CN109876730B - Preparation method of perfluorofluorocarbon cyclic ether emulsion - Google Patents
Preparation method of perfluorofluorocarbon cyclic ether emulsion Download PDFInfo
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Abstract
The invention discloses a preparation method of a perfluoro fluorocarbon cyclic ether emulsion, which comprises the following steps of mixing glycerol, perfluoro fluorocarbon cyclic ether and an emulsifier according to the mass ratio of 80-99.2: 1-19.2: 0.8, adding an emulsifier into glycerol, stirring for 5-10 min under a homogenizing emulsifying machine at the rotation speed of 10000-; adding the perfluor fluorocarbon cyclic ether into the emulsion A under stirring, and stirring for 5-10 min in a homogenizing stirrer at the rotation speed of 10000-. The invention has the advantages of good stability and long storage life.
Description
Technical Field
The invention relates to a preparation method of a perfluoro fluorocarbon cyclic ether emulsion.
Background
The perfluoro cyclic ether product is a colorless and transparent liquid with low viscosity, nonflammability, volatility and extremely high safety. The high-performance liquid lubricant is mainly used as a cleaning agent, a refrigerant, a cooling liquid, a silicone oil solvent and a precise electronic leakage detection liquid. The cleaning agent can be used for cleaning dust in the production process of plastic electronic products. The very fast volatilization rate can be used as a drying agent, and can dry the substances soaked in alcohol or the substances cleaned by water-based cleaning agents and semi-water-based cleaning agents. The solvent can be used as various reaction solvents, lubricant diluents and the like.
The perfluor fluorocarbon cyclic ether is used as a surfactant, is prepared into a cleaning agent with other reagents, and is suitable for cleaning electronic elements, in particular to the cleaning of the electronic elements with residual glue marks and printed circuit boards polluted by scaling powder residues. But the prepared cleaning agent can be dissolved in ethanol, but is not dissolved in water, and cannot be used as a water-based cleaning agent. Meanwhile, the perfluor fluorocarbon cyclic ether is possible to explode and is unsafe to use. The invention prepares the perfluor fluorocarbon cyclic ether into emulsion which can be used as a water-based cleaning agent. Meanwhile, the water-based cleaning agent has no flash point, can not be burnt or exploded, and can be directly discharged after the waste liquid of the water-based cleaning agent is neutralized without polluting the environment.
Emulsions are known in the art and are commonly referred to as oil-in-water or water-in-oil emulsions. Emulsions generally have limited stability, i.e., limited shelf life or shelf life, and separate or separate after long storage, or exhibit rapid droplet growth or droplet size increase.
Disclosure of Invention
The invention discloses a preparation method of a perfluoro fluorocarbon cyclic ether emulsion with good stability and long storage life.
An "emulsion" in the present invention refers to a suspension or dispersion of a first liquid suspended or dispersed in a second liquid, wherein the first liquid is poorly soluble or immiscible, i.e., substantially or completely immiscible, with the second liquid. By "substantially" it is meant that at least, or the two liquids are immiscible, the first liquid is referred to as the dispersed phase and the second liquid is referred to as the continuous phase. The dispersed phase may form droplets that are dispersed throughout the continuous phase in a heterogeneous or homogeneous manner. Illustrative examples of emulsions include oil-in-water emulsions where the oil forms the dispersed phase, aqueous solutions form the continuous phase, and water-in-oil emulsions where the water forms the dispersed phase and the oil forms the continuous phase.
The invention relates to a preparation method of perfluorofluorocarbon cyclic ether emulsion, which comprises the following steps:
according to the mass ratio of the glycerol to the perfluoro fluorocarbon cyclic ether to the emulsifier of 70-97: 28-1: 2, adding an emulsifier into glycerol, stirring for 5-10 min under a homogenizing emulsifying machine at the rotation speed of 10000-; adding the perfluor fluorocarbon cyclic ether into the emulsion A under stirring, and stirring for 5-10 min in a homogenizing stirrer at the rotation speed of 10000-.
The emulsifier is one of alkyl glycoside (APG), Sodium Dodecyl Sulfate (SDS) and sodium fatty alcohol polyoxyethylene ether sulfate (AES).
