liquid×100％
Wherein: c is the oil concentration in the emulsion,%;
Vemulsion liquidIs the volume of the emulsion, mL;
VoilVolume of oil, mL.
In some preferred embodiments, 100mL of the emulsion is directly measured, and the volume of oil is directly read after the water, soap and oil in the emulsion are separated. Since the value of the oil volume is equal to the value of the oil concentration in the emulsion. Therefore, the oil concentration in the emulsion can be obtained more conveniently and more quickly.
The temperature of the constant temperature box is set by dividing the temperature into three times: the temperature setting of the first two times is not too high at 30-50 ℃, 50-80 ℃ and 80-100 ℃, the concentration bottle is conveniently taken out to add the emulsion or the demulsification medium, but not too low, otherwise, the demulsification capability is influenced, the temperature is raised for the third time to reach the optimal demulsification temperature of 80-100 ℃, and the complete demulsification is ensured.
In some embodiments, the aging of the emulsion can also be analyzed by reading the soap data. Thereby being convenient for technicians to judge whether to replace the new emulsion.
The invention utilizes the characteristic that the oil and the soap float on the water surface due to the fact that the density of the oil and the soap is smaller than that of the water, adopts the concentration bottle to enable the oil and the soap to be positioned at the thin neck with scales, can conveniently read the volume without separating the oil or the soap separately, and saves time and detection cost.
In some embodiments, the water, soap, and oil of the emulsion can be separated in other containers (e.g., beaker, flask, etc.) by the rapid water, soap, and oil separation method of the present invention, and then the volume of oil can be measured separately to determine the oil concentration in the emulsion.
The method for determining the oil concentration in the emulsion adopts concentrated H2SO4And the thermally saturated NaCl solution is used as a demulsifier, and the oil and water in the emulsified oil-water mixed solution are separated by chemical action, so that the dispersion system of the emulsion is destroyed, and the aim of separating each component in the emulsion is fulfilled. In addition, the invention improves the equipment, and because the water bath kettle generates steam and is difficult to seal, the heating sample and the water bath have the defects of temperature difference, delayed temperature control, uneven sample heating and the like. The invention adopts the constant temperature box to replace a water bath, solves the problems of uneven heating of the sample, no separation of part of oil phase in the saponified part, long detection time and the like, thereby obtaining the proportional value of the oil and the water in the emulsion and accurately calculating the concentration value thereof.
Examples
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. Experimental procedures without specifying specific conditions in the following examples were carried out according to conventional methods and conditions. The starting materials used in the following examples are all conventionally commercially available.
Example 1
100mL of the 1# sample emulsion was measured in a measuring cylinder. Pouring one half of the emulsion into a concentration bottle, slowly adding 3mL of 98% concentrated sulfuric acid into the concentration bottle, shaking up, and placing in an oven at 30-40 ℃ for heating for 15 minutes. And taking the concentration bottle out of the oven, pouring the rest emulsion into the concentration bottle, shaking up, and placing in an oven at 50-60 ℃ for heating for 30 minutes. And (3) taking the concentration bottle out of the oven, slightly cooling, adding hot saturated NaCl to enable the liquid level to be positioned at a scale of 5mL, putting the concentration bottle into the oven at 80-100 ℃, taking the concentration bottle out when the oil, the soap and the water of the emulsion are completely separated, reading the volume of the oil to be 3.2mL, and calculating the concentration of the oil in the emulsion to be 3.2%.
Example 2
100mL of the 1# sample emulsion was measured in a measuring cylinder. Pouring one half of the emulsion into a concentration bottle, slowly adding 5mL of 98% concentrated sulfuric acid into the concentration bottle, shaking up, and placing in an oven at 30-40 ℃ for heating for 10 minutes. And taking the concentration bottle out of the oven, pouring the rest emulsion into the concentration bottle, shaking up, and placing in an oven at 50-60 ℃ for heating for 20 minutes. And (3) taking the concentration bottle out of the oven, slightly cooling, adding hot saturated NaCl to enable the liquid level to be positioned at a scale of 5mL, putting the concentration bottle into the oven at 80-100 ℃, taking the concentration bottle out when the oil, the soap and the water of the emulsion are completely separated, reading the volume of the oil to be 3.1mL, and calculating the concentration of the oil in the emulsion to be 3.1%.
