CN109319913A - A kind of slow-release oxone and preparation method thereof - Google Patents
A kind of slow-release oxone and preparation method thereof Download PDFInfo
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- CN109319913A CN109319913A CN201811184568.8A CN201811184568A CN109319913A CN 109319913 A CN109319913 A CN 109319913A CN 201811184568 A CN201811184568 A CN 201811184568A CN 109319913 A CN109319913 A CN 109319913A
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
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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
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
Abstract
The present invention provides a kind of slow-release oxones, from the inside to the outside successively include carrying pill core, inner layer film clothing and outer membrane clothing；The raw material components for carrying pill core include potassium hydrogen persulfate, filler, No.1 plasticizer, sodium carboxymethylcellulose and water, the raw material components of the inner layer film clothing include ethyl cellulose, No. two plasticizer, pore-foaming agent and organic solvent, and the raw material components of the outer membrane clothing include hydroxypropyl methyl cellulose, No. three plasticizer, potassium hydrogen persulfate and water.The present invention also provides a kind of preparation methods using above-mentioned slow-release oxone, comprising the following steps: (1) production carries pill core；(2) inner layer film clothing solution is synthesized；(3) outer membrane clothing solution is synthesized；(4) coating.The present invention can solve that the potassium hydrogen persulfate rate of release that existing oxone generates in use is uncontrollable, treatment effect is bad, cumbersome, preparation is easy the problem high with processing cost that become damp and rotten.
Description
Technical field
The present invention relates to a kind of slow-release oxones and preparation method thereof, belong to water-treatment technology field.
Background technique
Potassium hydrogen persulfate is due to non-toxic with superpower oxidisability and its oxidation product, frequently as disinfectant, water purification agent
With the preparations such as bleaching agent, it is more and more widely used in every field.In domestic market, potassium hydrogen persulfate is typically made
Ammonium persulfate-sodium bisulfate preparation such as carries out disinfection to water body and purifies at the processing.The property of ammonium persulfate-sodium bisulfate preparation is unstable
It is fixed, it is easy to meet water, is heated and decomposes, influence effect, thus the requirement of its holding conditions is high；In addition, potassium hydrogen persulfate is compound
The potassium hydrogen persulfate contained in salt pref it is expensive, during using ammonium persulfate-sodium bisulfate preparation, due to
It is readily dispersed in water body, and reaction rate and reaction density are unable to control, so that the function and effect of preparation are bad and act on
Time is of short duration, it is often necessary to artificially add preparation, to ensure that function and effect reach expected, therefore be easy to cause potassium hydrogen persulfate
Waste, processing cost improve.
A kind of effectively control potassium hydrogen persulfate rate of release how is invented, treatment effect is improved, simplifies operation, is easy to store
It is that current those skilled in the art is urgently to be resolved with the slow-release oxone of save the cost and preparation method thereof to ask
Topic.
Summary of the invention
It is an object of the invention to propose a kind of slow-release oxone and preparation method thereof, to solve existing mistake
The potassium hydrogen persulfate rate of release that potassium acid sulfate preparation generates in use is uncontrollable, treatment effect is bad, it is cumbersome,
Preparation is easy the problem high with processing cost that become damp and rotten.
To achieve this purpose, the present invention adopts the following technical scheme:
A kind of slow-release oxone successively includes carrying pill core, inner layer film clothing and outer membrane clothing from the inside to the outside；
The thickness of the inner layer film clothing is greater than 0.1mm, and the outer membrane clothing accounts for the slow-release oxone gross mass percentage
Than 0.1%~0.5%；
The raw material components for carrying pill core include potassium hydrogen persulfate, filler, No.1 plasticizer, sodium carboxymethylcellulose
And water, the mass ratio for carrying pill core each raw material component are as follows: potassium hydrogen persulfate 3~7: filler 14~16: No.1 plasticizer 3
~5: sodium carboxymethylcellulose 0.01~0.1: water 4~8, the No.1 plasticizer are water-soluble plasticizer；
The raw material components of the inner layer film clothing include ethyl cellulose, No. two plasticizer, pore-foaming agent and organic solvent, described
The mass ratio of inner layer film clothing each raw material component are as follows: 12~18: No. two plasticizer 2~4 of ethyl cellulose: pore-foaming agent 3~5: organic
Solvent 75~85, No. two plasticizer are fat-soluble plasticizer；
The raw material components of the outer membrane clothing include hydroxypropyl methyl cellulose, No. three plasticizer, potassium hydrogen persulfate and water,
The mass ratio of the outer membrane clothing each raw material component are as follows: 4~6: No. three plasticizer 4~6 of hydroxypropyl methyl cellulose: hydrogen persulfate
Potassium 1~3: water 80~120, No. three plasticizer are water-soluble plasticizer.