The molecular formula of the perfluor fluorocarbon cyclic ether is (C)8F18)nOr (C)8F16O)m 。
The particle size of the emulsion prepared by the invention is about 100-900 nm.
In the invention, the emulsifier is AES, and in AES-perfluorofluorocarbon cyclic ether emulsion, the AES has the following structural formula:
wherein n is 2 or 3.
The emulsifier is APG, and in the APG-perfluorofluorocarbon cyclic ether emulsion, the APG has the following structural formula:
wherein n is 1-2.
The emulsifier is SDS, and in the SDS-perfluoro fluorocarbon cyclic ether emulsion, the structural formula of the SDS is as follows:
the beneficial technical effects of the invention are as follows:
1. the prepared emulsion can be stored at normal temperature for 1 year, can still keep stable at the centrifugal speed of 7000r/min, and can also keep stable under the treatment of high temperature (40 ℃) and low temperature (-15 ℃).
2. The emulsion prepared by the invention can be dispersed in water, so that the perfluor fluorocarbon cyclic ether can be used as a water-soluble cleaning agent. The water-based cleaning agent has no flash point, can not be burnt and exploded, and can be directly discharged after the waste liquid of the water-based cleaning agent is neutralized without polluting the environment.
Detailed Description
In order to clearly understand the technical means of the present invention and to implement the technical means according to the content of the specification, the following embodiments are further described in detail in the following with reference to the specific examples, which are used for illustrating the present invention and are not intended to limit the scope of the present invention.
Example 1
Glycerol, perfluoro fluorocarbon cyclic ether (C)8F18)nMass ratio to AES was 78: 20: 2. 0.6g of AES was dissolved in 23.4g of glycerin, and stirred in a homomixer at 13000 r/min for 5min, followed by sufficient stirring to obtain emulsion A. Then, under stirring in a homogenizer, 6g of perfluorofluorocarbon cyclic ether (C)8F18)nSlowly adding the mixture into the emulsion A, timing after the addition is finished, stirring for 5min, and rotating speed of 13000 r/min. And then standing for defoaming, and testing the stability of the product. The product can be stored at room temperature for 1 year, can be kept stable even after centrifugation at 7000r/min, and can be kept stable even after hot storage (40 ℃) and cold storage (-15 ℃) for 24 hours. One drop is taken and dropped into water (about 100 ml), and the mixture is stirred, can be completely dissolved in the water without layering, and has good water solubility. The particle size range is 100-900 nm through the test of a laser particle size analyzer.
Example 2
Glycerol, perfluoro fluorocarbon cyclic ether (C)8F16O)mThe mass ratio to APG was 70: 28: 2. dissolving 0.6g of APG in 21g of glycerol, stirring for 6min under a homogenizing stirrer at the stirring speed of 10000 r/min, and fully stirring to obtain emulsion A. Then, 8.4g of perfluorofluorocarbon cyclic ether (C) was added under stirring in a homomixer8F16O)mSlowly adding into emulsion A, timing after adding, stirring for 6min, and rotating speed 10000 r/min. And then standing for defoaming, and testing the stability of the product. The product can be stored at room temperature for 1 year, can be kept stable even after centrifugation at 7000r/min, and can be kept stable even after hot storage (40 ℃) and cold storage (-15 ℃) for 24 hours. One drop is taken and dropped into water (about 100 ml), and the mixture is stirred, can be completely dissolved in the water without layering, and has good water solubility. The particle size range is 100-900 nm through the test of a laser particle size analyzer.
Example 3
Glycerol, perfluoro fluorocarbon cyclic ether (C)8F18)nMass ratio to SDS was 97: 1: 2. 0.60g of SDS was dissolved in 29.1g of glycerol, and the mixture was stirred in a homomixer at a stirring speed of 15000 r/min for 7min and sufficiently stirred to obtain emulsion A. Then, 0.3g of perfluorofluorocarbon cyclic ether (C) was added under stirring in a homogenizer8F18)nSlowly adding into the emulsion A, timing after adding, stirring for 5min, and rotating speed of 15000 r/min. And then standing for defoaming, and testing the stability of the product. The product can be stored at room temperature for 1 year, can be kept stable even after centrifugation at 7000r/min, and can be kept stable even after hot storage (40 ℃) and cold storage (-15 ℃) for 24 hours. One drop is taken and dropped into water (about 100 ml), and the mixture is stirred, can be completely dissolved in the water without layering, and has good water solubility. The particle size range is 100-900 nm through the test of a laser particle size analyzer.
