CN109592646A - A kind of preparation method of ozonated water emulsion - Google Patents
A kind of preparation method of ozonated water emulsion Download PDFInfo
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- CN109592646A CN109592646A CN201811565620.4A CN201811565620A CN109592646A CN 109592646 A CN109592646 A CN 109592646A CN 201811565620 A CN201811565620 A CN 201811565620A CN 109592646 A CN109592646 A CN 109592646A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B13/00—Oxygen; Ozone; Oxides or hydroxides in general
- C01B13/10—Preparation of ozone
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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Abstract
The present invention discloses a kind of preparation method of ozonated water emulsion, realizes ozonisation organic matter and the preparation of ozonated water/liquid two-step method.Ozone is generated first with ozone generating-device, ozone is reacted with organic matter then, ozonisation organic matter is prepared；Ozonisation organic matter is emulsified in water finally, obtains ozonated water emulsion.Have using the ozonated water emulsion of this method preparation easy to use, the stability of ozone in the solution is high, preparation process is not limited by place and equipment, the advantages that attenuation loss of ozone is few, realize preparation and the high-efficiency cleaning environmental protection of application process, with good economic efficiency and social benefit.
Description
Technical field
The present invention relates to a kind of preparation method of ozonated water emulsion, in particular to a kind of first to prepare ozonisation organic
Then object emulsifies the method for obtaining ozonated water emulsion in water.
Background technique
Ozone (O3) it is also known as super oxygen, it is oxygen (O2) allotrope, at normal temperature, it is that one kind has off-odor
Light blue gas, product after decomposition is oxygen.Ozone is a kind of strong oxidizer, its oxidation-reduction potential in water is
2.07 eV are only second to fluorine (2.5 eV), and oxidability is higher than chlorine (1.36 eV) and chlorine dioxide (1.5 eV).With hypochlorous acid class
Disinfectant is different, and the sterilizing ability of ozone is not influenced by pH value variation and ammonia, and sterilizing ability is 600-3000 times bigger than chlorine, it
Sterilizing, disinfection almost instantaneously occur, when the ozone concentration in water reaches 0.3-2 mg/L, in 0.5-1 min
It is interior can lethal bacterium.The dosage of Ozone Water needed for reaching identical sterilization effect (as made Escherichia coli killing rate up to 99%) is only
It is the 0.0048% of chlorine.In addition, ozone can also aoxidize, decompose pollutant in water, in water treatment field, to deodorization, decoloration,
It sterilization, removal phenol, cyanogen, iron, manganese and reduces COD, BOD etc. all there is significant effect.Therefore, ozone is in medicine, water process, food
, there is extensive purposes in the fields such as product and agricultural.
The producing method of ozone mainly has corona method, electrolysis method, ultraviolet method, nuclear radiation method, plasma method etc..Food
The industries such as product, medicine mainly manufacture ozone with corona discharge method and electrolysis method.Using air as gas source, using corona discharge method
When preparing ozone, the harmful nitrogen oxides of meeting by-product, this feature limits the applications of this method；Electrolyzing pure water output ozone,
It is to prepare the highest method of ozone concentration at present, and the by-product in gas is oxygen, without secondary pollution.In addition, using smelly
The difference of oxygen and oxygen boiling point, the ozone that can be enriched with by grading liquefaction.
But ozone is disorderly diffused into air and also brings along certain harm.And ozone liquidization can then be incited somebody to action
Ozone confinement in the liquid phase, can avoid effective consumption and the loss of ozone while improving the ozone concentration for applying part,
Ozone loss bring is avoided to endanger.But the stability of ozone is poor, and half-life period of the ozone in distilled water or tap water is about
It is 20 min(20 DEG C), then it is decomposed into oxygen rapidly in the aqueous solution containing impurity.Therefore, in actual use, ozone is past
It toward instant system is needed, is limited by equipment and place larger, significantly limits the application of ozone.