Further, the No.1 plasticizer is sucrose, and No. two plasticizer are triethyl citrate, No. three increasings
Modeling agent is polyethylene glycol-400.
Further, the pore-foaming agent is Polyethylene glycol-2000, and the organic solvent is dehydrated alcohol, the filler
For starch.
Further, the inner layer film clothing with a thickness of 0.2mm, the outer membrane clothing accounts for the slow-release potassium hydrogen persulfate
Preparation gross mass percentage 0.2%.
Further, the raw material components for carrying pill core include potassium hydrogen persulfate, filler, No.1 plasticizer, carboxylic first
Base sodium cellulosate and water, the mass ratio for carrying pill core each raw material component are as follows: potassium hydrogen persulfate 6: filler 15: No.1 plasticising
Agent 4: sodium carboxymethylcellulose 0.05: water 5；
The raw material components of the inner layer film clothing include ethyl cellulose, No. two plasticizer, pore-foaming agent and organic solvent, described
The mass ratio of inner layer film clothing each raw material component are as follows: 15: No. two plasticizer 3 of ethyl cellulose: pore-foaming agent 4: organic solvent 80；
The raw material components of the outer membrane clothing include hydroxypropyl methyl cellulose, No. three plasticizer, potassium hydrogen persulfate and water,
The mass ratio of the outer membrane clothing each component are as follows: 5: No. three plasticizer 5 of hydroxypropyl methyl cellulose: potassium hydrogen persulfate 2: water 100.
6. a kind of preparation method of slow-release oxone, comprising the following steps:
(1) production carries pill core: No.1 plasticizer and sodium carboxymethylcellulose is soluble in water, mixed liquor A is obtained, incited somebody to action
After potassium acid sulfate and filler mixing, it is dried after sufficiently being mixed with mixed liquor A, obtains and carry pill core；
(2) it synthesizes inner layer film clothing solution: ethyl cellulose is added in organic solvent, carry out heating water bath, stir, be added
No. two plasticizer and pore-foaming agent, stirring to ethyl cellulose are dissolved, and inner layer film clothing solution is obtained；
(3) it synthesizes outer membrane clothing solution: hydroxypropyl methyl cellulose and potassium hydrogen persulfate is added to the water, carry out water-bath and add
Heat adds No. three plasticizer, and stirring to hydroxypropyl methyl cellulose is dissolved, and obtains outer membrane clothing solution；
(4) coating: being repeatedly dipped to load pill core in inner layer film clothing solution, takes out, then be dipped to outer membrane clothing repeatedly
It in solution, shakes, filter after taking-up, carry out vacuum drying treatment to constant weight, obtain slow-release oxone.
Further, the step (2) synthesizes inner layer film clothing solution: ethyl cellulose being added in organic solvent, is carried out
Heating water bath No. two plasticizer is added while stirring, pore-foaming agent is added after stirring 30 minutes, stirs complete to ethyl cellulose
It keeps standing 10 minutes under heating water bath state after dissolution, obtains inner layer film clothing solution；
The step (3) synthesizes outer membrane clothing solution: hydroxypropyl methyl cellulose and potassium hydrogen persulfate is added to the water, into
Row heating water bath adds No. three plasticizer, keeps heating water bath to stir 30 minutes, is stirred under room temperature to hydroxypropyl methyl
Cellulose is completely dissolved, and stands 10 minutes under room temperature, obtains outer membrane clothing solution.
Further, it is 2~6 times that pill core is carried in the step (4) to impregnate the number of inner layer film clothing solution, the step
(4) number for carrying pill core immersion outer membrane clothing solution that inner layer film clothing is enclosed in is 2~3 times.
Further, it is 2 times that pill core is carried in the step (4) to impregnate the number of inner layer film clothing solution, the step (4)
In be enclosed with inner layer film clothing carry pill core impregnate outer membrane clothing solution number be 2 times.
Further, the condition of the step (2) and the heating water bath in the step (3) is not higher than 60 DEG C, described
Drying temperature in step (1) and the step (4) is not higher than 30 degrees Celsius.
