CN107176737A - The method that fluorine carbon solvent is extracted from perfluoro caprylic acid electrolysis by-products - Google Patents
The method that fluorine carbon solvent is extracted from perfluoro caprylic acid electrolysis by-products Download PDFInfo
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- CN107176737A CN107176737A CN201610136814.7A CN201610136814A CN107176737A CN 107176737 A CN107176737 A CN 107176737A CN 201610136814 A CN201610136814 A CN 201610136814A CN 107176737 A CN107176737 A CN 107176737A
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- Prior art keywords
- solvent
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- fluorine carbon
- caprylic acid
- perfluoro caprylic
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
Abstract
The present invention relates to a kind of method that fluorine carbon solvent is extracted in electrolysis by-products from perfluoro caprylic acid, electrolysis by-products fluorine carbon mix produced by this method is engineered in process units production process using perfluoro caprylic acid is used as raw material, utilize the physical separation methods such as alkaline hydrolysis, washing, drying, distillation and filtering, separating-purifying is carried out to electrolysis by-products, extract fluorine carbon solvent, the commercialization of perfluoro caprylic acid electrolysis by-products is realized, perfluoro caprylic acid production cost is reduced, utilization of resources value is improved.This method is applied to production process, simple with technique, it is easy to control, the stable advantage of product quality.
Description
Technical field
Carried the present invention relates to technical field of chemistry, more particularly to from perfluoro caprylic acid electrolysis by-products
The method for taking fluorine carbon solvent.
Background technology
The characteristics of high-quality fluorine carbon solvent has high stability, solvability is strong, it is extensive
Applied to precise electronic, instrument, equipment, highly dense huge capacity compact discs, mobile communication instrument etc.
Cleaning-drying field, with wide market prospects.
Fluorine carbon solvent is a kind of electrolysis by-products produced in perfluoro caprylic acid production process, work
Using caprylyl chloride and hydrogen fluoride electrolysis production perfluoro caprylic acid in industry, but the normal companion in electrolytic process
With some side reactions, its accessory substance produced is mainly perfluor ether epoxy, PF 5070 etc.,
Wherein key reaction mechanism is as follows：
Main reaction：
(1) electrowinning process
2HF→H2+F2
(2) fluorination reaction
C7H15COCl+15F2→C7F15COF+14HF+HCl
(3) neutralization reaction
C7F15COF+2NaOH→C7F15COONa+NaF+H2O
NaOH+HF→NaF+H2O
(4) acidification reaction
C7F15COONa+H2SO4→C7F15COOH+Na2SO4
Side reaction：
(1) electrolysis cyclisation generation perfluor 2- normal-butyl tetrahydrofurans
(2) cyclic ethers of electrolysis cyclisation generation perfluor 2- n-propyls penta
(3) in the presence of a small amount of water, fluorination decarboxylation produces PF 5070 to caprylyl chloride
C7H15COCl+H2O+16F2→C7F16+CO2+HCl+16HF
After electrolysis terminates, generally carried using methods such as acidifying, alkali cleaning, extractions from electrolyte
Perfluoro caprylic acid product is taken, remaining accessory substance is often fallen as " three wastes " by burning disposal, provided
Source value is not high.But, in recent years, with environmental protection consciousness continuous enhancing and
Shortage of resources is highlighted, and people start to pay attention to and carry out perfluoro caprylic acid electrolysis by-products fluorine carbon mix
Separation and purification work, at present, the whole nation production perfluoro caprylic acid producer it is mainly that fluorine carbon crude product is straight
Connect and sold as fluorine carbon solvent, or by being used as product pin after simply washing and distilling
Sell, due to there are a large amount of impurity, it is impossible to be used in precise electronic, instrument, equipment, highly dense great Rong
Measure CD, the cleaning of mobile communication instrument, can only certain applications in general cleaning and solvent occasion,
Limit the use field of fluorine carbon solvent.
At present, it there is no the open report of the fine method of purification of fluorine carbon solvent.
The content of the invention
The perfluoro caprylic acid electrolysis by-products profit that the purpose of the present invention exists aiming at prior art
It is not high with rate, halfway defect is purified there is provided a kind of method of separating-purifying, to background skill
What the perfluoro caprylic acid industrialized preparing process that art part is referred to was produced contains perfluor -2- normal-butyls four
The fluorine carbon mixing of hydrogen furans, the cyclic ethers of perfluor -2- n-propyls penta, PF 5070 and a small amount of moisture etc.