Summary of the invention
The present invention is intended to provide a kind of preparation method of ozonated water emulsion, realizes ozonisation organic matter and ozonisation
The preparation of water/liquid two-step method opens the new route of liquid phase ozonisation, and the stability of ozonated water emulsion is high,
The preparation of ozone uses the limitation that will not be subject to place and equipment.
To achieve the goals above, the technical solution adopted in the present invention is as follows: the present invention relates to a kind of ozonisation water and milk
The preparation method for changing liquid, specifically comprises the following steps:
A, high-concentrated ozone is generated using ozone generating-device；
B, ozone is reacted with unsaturated long-chain organic matter, ozonisation organic matter is prepared；
C, ozonisation organic matter is emulsified in water, obtains ozonated water emulsion.
Further, the ozone generating-device is electrolytic ozone generator or smelly as the electrion of gas source using oxygen
Oxygengenerating plant.
Further, the high-concentrated ozone is rich gaseous mixture ozoniferous, and ozone concentration is higher than 100 ppm, ozone
Content is 5 ~ 30%.
Further, the unsaturated long-chain organic matter includes the unsaturated long-chain hydrocarbon of carbon atom number >=6 in molecule
The mixture of compound, unsaturated fatty acid, unsaturated fat compounds of group or any the two and three；Specifically may be selected include
The animal oil such as fish oil also may be selected in vegetable oil including long-chain olefin, olive oil, tea oil etc..
Further, the ozonation of the ozonisation organic matter is 20 ~ 50%.
Further, the ozone is heterogeneous reaction with unsaturated reacting for long-chain organic matter progress, which can
Using be bubbled mixing, jet mixing, be stirred, pipeline mixed form progress gas and oil be mixed.
Further, the ozone is reacted with unsaturated long-chain organic matter, and the temperature of reaction is dodged lower than organic matter
It puts and is higher than melting point of organic matter.
Further, the ozone is reacted with unsaturated long-chain organic matter, the equipment material energy contacted with material
Enough resistance against ozone and organic matter corrode, and to ozone and ozonide without catalyticing decomposition action, and suitable material includes glass, pottery
Porcelain, PTFE, stainless steel and titanium.
Further, ozonisation organic matter emulsifies in water, and nonaqueous component, but respective components can be contained in used water
There must not be apparent catalyticing decomposition action to ozone and ozonisation organic matter, and the use that can satisfy ozonated water emulsion is wanted
It asks.
Further, described to emulsify ozonisation organic matter as heterogeneous process in water, which can be used jet stream
Emulsification, mechanical shearing emulsification, film emulsification, ultrasonic emulsification form carry out, ozonisation organic matter shared volume in aqueous solution
Ratio is 0.1 ~ 10%.
Further, described to emulsify ozonisation organic matter in water, the continuous phase after emulsification is water, and dispersed phase is to have
Machine object, and dispersed phase particle average grain diameter is less than 100 μm.
The beneficial effects of the present invention are:
1) preparation method of ozonated water emulsion disclosed by the invention realizes ozonisation organic matter and ozonated water/liquid
Two-step method preparation, by raw material selection, preparation process control and application conditions optimize, effectively cooperateed with the preparation and storage of ozone
Deposit with the preparation of ozonated water/liquid and use, open a liquid phase ozonisation new route；
2) using this method solve ozone in use because of the problem that itself unstable (rapid decay) need to be prepared in situ,
It is not limited by ozone preparation conditions such as live power supply, equipment, the bottleneck for breaching the preparation of ozonated water/liquid and using；
3) preparation method for using this ozonated water emulsion, while realizing water phase ozonisation, by being dispersed in water phase
Ozonisation oil droplet ozonidation, improve the stability of ozonated liquid, solve ozone in the homogeneous object system of single water
In time stability problem；
4) preparation method of this ozonated water emulsion is used, in the ozonated liquid being prepared, the ozonisation of dispersion has
Machine object droplet is not only that the ozonisation of water phase provides ozone source, in use, also because volatility is low, stability is good etc.