The beneficial effects of the present invention are: the outer membrane clothing of (1) this slow-release oxone has selected hydroxypropyl first
Base cellulose, inner layer film clothing have selected ethyl cellulose, so that pill core is carried after outer membrane clothing and inner layer film clothing package, preparation
Whole stability is improved, and prevents this slow-release oxone rotten；(2) when potassium hydrogen persulfate is above two
It is placed in water after coating package, outer membrane clothing is contacted with water at first and dissolved, and releases the persulfuric acid contained in outer membrane clothing
Hydrogen potassium, after outer membrane clothing is completely dissolved, inner layer film clothing is contacted with water, and forms duct in inner layer film clothing by pore-foaming agent,
Potassium hydrogen persulfate is gradually released, achievees the purpose that be sustained potassium hydrogen persulfate, realize to oxone rate of release
Control；(3) release concentration of this slow-release oxone control potassium hydrogen persulfate can be played persistently whithin a period of time
It the effects of to the disinfection of water body, purification, to extend the effective reaction time of potassium hydrogen persulfate, can both save to greatest extent
Cost, and good treatment effect can be played；(4) during processing, without going dispensing said preparation also can be one on time daily
The amount of potassium hydrogen persulfate is in the state of reaction balance in control water in the section more long time, simplifies operation.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of this slow-release oxone；
Fig. 2 is influence diagram of the concentration to the aperture in the duct of inner layer film clothing of pore-foaming agent；
Fig. 3 is influence diagram of the concentration to potassium hydrogen persulfate burst size of pore-foaming agent；
Fig. 4 is influence diagram of the number of plies to the thickness of inner layer film clothing of inner layer film clothing；
Fig. 5 is influence diagram of the number of plies to potassium hydrogen persulfate burst size of inner layer film clothing；
Fig. 6 is the test chart of the thermal stability of this slow-release oxone.
Wherein: carrying pill core 1；Inner layer film clothing 2；Outer membrane clothing 3.
Specific embodiment
In order to which technical characteristic of the invention, purpose and beneficial effect are more clearly understood, now to skill of the invention
Art scheme carries out described further below, but should not be understood as that limiting the scope of the invention.
The present invention is the ingredient for being analyzed as follows the experimental result of influence factor to determine this buffer-type oxone
Proportion and preparation condition.
One, influence of the pore-foaming agent concentration to fat-soluble membrane aperture size
Pore-foaming agent selects Polyethylene glycol-2000, using Polyethylene glycol-2000 concentration as single argument factor, setting 1g/100mL,
Five concentration groups of 2g/100mL, 3g/100mL, 4g/100mL and 5g/100mL, the quality of 2 remaining raw material components of inner layer film clothing
It is constant are as follows: ethyl cellulose 15g, triethyl citrate 3g and dehydrated alcohol 100mL (80g).By the poly- of above-mentioned various concentration group
The inner layer film clothing 2 that ethylene glycol -2000 synthesizes, direct electricity consumption sem observation, as a result as shown in Fig. 2, with Polyethylene glycol-2000 concentration
Raising, aperture increases of micropore in inner layer film clothing 2, and Polyethylene glycol-2000 concentration is higher, the rate of aperture increases is bigger.
Two, influence of the pore-foaming agent concentration to potassium hydrogen persulfate burst size
Pore-foaming agent selects Polyethylene glycol-2000, using Polyethylene glycol-2000 concentration as single argument factor, setting 1g/100mL,
Five concentration groups of 2g/100mL, 3g/100mL, 4g/100mL and 5g/100mL, the quality of 2 remaining raw material components of inner layer film clothing
It is constant are as follows: ethyl cellulose 15g, triethyl citrate 3g and dehydrated alcohol 100mL (80g).By the poly- of above-mentioned various concentration group
The inner layer film clothing 2 that ethylene glycol -2000 synthesizes, and after being made into slow-release oxone, it puts into water and tests, as a result as schemed
Shown in 3, potassium hydrogen persulfate burst size is increasing over time, and pore-foaming agent concentration is higher, persulfuric acid in same time
Hydrogen Potassium release amount is more, and potassium hydrogen persulfate rate of release is faster.When the concentration of Polyethylene glycol-2000 reaches 5g/100mL
When, manufactured slow-release oxone, which enters in water to be no more than 10 hours, to be just disintegrated.
Three, influence of the thickness of inner layer film clothing to potassium hydrogen persulfate burst size
Using the thickness of inner layer film clothing 2 as single argument factor, time that pill core 1 impregnates inner layer film clothing solution is carried by control
Number, control is wrapped in the number of plies for carrying the inner layer film clothing 2 outside pill core 1, and then adjusts the thickness of inner layer film clothing 2, and setting is wrapped in
The number of plies for carrying the inner layer film clothing 2 outside pill core 1 is 1~6 layer.The quality of 2 each raw material component of inner layer film clothing are as follows: ethyl cellulose
15g, triethyl citrate 3g, Polyethylene glycol-2000 4g and dehydrated alcohol 100mL (80g).By load pill core 1 obtained according to
The number of plies of the inner layer film clothing 2 of above-mentioned setting is wrapped up, and after being finally made slow-release oxone, is put into water and is surveyed
As a result as shown in Figure 4, Figure 5 examination carries the every immersion of pill core 1 once, the thickness of the inner layer film clothing 2 of surface package is each about
0.10mm；The number of plies of inner layer film clothing 2 is only that 1 layer of slow-release oxone enters to be no more than in water and just collapses for 10 hours
Solution；Over time, potassium hydrogen persulfate burst size is more and more, the inner layer film clothing 2 of slow-release oxone
The number of plies number of plies is more, and thickness is thicker, and the burst size of potassium hydrogen persulfate is fewer in same time, and potassium hydrogen persulfate rate of release is got over
Slowly.