Thing (perfluoro caprylic acid electrolysis by-products) carries out separating-purifying processing, the fluorine that this method processing is obtained
Carbon solvent purity height, quality better, resource utilization are high.
One of technical scheme is：Fluorine carbon is extracted from perfluoro caprylic acid electrolysis by-products
The method of solvent, comprises the following steps：
(1) alkaline hydrolysis：Alkaline matter is added into perfluoro caprylic acid electrolysis by-products, alkaline hydrolysis is carried out
Reaction；
(2) wash and dry：Basic fluxing raction liquid is washed to water layer pH most 7-8, thick fluorine carbon is obtained
Plain solvent, dries the moisture removed in the thick fluorocarbon solvent；
(3) distill：Dried thick fluorocarbon solvent is distilled, and takes 85-102 DEG C of temperature range
Cut produce.
The present invention carries out Basic fluxing raction to perfluoro caprylic acid electrolysis by-products first, and Basic fluxing raction can
Remove electrolysis by-products in acidic materials, wherein, the alkaline matter may be selected from organic base or
Inorganic base, inorganic base may be selected from one kind or several in sodium hydroxide, calcium hydroxide, potassium hydroxide
Kind, organic base may be selected from the one or more in potassium tert-butoxide, sodium tert-butoxide, and the present invention is preferably
Using organic base, alkaline hydrolysis material is further preferably used as using potassium tert-butoxide.The alkaline matter
Addition be perfluoro caprylic acid electrolysis by-products weight 1-5%, with using compared with inorganic base,
It is more beneficial for ensuring using organic base when carrying out Basic fluxing raction to perfluoro caprylic acid electrolysis by-products
The abundant progress of neutralization reaction, so that it is guaranteed that the quality of finished product.
Preferably, it is pungent that the aqueous solution for the alkaline matter being configured into concentration 5-40% adds perfluor
In sour electrolysis by-products, the concentration is preferably 10-20%.
It is further preferred that the condition of the Basic fluxing raction is：20-50 DEG C of temperature, during reaction
Between 1-5h；More preferably：30-40 DEG C of temperature, reaction time 3-4h.
The Basic fluxing raction is preferably carried out under agitation.
After alkaline hydrolysis, the water-soluble substances produced during alkaline hydrolysis is removed by washing, further
Remove the impurity in solvent.Washing can be carried out using industry water, deionized water or distilled water, excellent
Elect deionized water as.Deionized water addition is preferably 1-2 times of Basic fluxing raction liquid weight.Water
Number of times is washed to be generally 3-8 times.
Using the moisture in molecular sieve or the activated carbon removing thick fluorocarbon solvent after washing, preferably
Using molecular sieve, the consumption of further preferred molecular sieve is the thick fluorocarbon solvent weight
10-20%.In addition, solvent, which is handled, using molecular sieve or activated carbon also has what is decolourized
Effect, can further provide for the quality of solvent.
Solvent is further purified using distillation means after washing, the distillation can be in atmospheric conditions
Progress can also be carried out at reduced pressure conditions, and present invention preferably employs air-distillation mode, normal pressure essence
The purification of solvent can successfully be realized by evaporating, and energy consumption is small.
Preferably, the reflux ratio of distillation is (1.5-2.5)：1, more preferably 2:1.
In order to further improve the quality of finished product, after the method for the invention also includes to distillation
Product the step of filtered, filtering can further remove the suspension and machinery in solvent
Impurity.
Preferably, the filtering is using in alkaline carclazyte, Emathlite, diatomite, kaolin
One or more be used as filter medium, more preferably diatomite.
Preferably, the consumption of filter medium is the 5-20% of products weight, more preferably
5-10%.
Preferably, described to be filtered into pressure filtration, filter pressure is 1-4kgf/cm2, further
Preferably 1.5-2.5kgf/cm2。
The suspension and mechanical admixture in solvent can be ideally removed using above-mentioned condition so that
Solvent is more clarified, and quality is more preferable.