Example 3
100mL of the 1# sample emulsion was measured in a measuring cylinder. Pouring one half of the emulsion into a concentration bottle, slowly adding 8mL of 98% concentrated sulfuric acid into the concentration bottle, shaking up, and placing in an oven at 40-50 ℃ for heating for 15 minutes. And taking the concentration bottle out of the oven, pouring the rest emulsion into the concentration bottle, shaking up, and placing in an oven at 70-80 ℃ for heating for 30 minutes. And (3) taking the concentration bottle out of the oven, slightly cooling, adding hot saturated NaCl to enable the liquid level to be positioned at a scale of 5mL, putting the concentration bottle into the oven at 90-100 ℃, taking the concentration bottle out when the oil, the soap and the water of the emulsion are completely separated, reading the volume of the oil to be 3.2mL, and calculating the concentration of the oil in the emulsion to be 3.2%.
Example 4
100mL of the 1# sample emulsion was measured in a measuring cylinder. Pouring one half of the emulsion into a concentration bottle, slowly adding 10mL of 98% concentrated sulfuric acid into the concentration bottle, shaking up, and placing in an oven at 30-40 ℃ for heating for 20 minutes. And taking the concentration bottle out of the oven, pouring the rest emulsion into the concentration bottle, shaking up, and placing in an oven at 50-60 ℃ for heating for 40 minutes. And (3) taking the concentration bottle out of the oven, slightly cooling, adding hot saturated NaCl to enable the liquid level to be positioned at a scale of 5mL, putting the concentration bottle into the oven at 80-90 ℃, taking the concentration bottle out when the oil, the soap and the water of the emulsion are completely separated, reading the volume of the oil to be 3.2mL, and calculating the concentration of the oil in the emulsion to be 3.2%.
From the results of examples 1-4, it can be seen that the oil concentration of the emulsion can be accurately determined according to the technical parameters defined in the method for determining the oil concentration of the emulsion of the present invention.
Performance analysis
In order to verify that the method for determining the oil concentration in the emulsion has better accuracy, the method comprises the following step of performing 5 groups of parallel tests by using the method, a halogen moisture meter detection method and a water bath heating acid separation method.
The method of example 1 is adopted to detect the oil concentration in the emulsion of the sample No. 1-5, and the detection results are shown in Table 1.
The steps of the conventional halogen moisture meter method include: starting up, peeling, drying, weighing and reading data (the sum of oil and soap is read by the method).
The traditional water bath heating acid separation method comprises the following steps: measuring 100mL of emulsion, adding 20mL of 98% concentrated sulfuric acid, placing in a water bath, heating for 2-4 hours, cooling to room temperature, and reading the volume data of an oil layer and a 1/2 soap layer to obtain an oil concentration value.
TABLE 1 examination of the same samples for the results of the measurements in different ways
As can be seen from the results shown in table 1, the halogen moisture meter method has a high concentration value of the emulsion and a low detection accuracy because impurities in the sample cannot be removed.
The water bath heating acid separation method has two problems: (1) the pure strong acid has poor demulsification capability, the emulsion with strong stability is not completely demulsified, and the oil phase cannot be separated from the soap layer; (2) the problems that the sample heated by the water bath kettle is not uniformly heated, part of oil phase at the saponification part can not be completely separated out, the detection time is long and the like are solved. The detection result of the water bath heating acid separation method is lower than the actual oil concentration, and the detection accuracy is poor.
The method for separating water, soap and oil in the oil concentration during the process of measuring the cold-rolled emulsion for silicon steel can accurately detect the emulsion concentration with higher oil aging degree and higher impurity content, and the analysis result is satisfactory.
The present invention has been disclosed in the foregoing in terms of preferred embodiments, but it will be understood by those skilled in the art that these embodiments are merely illustrative of the present invention and should not be construed as limiting the scope of the present invention. It should be noted that all changes and substitutions equivalent to those of the embodiments are intended to be included within the scope of the claims of the present invention. Therefore, the protection scope of the present invention should be subject to the scope defined in the claims.
Claims (10)
1. A method for quickly separating water, soap and oil in emulsion is characterized by comprising the following steps:
(1) adding concentrated sulfuric acid into the emulsion, uniformly mixing, and heating to 50-80 ℃;
(2) adding saturated sodium chloride solution at 50-80 deg.c and heating to 80-100 deg.c;
(3) and (4) separating water, soap and oil in the emulsion and then stopping heating.
2. The method for rapidly separating water, soap and oil from emulsion according to claim 1, wherein the heating is performed in a thermostat.
3. The method for rapidly separating the emulsion water, the soap and the oil as claimed in claim 1, wherein the concentration of the concentrated sulfuric acid is 80-98%.
