CN109876730A - A kind of preparation method of perfluor fluorine carbocyclic ring ether lotion - Google Patents
A kind of preparation method of perfluor fluorine carbocyclic ring ether lotion Download PDFInfo
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- CN109876730A CN109876730A CN201910119163.4A CN201910119163A CN109876730A CN 109876730 A CN109876730 A CN 109876730A CN 201910119163 A CN201910119163 A CN 201910119163A CN 109876730 A CN109876730 A CN 109876730A
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Abstract
The invention discloses a kind of preparation methods of perfluor fluorine carbocyclic ring ether lotion, be by glycerine, perfluor fluorine carbocyclic ring ether and emulsifier mass ratio be 80-99.2:1-19.2:0.8, emulsifier is added in glycerine, 5-10 min is stirred under homogeneous emulsifying machine, revolving speed 10000-20000 r/min, pre-emulsification obtain latex A；Perfluor fluorine carbocyclic ring ether is added in latex A under stiring, stirs 5-10 min in homogeneous blender, revolving speed 10000-20000 r/min obtains lotion to the end.The present invention has stability good, the advantage of storage life length.
Description
Technical field
The present invention relates to a kind of preparation methods of perfluor fluorine carbocyclic ring ether lotion.
Background technique
Perfluoro-cyclicether product is that a kind of colorless and transparent and viscosity is low, nonflammable, volatile, the high liquid of safety.It is main
To be used as cleaning agent, refrigerant, coolant liquid, silicone oil solvent, precise electronic leaks hunting liquid.Plastic electronic production can be cleaned by making cleaning agent
Dust in product production process.The evaporation rate being exceedingly fast can dry alcohol and be impregnated with rear substance, or is dry as desiccant
Substance after being cleaned with aqua type cleaning agent and half aqua type cleaning agent.Various action solvents can be made by making solvent, lubricate dilution agent
Agent etc..
Perfluor fluorine carbocyclic ring ether is as surfactant, with other preparation of reagents at cleaning agent, suitable for the clear of electronic component
It washes, especially there is the cleaning of the electronic component of removing residual glue trace and the printed circuit board of film of flux residue pollution.But it is made
Cleaning agent dissolves in ethyl alcohol, not soluble in water, not can be used as aqueous cleaning agent.Meanwhile perfluor fluorine carbocyclic ring ether may fire, and use
It is dangerous.And perfluor fluorine carbocyclic ring ether is prepared into lotion by the present invention, can be used as aqueous cleaning agent.Aqueous cleaning agent is without sudden strain of a muscle simultaneously
Point will not burn and explode, aqueous cleaning agent waste liquid neutralize after can direct emission it is free from environmental pollution.
Lotion is known in the art and commonly referred to as oil-in-water or water-in-oil emulsion.Lotion usually has limited steady
It is qualitative, i.e., limited storage life or shelf life, and separate or separate after storage for a long period, or show quick drop
Growth or drop size increase.
Summary of the invention
It is good that the invention discloses a kind of stability, the preparation method of the perfluor fluorine carbocyclic ring ether lotion of storage life length.
" lotion " refers to the suspension or dispersion liquid of suspension or the first liquid dispersed in second liquid in the present invention,
Described in the first liquid be indissoluble or unmixing, i.e., it is substantially or entirely unmixing with second liquid.For " substantially ",
Be meant that at least or described two liquid be it is unmixing, the first liquid is referred to as dispersed phase, and second liquid is referred to as continuous
Phase.Dispersed phase can form drop, and the drop is with out-phase or homogeneous mode dispersed throughout continuous phase.The illustrative reality of lotion
Example includes that wherein oil forms dispersed phase, water aqueous solution formation continuous phase, and water-in-oil emulsion wherein water to water aqueous solution packet fat liquor
Dispersed phase is formed, oil forms continuous phase.
A kind of preparation method for preparing perfluor fluorine carbocyclic ring ether lotion of the present invention, includes the following steps:
It is 70-97:28-1:2 by the mass ratio of glycerine, perfluor fluorine carbocyclic ring ether and emulsifier, emulsification is added in glycerine
Agent, stirs 5-10 min, revolving speed 10000-20000 r/min under homogeneous emulsifying machine, and pre-emulsification obtains latex A；It is stirring
It is lower that perfluor fluorine carbocyclic ring ether is added in latex A, 5-10 min, revolving speed 10000-20000 r/ are stirred in homogeneous blender
Min obtains lotion to the end.
Emulsifier as described above is alkyl glycosides (APG), lauryl sodium sulfate (SDS), fatty alcohol polyoxyethylene ether
Sodium sulphate (AES) is one such.