Feature improves ozonated liquid in different use conditions (such as quickly volatilization environment and the high temperature, drying such as spraying, liquid film
Etc. factors) under stability, improve use condition stability problem of the ozone in the homogeneous object system of single water；
5) preparation method of this ozonated water emulsion is used, it can be reduced simultaneously by ozone content in improving ozonated liquid
The volatilization escape amount of middle ozone is realized ozonated liquid preparation and is made to avoid environmental pollution simultaneously improving using effect
High-efficiency cleaning environmental protection.
Specific embodiment
In order to make those skilled in the art be better understood on technical solution of the present invention, below with reference to embodiment
Technical solution of the present invention is further described.
In order to solve ozone in the prior art, stability is poor in the solution, the high problem of the attenuation loss of ozone, the present invention
A kind of ozonated water emulsification liquid and preparation method thereof is disclosed, based on principle be ozone can occur with organic matter containing double bonds plus
Primary ozonide is generated at reaction, then primary ozonide resolves into carbonyls aldehydes or ketones and oxidation carbonyl, aoxidizes carbonyl
Ozonide can also be recombined into aldehydes or ketones.Organic matter is ozonized, the available ozonisation with certain stability
Object.The ozonide can show the typical characteristics of the ozone such as strong oxidizing property in the application.Ozonide is prepared, then by it
It is distributed in water phase, ozonated water emulsion can be prepared simultaneously, improve the ozone stable of the liquid.
Method disclosed by the invention specifically comprises the following steps:
A, high-concentrated ozone is generated using ozone generating-device；
B, ozone is reacted with unsaturated long-chain organic matter, ozonisation organic matter is prepared；
C, ozonisation organic matter is emulsified in water, obtains ozonated water emulsion.
Ozone generating-device used in step a is electrolytic ozone generator or smelly as the electrion of gas source using oxygen
Oxygengenerating plant.Wherein, ozone is prepared using pure water electrolysis method, has ozone concentration height, gas composition simple (for ozone and oxygen
The mixture of gas), it is safe and convenient to use the advantages that, be preferred method.When preparing ozone using electrion process, oxygen should be used
As gas source, paying particular attention to, which should be avoided, uses air as gas source for gas or oxygen rich gas, to prevent nitrogen oxides from generating simultaneously
Into in ozonisation organic matter.
Efficiency is ozonized to improve, in ozonisation organic matter preparation process, used ozone is rich ozoniferous mixed
Gas is closed, ozone concentration is higher than 100ppm, and preferably ozone content is 5 ~ 30%.In addition, during the reaction, gas can be used and press again
The forms such as contracting or optimization gassing rate carry out concerted reaction process, to avoid the waste of ozone, and improve ozonation efficiency.
Unsaturation long-chain organic matter used in step b is the unsaturated long chain hydrocarbon of carbon atom number >=6 in molecule
The mixture of object, unsaturated fatty acid, unsaturated fat compounds of group or any the two and three.Choose the conduct of long-chain organic matter
Raw material, can be volatile, flash-point is low to avoid small organic molecule the problems such as.In as needed, can choose long-chain olefin,
The vegetable oil such as olive oil, tea oil also can choose the animal oil such as fish oil.Before use necessary removal of impurities, essence should be carried out to organic matter
The pretreatment such as refining.In addition, in terms of unsaturated bond ozonation, the ozonation for ozonizing organic matter is generally 0.1% ~
90%, preferred ozonation is generally 20% ~ 50%.
It is heterogeneous reaction that ozone, which react with organic matter, in step b, which can be used bubbling mixing, jet stream mixes
It closes, be stirred, pipeline mixed form carries out heterogeneous be mixed.By strengthening effect of mass transmitting, ozone gas can be dispersed
In organic matter, to improve gas liquid film, accelerate ozonization and absorption rate, while also improving releasing for reaction residual gas
It puts, organic matter inner transition is avoided to inflate.