The two of technical scheme are：A kind of fluorine carbon solvent, the fluorine carbon solvent is
Prepared by any one above-mentioned method.
Preferably, the fluorine carbon solvent includes perfluor -2- normal-butyls tetrahydrofuran, perfluor -2-
The cyclic ethers of n-propyl penta, PF 5070 component.
It is further preferred that the boiling range (101.3Kpa) of the fluorine carbon solvent is 85-102 DEG C,
Moisture≤50PPm, pH value 7-7.5.
On the basis of common sense in the field is met, above-mentioned each optimum condition can be mutually combined,
Produce each preferred embodiment of the invention.
By above-mentioned processing, it is miscellaneous that the fluorine carbon solvent prepared does not contain acidic materials, machinery
Matter and moisture, product purity are high, and quality is high, and stability is good, can be used in precise electronic, sets
Standby, instrument, highly dense huge capacity compact discs, the cleaning-drying for collecting communication tool etc., with wide
Market prospects.
Embodiment
Following examples are used to illustrate the present invention, but are not limited to the scope of the present invention.Implement
The reagent or material being related in example are commercially available to be obtained, and the operation being related to is unless otherwise specified
It is this area routine operation.The percentage composition being related in the present invention is unless otherwise specified
Weight/mass percentage composition.The perfluoro caprylic acid electrolysis by-products being related in embodiment are by such as lower section
What method was obtained：Using caprylyl chloride and hydrogen fluoride as raw material, electrolysis produces perfluoro caprylic acid, and electrolysis terminates
Afterwards, perfluoro caprylic acid product is extracted from electrolyte using acidifying, alkali cleaning, extracting process, it is remaining
Liquid be perfluoro caprylic acid electrolysis by-products, mainly contain perfluor -2- normal-butyl tetrahydrochysenes in it
Furans, the cyclic ethers of perfluor -2- n-propyls penta, PF 5070 active ingredient and other impurities.
Embodiment 1
The method that fluorine carbon solvent is extracted from perfluoro caprylic acid electrolysis by-products, including following step
Suddenly：
(1) alkaline hydrolysis：200kg perfluoro caprylic acid electrolysis by-products are taken, concentration is added thereto is
10% sodium hydrate aqueous solution 20kg, in reacting 4h under 30 DEG C, stirring；
(2) wash：The deionized water of 1.5 times of reaction solution weight is added into Basic fluxing raction liquid
Washing, repeats washing 5 times, and it is 7.5 to measure water layer pH value, discards water layer and produces thick fluorine carbon
Solvent；
(3) dry：The molecular sieve of its weight 20% is added into thick fluorocarbon solvent, shape is stirred
12h, isolated water-free thick fluorine carbon mix are dried under state；
(4) distill：Obtained rough fluorine carbon is added into tower bottom of rectifying tower, implements atmospheric distillation,
It is 2 to control reflux ratio:1, the cut of 80-100 DEG C of temperature range is collected in interception；
(5) filter：The cut being collected into is added into filtering machine with horizontal blade, cut weight is added
The diatomite of amount 5% starts precise filtering device, and it is 2.5kgf/cm to control filter pressure2, it is real
Filter operation is applied, as clear as crystal filtrate is collected, obtains 180kg fluorine carbon solvent finished products.
Embodiment 2
The method that fluorine carbon solvent is extracted from perfluoro caprylic acid electrolysis by-products, including following step
Suddenly：
(1) alkaline hydrolysis：200kg perfluoro caprylic acid electrolysis by-products are taken, concentration is added thereto is
20% potassium tert-butoxide aqueous solution 40kg, in reacting 3h under 30 DEG C, stirring；
(2) wash：The deionized water of 1.5 times of reaction solution weight is added into Basic fluxing raction liquid
Washing, repeats washing 6 times, and it is 7.5 to measure water layer pH value, discards water layer and produces thick fluorine carbon
Solvent；
(3) dry：The molecular sieve of its weight 20% is added into thick fluorocarbon solvent, shape is stirred
24h, isolated water-free thick fluorine carbon mix are dried under state；
(4) distill：Obtained rough fluorine carbon is added into tower bottom of rectifying tower, implements atmospheric distillation,
It is 2 to control reflux ratio:1, the cut of 85-100 DEG C of temperature range is collected in interception；
(5) filter：The cut being collected into is added into filtering machine with horizontal blade, cut weight is added
The diatomite of amount 10% starts precise filtering device, and it is 2.5kgf/cm to control filter pressure2, it is real
Filter operation is applied, as clear as crystal filtrate is collected, obtains 175kg fluorine carbon solvent finished products.