The molecular formula of the perfluor fluorine carbocyclic ring ether is (C8F18)nOr (C8F16O)m 。
The partial size for the lotion that the present invention is prepared is about 100-900 nm.
In the present invention, the emulsifier is AES, and in AES- perfluor fluorine carbocyclic ring ether lotion, the structural formula of AES is as follows:
Wherein n is 2 or 3.
The emulsifier is APG, and in APG- perfluor fluorine carbocyclic ring ether lotion, the structural formula of APG is as follows:
Wherein n is 1-2.
The emulsifier is SDS, and in SDS- perfluor fluorine carbocyclic ring ether lotion, the structural formula of SDS is as follows:。
The method have the benefit that:
1, being stored at room temperature for the lotion prepared is 1 year, can still keep steady in the case where revolving speed is the centrifugal speed of 7000r/min
Fixed, under high temperature (40 DEG C) and (- 15 DEG C) of low temperature processing, which can also keep stable.
2, the lotion prepared by the present invention is dispersed in water, so that perfluor fluorine carbocyclic ring ether can be used as water-soluble cleaning
Agent.Aqueous cleaning agent will not burn and explode without flash-point, aqueous cleaning agent waste liquid neutralize after can direct emission it is free from environmental pollution.
Specific embodiment
In order to better understand the technical means of the present invention, it and can be implemented in accordance with the contents of the specification, below
In conjunction with specific embodiments, specific embodiments of the present invention will be described in further detail, and following embodiment is for illustrating this hair
It is bright, but be not intended to limit the scope of the invention.
Embodiment 1
Glycerine, perfluor fluorine carbocyclic ring ether (C8F18)nMass ratio with AES is 78:20:2.0.6g AES is dissolved in 23.4g the third three
In alcohol, 5min is stirred under Yu Junzhi blender, 13000 r/min of mixing speed is sufficiently stirred to obtain latex A.Later in homogeneous
Under the stirring of blender, by 6g perfluor fluorine carbocyclic ring ether (C8F18)nIt is slowly added into latex A, starts timing after adding, stir
5min, 13000 r/min of revolving speed.Defoaming is stood later, tests its stability.Storage time is up to 1 year at normal temperature for it,
Being centrifuged under 7000 r/min can still keep stable, can also keep stable after for 24 hours in thermmal storage (40 DEG C) and cold storage (- 15 DEG C).
Take it is one after another drop of enter water (about 100ml) in, stirring is completely soluble in water and is not layered, it is water-soluble very well.Through laser particle size analyzer
Test, particle size range 100-900nm.
Embodiment 2
Glycerine, perfluor fluorine carbocyclic ring ether (C8F16O)mMass ratio with APG is 70:28:2.0.6g APG is dissolved in 21g glycerine
In, 6min is stirred under Yu Junzhi blender, 10000 r/min of mixing speed is sufficiently stirred to obtain latex A.It is stirred later in homogeneous
Under the stirring for mixing machine, by 8.4g perfluor fluorine carbocyclic ring ether (C8F16O)mIt is slowly added into latex A, starts timing after adding, stir
6min, 10000 r/min of revolving speed.Defoaming is stood later, tests its stability.Storage time is up to 1 year at normal temperature for it,
Being centrifuged under 7000 r/min can still keep stable, can also keep stable after for 24 hours in thermmal storage (40 DEG C) and cold storage (- 15 DEG C).
Take it is one after another drop of enter water (about 100ml) in, stirring is completely soluble in water and is not layered, it is water-soluble very well.Through laser particle size analyzer
Test, particle size range 100-900nm.
Embodiment 3
Glycerine, perfluor fluorine carbocyclic ring ether (C8F18)nMass ratio with SDS is 97:1:2.0.60g SDS is dissolved in 29.1g the third three
In alcohol, 7min is stirred under Yu Junzhi blender, 15000 r/min of mixing speed is sufficiently stirred to obtain latex A.Later in homogeneous
Under the stirring of blender, by 0.3g perfluor fluorine carbocyclic ring ether (C8F18)nIt is slowly added into latex A, starts timing after adding, stir
5min, 15000 r/min of revolving speed.Defoaming is stood later, tests its stability.Storage time is up to 1 year at normal temperature for it,
Being centrifuged under 7000 r/min can still keep stable, can also keep stable after for 24 hours in thermmal storage (40 DEG C) and cold storage (- 15 DEG C).