Object system is kept to be in preferable flow regime in the disclosed ozonisation organic matter preparation process of the step b, favorably
Mass transfer and heat transfer in process, wherein the temperature of material becomes an important control parameter.To realize above-mentioned requirements and avoiding
The security risks such as fire explosion, according to the difference of used raw material organic matter, the ozone is reacted with organic matter, reaction
Temperature lower than organic matter flash-point and be higher than melting point of organic matter.At typical condition, nearly room temperature (0-50 DEG C) is one preferred
Temperature range.The preparation method of a kind of ozonated water emulsion, characterized in that the ozone and organic matter carries out anti-
Answer, the equipment material contacted with material should be able to resistance against ozone and organic matter corrode, and to ozone and ozonisation organic matter without urging
Change decomposition.Typically applicable material includes glass, ceramics, PTFE, stainless steel, titanium etc., but the metals such as aluminium, copper, iron, carbon steel
And use should be avoided in polyvinyl chloride, silica gel, rubber etc., to prevent ozone depletion, material pollution and equipment damage.
Ozonisation organic matter is emulsified in water in the step c, nonaqueous component can be contained in used water, but corresponding
Component must not have apparent catalyticing decomposition action to ozone and ozonated water emulsion, and can satisfy ozonated water emulsion
Requirement.Ozonated water emulsion can be used pure water, tap water, underground water, surface water or particular solution (such as salting liquid,
Diluted acid, diluted alkaline etc.) it prepares, but substance contained therein should have the reactionlessness to ozone and organic matter, while should be able to
Meet storage, the requirement of ozonated water emulsion.In general, pure water is a preferred raw material.
Ozonisation organic matter is emulsified in water as heterogeneous process in the step c, the process can be used aqualase,
Mechanical shearing emulsification, film emulsification, the form progress of ultrasonic emulsification.By strengthening mass transfer, water-oil phase can be dispersed.Root
According to the state (liquid, paste, nearly solid-state) of ozonisation organic matter, emulsifying manner can be chosen suitably to reinforce emulsifying.Generally smelly
It aoxidizes in water-in-oil emulsion, shared volume ratio is not higher than 50% to ozonisation organic matter in aqueous solution, and preferred ratio is 0.1%
~10%.For paste and nearly solid ozonisation organic matter, temperature or addition solvent, surfactant can be properly increased to mention
The efficiency of height emulsification.But when adding third component, it should be avoided, ozonisation organic matter and ozonated water emulsion are generated not
Acceptable influence.
The preparation method of a kind of ozonated water emulsion, characterized in that described will ozonize organic matter in water
Middle emulsification, the continuous phase after emulsification are water, and dispersed phase is oil, and dispersed phase oil droplet average grain diameter is less than 100 μm.Actually make
The partial size of emulsified oil droplet is adjusted in the process, can according to need, but be should be noted that and avoided the poly- of oil droplet and divide with grease
Phase phenomenon.
In the preparation process of ozonated water emulsion, the addition aromatic, coloring agent, liquid in object system can according to need
The modifying agents such as body paraffin, to improve the application performance and effect of ozonated water emulsion.But the component being added, general additive amount
Less than the 50% of ozonisation organic matter additive amount, and should be avoided can not to ozonisation organic matter and the generation of ozonated water emulsion
The influence of receiving.
The several specific embodiments of following discloses
Embodiment one
High-concentrated ozone gas (wherein ozone content about 15%) is generated using Low Voltage Pure water Electrooxidation ozone generator, by ozone
The 316L stainless steel blistering reaction equipped with olive oil Yu acid mixture (the two volume ratio 1:1) is passed through after gas collection
In kettle, reacted under the conditions of stirring and 20 DEG C, the ozonation of sampling and testing organic matter, when ozonation >=20%
Stop blasting ozone afterwards.Organic matter will be ozonized according to the ratio of ozonisation organic matter and the volume ratio 1:100 of water to mix with pure water
It closes, is emulsified using high-speed shearing machine, the ozonisation organic particle partial size to suspend in continuous aqueous phase after emulsification is about 50 μ
m.The ozonated water emulsion is diluted 10 times, ozone under the conditions of closed, glass container and 20 DEG C, with same ozone concentration
Pure water solution is compared, and the ozone concentration of rear ozonated water emulsion is 10 times of Ozone Water or more for 24 hours.