Embodiment 3
The method that fluorine carbon solvent is extracted from perfluoro caprylic acid electrolysis by-products, including following step
Suddenly：
(1) alkaline hydrolysis：200kg perfluoro caprylic acid electrolysis by-products are taken, concentration is added thereto is
20% potassium tert-butoxide aqueous solution 20kg, in reacting 2h under 30 DEG C, stirring；
(2) wash：The deionized water of 1.5 times of reaction solution weight is added into Basic fluxing raction liquid
Washing, repeats washing 5 times, measures water layer pH value for 7, and discarding water layer, to produce thick fluorine carbon molten
Agent；
(3) dry：The molecular sieve of its weight 10% is added into thick fluorocarbon solvent, shape is stirred
24h, isolated water-free thick fluorine carbon mix are dried under state；
(4) distill：Obtained rough fluorine carbon is added into tower bottom of rectifying tower, implements atmospheric distillation,
It is 2 to control reflux ratio:1, the cut of 88-100 DEG C of temperature range is collected in interception；
(5) filter：The cut being collected into is added into filtering machine with horizontal blade, cut weight is added
The diatomite of amount 5% starts precise filtering device, and it is 2kgf/cm to control filter pressure2, implement
Filter operation, collects as clear as crystal filtrate, obtains 185kg fluorine carbon solvent finished products.
Embodiment 4
The operation be the same as Example 1 of the embodiment, it is differed only in：In step (5), mistake
Filter medium is kaolin.
Embodiment 5
The operation be the same as Example 1 of the embodiment, it is differed only in：In step (3), to
The activated carbon water removal of its weight 15% is added in thick fluorocarbon solvent, the water removal time is 20h.
After testing, the technical indicator for the fluorine carbon solvent that embodiment 1 is obtained is：
(1) outward appearance：Colourless transparent liquid, no mechanical admixture
(2) boiling range (101.3KPa)：88~102 DEG C
(3) moisture (PPm)：26
(4) pH value：7.0
The technical indicator for the fluorine carbon solvent that embodiment 2 is obtained is：
(1) outward appearance：Colourless transparent liquid, no mechanical admixture
(2) boiling range (101.3KPa)：90~100 DEG C
(3) moisture (PPm)：28
(4) pH value：7.3
The technical indicator for the fluorine carbon solvent that embodiment 3 is obtained is：
(1) outward appearance：Colourless transparent liquid, no mechanical admixture
(2) boiling range (101.3KPa)：92~100 DEG C
(3) moisture (PPm)：30
(4) pH value：7.2
The technical indicator for the fluorine carbon solvent that embodiment 4 is obtained is：
(1) outward appearance：Colourless transparent liquid, no mechanical admixture
(2) boiling range (101.3KPa)：88~102 DEG C
(3) moisture (PPm)：26
(4) pH value：7.0
The technical indicator for the fluorine carbon solvent that embodiment 5 is obtained is：
(1) outward appearance：Colourless transparent liquid, no mechanical admixture
(2) boiling range (101.3KPa)：88~102 DEG C
(3) moisture (PPm)：25
(4) pH value：7.0
The fluorine carbon solvent quality that embodiment 1-5 is prepared is good, available for precise electronic,
Instrument, equipment, highly dense huge capacity compact discs, the cleaning-drying for collecting communication tool etc..
Although, above with general explanation, embodiment and experiment, to this hair
It is bright to have made detailed description, but on the basis of the present invention, it can be made some modifications or improvements,
This will be apparent to those skilled in the art.Therefore, without departing from spirit of the invention
On the basis of these modifications or improvements, belong to the scope of protection of present invention.