Take it is one after another drop of enter water (about 100ml) in, stirring is completely soluble in water and is not layered, it is water-soluble very well.Through laser particle size analyzer
Test, particle size range 100-900nm.
Embodiment 4
Glycerine, perfluor fluorine carbocyclic ring ether (C8F16O)mMass ratio with AES is 88:10:2.0.8g AES is dissolved in 35.2g the third three
In alcohol, 5min is stirred under Yu Junzhi blender, 17000 r/min of mixing speed is sufficiently stirred to obtain latex A.Later in homogeneous
Under the stirring of blender, by 4g perfluor fluorine carbocyclic ring ether (C8F16O)mIt is slowly added into latex A, starts timing after adding, stir
8min, 17000 r/min of revolving speed.Defoaming is stood later, tests its stability.Storage time is up to 1 year at normal temperature for it,
Being centrifuged under 7000 r/min can still keep stable, can also keep stable after for 24 hours in thermmal storage (40 DEG C) and cold storage (- 15 DEG C).
Take it is one after another drop of enter water (about 100ml) in, stirring is completely soluble in water and is not layered, it is water-soluble very well.Through laser particle size analyzer
Test, particle size range 100-900nm.
Embodiment 5
Glycerine, perfluor fluorine carbocyclic ring ether (C8F16O)mMass ratio with APG is 78:20:2.0.8g APG is dissolved in 31.9g the third three
In alcohol, 10min is stirred under Yu Junzhi blender, 19000 r/min of mixing speed is sufficiently stirred to obtain latex A.Later in homogeneous
Under the stirring of blender, by 8g perfluor fluorine carbocyclic ring ether (C8F16O)mIt is slowly added into latex A, starts timing after adding, stir
5min, 19000 r/min of revolving speed.Defoaming is stood later, tests its stability.Storage time is up to 1 year at normal temperature for it,
Being centrifuged under 7000 r/min can still keep stable, can also keep stable after for 24 hours in thermmal storage (40 DEG C) and cold storage (- 15 DEG C).
Take it is one after another drop of enter water (about 100ml) in, stirring is completely soluble in water and is not layered, it is water-soluble very well.Through laser particle size analyzer
Test, particle size range 100-900nm.
Embodiment 6
Glycerine, perfluor fluorine carbocyclic ring ether (C8F18)nMass ratio with SDS is 76:22:2.0.80g SDS is dissolved in 30.4g the third three
In alcohol, 5min is stirred under Yu Junzhi blender, 20000 r/min of mixing speed is sufficiently stirred to obtain latex A.Later in homogeneous
Under the stirring of blender, by 8.8g perfluor fluorine carbocyclic ring ether (C8F18)nIt is slowly added into latex A, starts timing after adding, stir
8min, 20000 r/min of revolving speed.Defoaming is stood later, tests its stability.Storage time is up to 1 year at normal temperature for it,
Being centrifuged under 7000 r/min can still keep stable, can also keep stable after for 24 hours in thermmal storage (40 DEG C) and cold storage (- 15 DEG C).
Take it is one after another drop of enter water (about 100ml) in, stirring is completely soluble in water and is not layered, it is water-soluble very well.Through laser particle size analyzer
Test, particle size range 100-900nm.
Embodiment 7
Glycerine, perfluor fluorine carbocyclic ring ether (C8F16O)mMass ratio with AES is 88:10:2.0.6g AES is dissolved in 26.4g the third three
In alcohol, 5min is stirred under Yu Junzhi blender, 13000 r/min of mixing speed is sufficiently stirred to obtain latex A.Later in homogeneous
Under the stirring of blender, by 3g perfluor fluorine carbocyclic ring ether (C8F16O)mIt is slowly added into latex A, starts timing after adding, stir
5min, 13000 r/min of revolving speed.Defoaming is stood later, tests its stability.Storage time is up to 1 year at normal temperature for it,
Being centrifuged under 7000 r/min can still keep stable, can also keep stable after for 24 hours in thermmal storage (40 DEG C) and cold storage (- 15 DEG C).
Take it is one after another drop of enter water (about 100ml) in, stirring is completely soluble in water and is not layered, it is water-soluble very well.Through laser particle size analyzer
Test, particle size range 100-900nm.
Embodiment 8
Glycerine, perfluor fluorine carbocyclic ring ether (C8F18)nMass ratio with APG is 88:10:2.0.6g APG is dissolved in 26.4g the third three
In alcohol, 9min is stirred under Yu Junzhi blender, 13000 r/min of mixing speed is sufficiently stirred to obtain latex A.Later in homogeneous
Under the stirring of blender, by 3g perfluor fluorine carbocyclic ring ether (C8F18)nIt is slowly added into latex A, starts timing after adding, stir
8min, 13000 r/min of revolving speed.Defoaming is stood later, tests its stability.Storage time is up to 1 year at normal temperature for it,
Being centrifuged under 7000 r/min can still keep stable, can also keep stable after for 24 hours in thermmal storage (40 DEG C) and cold storage (- 15 DEG C).