Embodiment two
High-concentrated ozone gas (wherein ozone content about 20%) is generated using pure water Electrooxidation ozone generator, by ozone gas
It is passed through after collection in the enamel pipeline reactor equipped with C8 alkene and fish oil blend (the two volume ratio 1:5), in pipeline
Circulation be mixed and 30 DEG C under the conditions of reacted, the ozonation of sampling and testing organic matter, when ozonation reaches
Stop being passed through ozone after 30%.It, will be smelly using film emulsifying device according to the ratio of ozonisation organic matter and the volume ratio 1:50 of pure water
Oxidation of organic compounds emulsifies in aqueous solution, and 100ppm dodecyl sodium sulfate is added in emulsion, hangs in continuous aqueous phase after emulsification
Floating ozonisation organic particle partial size is about 20 μm.The ozonated water emulsion is diluted 100 times, in closed, glass container
Under the conditions of 20 DEG C, compared with the ozone pure water solution of same ozone concentration, the ozone concentration of rear ozonated water emulsion is for 24 hours
10 times or more of Ozone Water.
Embodiment three
Using purity oxygen as gas source, high-concentrated ozone gas (wherein ozone content > 5%) is generated using corona method ozone generator,
The PTFE coating still reaction equipped with olive oil Yu fish oil blend (the two volume ratio 4:1) is passed through after ozone gas is collected
In device, gas is exposed in organic matter using micro porous aeration head, is reacted under the conditions of being mixed with 35 DEG C, sampling and testing has
The ozonation of machine object stops being passed through ozone after ozonation reaches 50%.According to the carbon of ozonisation organic matter and pH=8
The ratio of sour sodium pure water solution volume ratio 1:500 will ozonize organic matter emulsification in aqueous solution using ultrasonic emulsification equipment, cream
The ozonisation organic particle partial size to suspend in continuous aqueous phase after change is about 30 μm.Iodine is added in the ozonated water emulsion
Change sodium chromogenic reagent (until instilling IodineSodium Solution to ozonated water emulsion colour developing), takes the ozonated water emulsion,
Under the conditions of closed, glass container and 20 DEG C, compared with the ozone pure water solution of same ozone concentration, for 24 hours after ozonated water emulsification
The ozone concentration of liquid is 10 times of Ozone Water or more, and ozone concentration and ozone in ozonated water emulsion liquid layer surface vapor
Ozone concentration in aqueous layer surface gas phase is suitable, this shows that ozonated water emulsion has good ozone hold capacity, together
When can effectively avoid the decomposition and volatilization of ozone.
Embodiment four
Using purity oxygen as gas source, high-concentrated ozone gas (wherein ozone content > 5%) is generated using corona method ozone generator,
The glass equipped with olive oil, fish oil and C10 alkene mixture (three volume ratio 2:3:1) is passed through after ozone gas is collected to turn
In disk tower reactor, gas is exposed in tower reactor organic matter using micro porous aeration head, and in mixing, gas lift promotes and 15 DEG C of items
It is reacted under part, the ozonation of sampling and testing organic matter, stops being passed through ozone after ozonation reaches 60%.It presses
It, will using emulsification pretreatment equipment according to the ratio of ozonisation organic matter and the sodium hydroxide pure water solution volume ratio 1:300 of pH=8.5
Ozonize organic matter emulsification in aqueous solution, the ozonisation organic particle partial size to suspend in continuous aqueous phase after emulsification is about 60 μ
m.The ozonated water emulsion is taken, ozone pure water solution under the conditions of closed, glass container and 20 DEG C, with same ozone concentration
It compares, the ozone concentration of rear ozonated water emulsion is 10 times of Ozone Water or more for 24 hours, and ozonated water emulsion liquid layer surface
Ozone concentration in gas phase is suitable with the ozone concentration in Ozone Water liquid layer surface vapor.
Basic principles and main features and advantage of the invention have been shown and described above.But the foregoing is merely this hairs
Bright specific embodiment, technical characteristic of the invention are not limited thereto, and any those skilled in the art is not departing from this hair
The other embodiments obtained under bright technical solution should all cover within the scope of the patent of the present invention.