Example 4
Glycerol, perfluoro fluorocarbon cyclic ether (C)8F16O)mMass ratio to AES was 88: 10: 2. 0.8g of AES was dissolved in 35.2g of glycerol, and stirred in a homomixer at a stirring speed of 17000 r/min for 5min, followed by sufficient stirring to obtain emulsion A. Then, 4g of perfluorofluorocarbon cyclic ether (C) was added under stirring in a homomixer8F16O)mSlowly adding into the emulsion A, timing after adding, stirring for 8min, and rotating at 17000 r/min. And then standing for defoaming, and testing the stability of the product. The product can be stored at room temperature for 1 year, can be kept stable even after centrifugation at 7000r/min, and can be kept stable even after hot storage (40 ℃) and cold storage (-15 ℃) for 24 hours. One drop is taken and dropped into water (about 100 ml), and the mixture is stirred, can be completely dissolved in the water without layering, and has good water solubility. The particle size range is 100-900 nm through the test of a laser particle size analyzer.
Example 5
Glycerol, perfluoro fluorocarbon cyclic ether (C)8F16O)mMass ratio to APG 78: 20: 2. dissolving 0.8g of APG in 31.9g of glycerol, stirring for 10min under a homogenizing stirrer at a stirring speed of 19000 r/min, and fully stirring to obtain emulsion A. Then, 8g of perfluorofluorocarbon cyclic ether (C) was added under stirring in a homogenizer8F16O)mSlowly adding the mixture into the emulsion A, timing after the addition is finished, stirring for 5min, and rotating speed of 19000 r/min. And then standing for defoaming, and testing the stability of the product. The product can be stored at room temperature for 1 year, can be kept stable even after centrifugation at 7000r/min, and can be kept stable even after hot storage (40 ℃) and cold storage (-15 ℃) for 24 hours. Take one drop and drip into water (about 100)ml) can be completely dissolved in water without layering by stirring, and has good water solubility. The particle size range is 100-900 nm through the test of a laser particle size analyzer.
Example 6
Glycerol, perfluoro fluorocarbon cyclic ether (C)8F18)nMass ratio to SDS 76: 22: 2. dissolving 0.80g SDS in 30.4g glycerol, stirring for 5min under homogenizing mixer at 20000 r/min, and stirring thoroughly to obtain emulsion A. Then, 8.8g of perfluorofluorocarbon cyclic ether (C) was added under stirring in a homogenizer8F18)nSlowly adding into emulsion A, timing after adding, stirring for 8min at rotation speed of 20000 r/min. And then standing for defoaming, and testing the stability of the product. The product can be stored at room temperature for 1 year, can be kept stable even after centrifugation at 7000r/min, and can be kept stable even after hot storage (40 ℃) and cold storage (-15 ℃) for 24 hours. One drop is taken and dropped into water (about 100 ml), and the mixture is stirred, can be completely dissolved in the water without layering, and has good water solubility. The particle size range is 100-900 nm through the test of a laser particle size analyzer.
Example 7
Glycerol, perfluoro fluorocarbon cyclic ether (C)8F16O)mMass ratio to AES was 88: 10: 2. 0.6g of AES was dissolved in 26.4g of glycerin, and stirred in a homomixer at 13000 r/min for 5min, followed by sufficient stirring to obtain emulsion A. Then, 3g of perfluorofluorocarbon cyclic ether (C) was added under stirring in a homomixer8F16O)mSlowly adding the mixture into the emulsion A, timing after the addition is finished, stirring for 5min, and rotating speed of 13000 r/min. And then standing for defoaming, and testing the stability of the product. The product can be stored at room temperature for 1 year, can be kept stable even after centrifugation at 7000r/min, and can be kept stable even after hot storage (40 ℃) and cold storage (-15 ℃) for 24 hours. One drop is taken and dropped into water (about 100 ml), and the mixture is stirred, can be completely dissolved in the water without layering, and has good water solubility. The particle size range is 100-900 nm through the test of a laser particle size analyzer.