Take it is one after another drop of enter water (about 100ml) in, stirring is completely soluble in water and is not layered, it is water-soluble very well.Through laser particle size analyzer
Test, particle size range 100-900nm.
Embodiment 9
Glycerine, perfluor fluorine carbocyclic ring ether (C8F18)nMass ratio with SDS is 88:10:2.0.60g SDS is dissolved in 26.40g third
In triol, 5min is stirred under Yu Junzhi blender, 13000 r/min of mixing speed is sufficiently stirred to obtain latex A.Later equal
Under the stirring of matter blender, by 3g perfluor fluorine carbocyclic ring ether (C8F18)nIt is slowly added into latex A, starts timing after adding, stir
5min, 13000 r/min of revolving speed.Defoaming is stood later, tests its stability.Storage time is up to 1 year at normal temperature for it,
Being centrifuged under 7000 r/min can still keep stable, can also keep stable after for 24 hours in thermmal storage (40 DEG C) and cold storage (- 15 DEG C).
Take it is one after another drop of enter water (about 100ml) in, stirring is completely soluble in water and is not layered, it is water-soluble very well.Through laser particle size analyzer
Test, particle size range 100-900nm.
The median particle diameter contrast table of three kinds of lotions
In table is to use median particle diameter contrast table measured by the lotion of the preparation of example 1,2 and 3, and general trend is to increase.From
It sees in appearance, lotion can still keep emulsus, not be layered after the preservation up to 1 year.
Prepared lotion can the good dispersion in water, have water solubility, can be used as aqueous cleaning agent.
Claims (7)
1. a kind of preparation method of perfluor fluorine carbocyclic ring ether lotion, it is characterised in that include the following steps:
It is 80-99.2:1-19.2:0.8 by the mass ratio of glycerine, perfluor fluorine carbocyclic ring ether and emulsifier, adds in glycerine
Enter emulsifier, 5-10 min, revolving speed 10000-20000 r/min are stirred under homogeneous emulsifying machine, pre-emulsification obtains latex A；
Perfluor fluorine carbocyclic ring ether is added in latex A under stiring, stirs 5-10 min, revolving speed 10000- in homogeneous blender
20000 r/min obtain lotion to the end.
2. a kind of preparation method of perfluor fluorine carbocyclic ring ether lotion as described in claim 1, it is characterised in that the emulsifier
It is one such for alkyl glycosides APG, lauryl sodium sulfate SDS, sodium sulfate of polyethenoxy ether of fatty alcohol AES.
3. a kind of preparation method of perfluor fluorine carbocyclic ring ether lotion as described in claim 1, it is characterised in that the perfluor fluorine carbon
The molecular formula of cyclic ethers is (C8F18)nOr (C8F16O)m 。
4. such as the perfluor fluorine carbocyclic ring ether lotion of any one of claim 1-3 the method preparation, it is characterised in that the partial size of lotion
For 100-900 nm.
5. perfluor fluorine carbocyclic ring ether lotion as claimed in claim 4, it is characterised in that the structural formula of emulsifier AES, AES are such as
Under:
Wherein n is 2 or 3.
6. perfluor fluorine carbocyclic ring ether lotion as claimed in claim 4, it is characterised in that the structural formula of emulsifier APG, APG are such as
Under:
Wherein n is 1-2.
7. perfluor fluorine carbocyclic ring ether lotion as claimed in claim 4, it is characterised in that the structural formula of emulsifier SDS, SDS are such as
Under:
。
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| KR20180030357A (en) * | 2016-09-13 | 2018-03-22 | 한국콜마주식회사 | Skin cleansing composition ejected with sherbet-like state and article for skin creansing comprising the same |
| CN109536009A (en) * | 2018-11-20 | 2019-03-29 | 萍乡亨厚新材科技有限公司 | A kind of car surface maintenance hydrophobic latex and preparation method thereof |
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2019
- 2019-02-18 CN CN201910119163.4A patent/CN109876730B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN102406945A (en) * | 2011-10-24 | 2012-04-11 | 上海纳米技术及应用国家工程研究中心有限公司 | Fluorocarbon and cyclodextrin inclusion compound and preparation method thereof |
| 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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