Claims (10)
1. extracting the method for fluorine carbon solvent from perfluoro caprylic acid electrolysis by-products, its feature exists
In comprising the following steps：
(1) alkaline hydrolysis：Alkaline matter is added into perfluoro caprylic acid electrolysis by-products, alkaline hydrolysis is carried out
Reaction；
(2) wash and dry：Basic fluxing raction liquid is washed to water layer pH most 7-8, thick fluorine carbon is obtained
Plain solvent, dries the moisture removed in the thick fluorocarbon solvent；
(3) distill：Dried thick fluorocarbon solvent is distilled, and takes 85-102 DEG C of temperature range
Cut produce.
2. according to the method described in claim 1, it is characterised in that：The alkaline matter is
One kind or several in sodium hydroxide, calcium hydroxide, potassium hydroxide, potassium tert-butoxide, sodium tert-butoxide
Plant, preferably potassium tert-butoxide, it is further preferred that the addition of the alkaline matter is perfluor
The 1-5% of sad electrolysis by-products weight.
3. method according to claim 1 or 2, it is characterised in that：By the alkalescence
Material is configured to the concentration 5-40% aqueous solution and added in perfluoro caprylic acid electrolysis by-products, described dense
Degree is preferably 10-20%.
4. the method according to claim any one of 1-3, it is characterised in that：The alkali
Solving the condition reacted is：20-50 DEG C of temperature, reaction time 1-5h；Preferably：30-40 DEG C of temperature,
Reaction time 3-4h.
5. the method according to claim any one of 1-4, it is characterised in that：Using point
Moisture in son sieve or the activated carbon removing thick fluorocarbon solvent, preferably molecular sieve, further
The consumption of preferred molecular sieve is the 10-20% of the thick fluorocarbon solvent weight.
6. the method according to claim any one of 1-5, it is characterised in that：It is described to steam
Evaporate for air-distillation, preferably reflux ratio is (1.5-2.5)：1, more preferably 2:1.
7. the method according to claim any one of 1-6, it is characterised in that：Also include
The step of being filtered to the product after distillation, the filtering using alkaline carclazyte, Emathlite,
One or more as filter medium in diatomite, kaolin, preferably diatomite enters one
The consumption for walking preferred filter media is the 5-20% of products weight.
8. the method according to claim any one of 1-7, it is characterised in that：The mistake
Filter as pressure filtration, filter pressure is 1-4kgf/cm2, preferably 1.5-2.5kgf/cm2。
9. any one of claim 1-8 methods described extracts obtained fluorine carbon solvent, it is special
Levy and be：Including perfluor -2- normal-butyls tetrahydrofuran, the cyclic ethers of perfluor -2- n-propyls penta, perfluor
Heptane component.
10. fluorine carbon solvent according to claim 9, it is characterised in that：The fluorine carbon
85-102 DEG C of the boiling range (101.3Kpa) of plain solvent, moisture≤50PPm, pH value 7-7.5.
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| CN201610136814.7A CN107176737A (en) | 2016-03-10 | 2016-03-10 | The method that fluorine carbon solvent is extracted from perfluoro caprylic acid electrolysis by-products |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115806459A (en) * | 2022-12-13 | 2023-03-17 | 山东新时代药业有限公司 | Purification method for recovering fluorocarbon solvent from mixed waste solvent |
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| CN100999456A (en) * | 2006-12-30 | 2007-07-18 | 山东东岳神舟新材料有限公司 | Preparation method of perfluoro caprylic acid |
| CN103086865A (en) * | 2013-01-29 | 2013-05-08 | 浙江大学 | Treatment method of perfluoroalkyl acyl fluoride waste |
| CN103570202A (en) * | 2013-11-04 | 2014-02-12 | 中昊晨光化工研究院有限公司 | Method and device for recovering electrolytic residues produced in process of producing perfluorocaprylic acid by electrolytic process |
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| US2999885A (en) * | 1959-09-17 | 1961-09-12 | Du Pont | Purification of fluorocarbons |
| CN1119853A (en) * | 1993-03-30 | 1996-04-03 | 美国3M公司 | Continuous process for purifying perfluorochemical compositions |
| CN100999456A (en) * | 2006-12-30 | 2007-07-18 | 山东东岳神舟新材料有限公司 | Preparation method of perfluoro caprylic acid |
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| CN115806459A (en) * | 2022-12-13 | 2023-03-17 | 山东新时代药业有限公司 | Purification method for recovering fluorocarbon solvent from mixed waste solvent |
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