4. A method of determining the concentration of oil in an emulsion comprising the steps of:
(1) weighing a certain amount of emulsion, putting the emulsion into a concentration bottle, adding concentrated sulfuric acid, uniformly mixing, and heating to 50-80 ℃;
(2) adding a saturated sodium chloride solution at the temperature of 50-80 ℃ to ensure that the liquid surface is positioned at the narrow neck of the concentration bottle with scale marks, and heating to 80-100 ℃;
(3) separating water, soap and oil in the emulsion, stopping heating, and reading the volume of the oil;
(4) the oil concentration in the emulsion was calculated according to the following formula:
C＝Voil/VEmulsion liquid×100％
Wherein: c is the oil concentration in the emulsion,%;
Vemulsion liquidIs the volume of the emulsion, mL;
VoilVolume of oil, mL.
5. The method according to claim 4, wherein in step (1), half of the emulsion is added into the concentration bottle, concentrated sulfuric acid is added and mixed uniformly, the mixture is preheated to 30-50 ℃, then the other half of the emulsion is added, and the mixture is heated to 50-80 ℃.
6. The method of claim 4, wherein the heating is performed in a thermostat.
7. The method of claim 4, wherein the concentrated sulfuric acid has a concentration of 80% to 98%.
8. The method for determining the oil concentration in an emulsion according to claim 5, wherein in the step (1), the preheating time period is 10-20min, and the heating time period is 20-40 min.
9. The method for determining the oil concentration in an emulsion according to claim 8, wherein in the step (1), the preheating time period is 15min, and the heating time period is 30 min.
10. The method of claim 4, wherein the strength flask comprises a flat bottom flask and a narrow neck; wherein, the thin neck is carved with scale marks.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112305176A (en) * | 2020-12-04 | 2021-02-02 | 中铝东南材料院（福建）科技有限公司 | Method for detecting concentration of emulsion for hot aluminum rolling |
| CN112378944A (en) * | 2020-10-30 | 2021-02-19 | 中铝东南材料院（福建）科技有限公司 | Method for measuring hot separability of hot-rolling emulsion |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102179311A (en) * | 2011-03-16 | 2011-09-14 | 内蒙古包钢稀土林峰科技有限公司 | Anion collecting agent prepared from illegal cooking oil |
| CN103305568A (en) * | 2013-06-28 | 2013-09-18 | 江南大学 | Preparation method of starch nanocrystal ester |
| CN204824442U (en) * | 2015-07-01 | 2015-12-02 | 上海幽岫环保科技有限公司 | A device for giving up emulsion decrement treatment process |
| CN206671298U (en) * | 2017-04-13 | 2017-11-24 | 黄继明 | A kind of measurer for testing oil-water content of emulsion |
| CN108911260A (en) * | 2018-08-09 | 2018-11-30 | 山西太钢不锈钢股份有限公司 | A kind of waste emulsified mixture treatment process |
-
2019
- 2019-11-12 CN CN201911102743.9A patent/CN110763807A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102179311A (en) * | 2011-03-16 | 2011-09-14 | 内蒙古包钢稀土林峰科技有限公司 | Anion collecting agent prepared from illegal cooking oil |
| CN103305568A (en) * | 2013-06-28 | 2013-09-18 | 江南大学 | Preparation method of starch nanocrystal ester |
| CN204824442U (en) * | 2015-07-01 | 2015-12-02 | 上海幽岫环保科技有限公司 | A device for giving up emulsion decrement treatment process |
| CN206671298U (en) * | 2017-04-13 | 2017-11-24 | 黄继明 | A kind of measurer for testing oil-water content of emulsion |
| CN108911260A (en) * | 2018-08-09 | 2018-11-30 | 山西太钢不锈钢股份有限公司 | A kind of waste emulsified mixture treatment process |
Non-Patent Citations (6)
| Title |
|---|
| 师培俭: "冷轧含油和乳化液废水深度处理回用工艺研究", 《工业水处理》 * |
| 张斌: "破乳法检测轧制油乳化液浓度的改进", 《石油商技》 * |
| 张涛 等: "化学破乳-芬顿氧化处理乳化液废水", 《西安工程大学学报》 * |
| 王沛: "《全国中医药行业高等教育"十三五"规划教材 制药工艺学》", 31 August 2017, 中国中医药出版社 * |
| 玻璃计量仪器手册编写组: "《玻璃计量仪器手册》", 31 October 1993, 中国计量出版社 * |
| 罗晓民 等: "《普通高等教育十二五规划教材 皮革理化分析》", 30 September 2013, 中国轻工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112378944A (en) * | 2020-10-30 | 2021-02-19 | 中铝东南材料院（福建）科技有限公司 | Method for measuring hot separability of hot-rolling emulsion |
| CN112305176A (en) * | 2020-12-04 | 2021-02-02 | 中铝东南材料院（福建）科技有限公司 | Method for detecting concentration of emulsion for hot aluminum rolling |
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