Example 8
Glycerol, perfluoro fluorocarbon cyclic ether (C)8F18)nThe mass ratio of APG to APG is 88: 10: 2. 0.6gDissolving APG in 26.4g glycerol, stirring for 9min with a homogenizing mixer at 13000 r/min, and stirring thoroughly to obtain emulsion A. Then, 3g of perfluorofluorocarbon cyclic ether (C) was added under stirring in a homomixer8F18)nSlowly adding the mixture into the emulsion A, timing after the addition is finished, stirring for 8min, and rotating speed of 13000 r/min. And then standing for defoaming, and testing the stability of the product. The product can be stored at room temperature for 1 year, can be kept stable even after centrifugation at 7000r/min, and can be kept stable even after hot storage (40 ℃) and cold storage (-15 ℃) for 24 hours. One drop is taken and dropped into water (about 100 ml), and the mixture is stirred, can be completely dissolved in the water without layering, and has good water solubility. The particle size range is 100-900 nm through the test of a laser particle size analyzer.
Example 9
Glycerol, perfluoro fluorocarbon cyclic ether (C)8F18)nThe mass ratio to SDS was 88: 10: 2. 0.60g of SDS was dissolved in 26.40g of glycerol, and the mixture was stirred in a homomixer at 13000 r/min for 5min and sufficiently stirred to give emulsion A. Then, 3g of perfluorofluorocarbon cyclic ether (C) was added under stirring in a homomixer8F18)nSlowly adding the mixture into the emulsion A, timing after the addition is finished, stirring for 5min, and rotating speed of 13000 r/min. And then standing for defoaming, and testing the stability of the product. The product can be stored at room temperature for 1 year, can be kept stable even after centrifugation at 7000r/min, and can be kept stable even after hot storage (40 ℃) and cold storage (-15 ℃) for 24 hours. One drop is taken and dropped into water (about 100 ml), and the mixture is stirred, can be completely dissolved in the water without layering, and has good water solubility. The particle size range is 100-900 nm through the test of a laser particle size analyzer.
Comparison table of median particle diameters of three emulsions
The median particle size measured for the emulsions prepared in examples 1, 2 and 3 is shown in the table, with the general trend being greater. In appearance, the emulsion remained milky and did not delaminate after storage for up to one year.
The prepared emulsion can be well dispersed in water, has water solubility and can be used as a water-based cleaning agent.
Claims (6)
1. A preparation method of perfluorofluorocarbon cyclic ether emulsion is characterized by comprising the following steps:
according to the mass ratio of the glycerol to the perfluoro fluorocarbon cyclic ether to the emulsifier of 80-99.2: 1-19.2: 0.8, adding an emulsifier into glycerol, stirring for 5-10 min under a homogenizing emulsifying machine at the rotation speed of 10000-; adding the perfluor fluorocarbon cyclic ether into the emulsion A under stirring, stirring for 5-10 min in a homogenizing stirrer at the rotation speed of 10000-; the molecular formula of the perfluor fluorocarbon cyclic ether is (C)8F18)n▪(C8F16O)m 。
2. The method of claim 1, wherein the emulsifier is one of alkyl glycoside APG, Sodium Dodecyl Sulfate (SDS), and sodium Alcohol Ether Sulfate (AES).
3. The perfluorofluorocarbon cyclic ether emulsion prepared by the process as set forth in any one of claims 1 to 2, characterized in that the particle size of the emulsion is 100-900 nm.
4. A perfluorocarbon cyclic ether emulsion as claimed in claim 3, wherein the emulsifier is AES having the formula:
wherein n is 2 or 3.
5. A perfluorofluorocarbon cyclic ether emulsion according to claim 3, wherein the emulsifier is APG, the APG having the formula:
wherein n is 1-2.
6. The perfluorofluorocarbon cyclic ether emulsion according to claim 3, wherein the emulsifier is SDS having the formula:
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Patent Citations (6)
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| CN101274969A (en) * | 2007-11-20 | 2008-10-01 | 山东东岳神舟新材料有限公司 | Microemulsion polymerization method for fluoropolymer |
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| CN105018195A (en) * | 2015-06-23 | 2015-11-04 | 东莞市佳丹润滑油有限公司 | Special lubricant for plastic part assembly, and preparation method thereof |
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