Claims (10)
1. a kind of preparation method of ozonated water emulsion, which is characterized in that specifically comprise the following steps:
A, high-concentrated ozone is generated using ozone generating-device；
B, ozone is reacted with unsaturated long-chain organic matter, ozonisation organic matter is prepared；
C, ozonisation organic matter is emulsified in water, obtains ozonated water emulsion；
Wherein, in terms of unsaturated bond ozonation, the ozonation of the ozonisation organic matter prepared in the step b is
Organic matter shared volume ratio in aqueous solution is ozonized in the ozonated water emulsion prepared in 0.1 ~ 90%, the step c
Not higher than 50%.
2. a kind of preparation method of ozonated water emulsion as described in claim 1, which is characterized in that the ozone fills
It is set to electrolytic ozone generator or using oxygen as the electrion ozone generating-device of gas source.
3. a kind of preparation method of ozonated water emulsion as claimed in claim 2, which is characterized in that the high concentration is smelly
Oxygen is rich gaseous mixture ozoniferous, and ozone concentration is higher than 100 ppm, and ozone content is 5 ~ 30%.
4. a kind of preparation method of ozonated water emulsion as claimed in claim 3, which is characterized in that the unsaturation is long
Chain organic matter includes the unsaturated long chain hydrocarbon of carbon atom number >=6 in molecule, unsaturated fatty acid, unsaturated aliphatic
The mixture of compound or any the two and three.
5. a kind of preparation method of ozonated water emulsion as claimed in claim 4, which is characterized in that the ozone with not
Be saturated long-chain organic matter carry out reaction be heterogeneous reaction, the reaction can be used be bubbled mixing, jet mixing, be stirred,
Pipeline mixed form carries out gas and oil and is mixed, and the ozonation of the ozonisation organic matter is 20 ~ 50%.
6. a kind of preparation method of ozonated water emulsion as claimed in claim 5, which is characterized in that ozone is long with unsaturation
The temperature that chain organic matter is reacted is lower than organic matter flash-point and is higher than melting point of organic matter.
7. a kind of preparation method of ozonated water emulsion as claimed in claim 6, which is characterized in that ozone is long with unsaturation
When chain organic matter is reacted, the equipment material contacted with material is resistant to ozone and organic matter and corrodes, and to ozone and smelly
For oxide without catalyticing decomposition action, suitable material includes glass, ceramics, PTFE, stainless steel and titanium.
8. a kind of preparation method of ozonated water emulsion as claimed in claim 7, which is characterized in that ozonisation organic matter exists
It is emulsified in water, nonaqueous component can be contained in used water, but respective components must not have obviously ozone and ozonisation organic matter
Catalyticing decomposition action, and can satisfy the requirement of ozonated water emulsion.
9. a kind of preparation method of ozonated water emulsion as claimed in claim 8, which is characterized in that described will ozonisation
It is heterogeneous process that organic matter emulsifies in water, which can be used aqualase, mechanical shearing emulsification, film emulsification, ultrasound cream
The form of change carries out, and shared volume ratio is 0.1 ~ 10% to ozonisation organic matter in aqueous solution.
10. a kind of preparation method of ozonated water emulsion as claimed in claim 9, which is characterized in that described by ozone
Change organic matter to emulsify in water, the continuous phase after emulsification is water, and dispersed phase is organic matter, and dispersed phase particle average grain diameter is less than
100 μm。
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| JP2008019359A (en) * | 2006-07-13 | 2008-01-31 | Shinkawa Yoshiro | Manufacturing method of emulsion composition and apparatus for emulsification |
| KR20160042209A (en) * | 2014-10-07 | 2016-04-19 | 세연에스앤알 주식회사 | Method of manufacturing ozonized composition of oil, and ozonized composition of oil manufactured by using the same |
| CN106881055A (en) * | 2017-04-10 | 2017-06-23 | 安徽嘉宝诺生物科技有限公司 | Ozone solidifies emulsifier unit and the sterilized agent and process for producing same of ozone solidification emulsification |
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Application publication date: 20190409 |
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