Four, the thermal stability of this slow-release oxone
This slow-release oxone is put into baking oven, respectively with 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C are placed
4 hours, then put it into water 10 hours, the case where observing sulfate ion release.As a result as shown in fig. 6,20 DEG C~
30 DEG C or so potassium hydrogen persulfates are still undecomposed, start slowly to decompose at 40 DEG C, decompose at 60 DEG C and slow down, close to dividing completely
Solution.
Five, the detection method of potassium hydrogen persulfate difference burst size
Since potassium hydrogen persulfate will resolve into potassium sulfate and potassium acid sulfate at 30 DEG C or more, so design will release
A period of time is boiled in potassium hydrogen persulfate heating, and suitable sodium hydroxide is added, and makes its complete decomposition and inversion at sulfate ion
Sulfate ion is surveyed further according to the gravimetric method described in State Environmental Protection Administration " water and effluent monitoring analysis method " fourth edition
Measure the amount of sulfate ion.Potassium hydrogen persulfate is finally calculated by the conversion of sulphur atom in barium sulfate and potassium hydrogen persulfate again
The quality discharged respectively.
This slow-release oxone measure of merit:
One, sterilizing ability is tested
Embodiment 1
(1) ingredient and proportion of slow-release oxone: the mass ratio of 1 each raw material component of pill core is carried are as follows: mistake
Potassium acid sulfate 0.5: starch 15: sucrose 4: sodium carboxymethylcellulose 0.05: water 5；The mass ratio of 2 each raw material component of inner layer film clothing
Are as follows: ethyl cellulose 15: triethyl citrate 3: Polyethylene glycol-2000 4: dehydrated alcohol 80；3 each raw material component of outer membrane clothing
Mass ratio are as follows: hydroxypropyl methyl cellulose 5: polyethylene glycol-400 5: potassium hydrogen persulfate 2: water 100.
(2) slow-release oxone is prepared:
1. production carries pill core 1: sucrose and sodium carboxymethylcellulose is soluble in water, mixed liquor A is obtained, by hydrogen persulfate
After potassium and starch mixing, it is dried after sufficiently being mixed with mixed liquor A, obtains and carry pill core 1；
2. synthesis inner layer film clothing solution: ethyl cellulose being added to absolute ethanol, heating water bath is carried out, is stirred, is added
Triethyl citrate and Polyethylene glycol-2000, stirring to ethyl cellulose are dissolved, and inner layer film clothing solution is obtained；
3. synthesis outer membrane clothing solution: hydroxypropyl methyl cellulose and potassium hydrogen persulfate being added to the water, water-bath is carried out and adds
Heat adds polyethylene glycol-400, and stirring to hydroxypropyl methyl cellulose is dissolved, and obtains outer membrane clothing solution；
4. coating: load pill core 1 is dipped to repeatedly in inner layer film clothing solution, is taken out, then be dipped to outer membrane clothing repeatedly
It in solution, shakes, filter after taking-up, carry out vacuum drying treatment to constant weight, obtain slow-release oxone.
Embodiment 2
The ingredient and proportion of preparation, specific preparation step repeat embodiment 1, unlike: carry the hydrogen persulfate of pill core 1
The mass ratio of potassium is 1.
Embodiment 3
The ingredient and proportion of preparation, specific preparation step repeat embodiment 1, unlike: carry the hydrogen persulfate of pill core 1
The mass ratio of potassium is 1.5.
Embodiment 4
The ingredient and proportion of preparation, specific preparation step repeat embodiment 1, unlike: carry the hydrogen persulfate of pill core 1
The mass ratio of potassium is 3.
Embodiment 5
The ingredient and proportion of preparation, specific preparation step repeat embodiment 1, unlike: carry the hydrogen persulfate of pill core 1
The mass ratio of potassium is 6.
5 kinds of slow-release oxones for preparing above-described embodiment 1~5, carry out following sterilizing ability test:
(1) prepare bacteria suspension: choosing staphylococcus aureus, Escherichia coli, hemolytic streptococcus is test organisms.Take each jelly
Dry strain by Zengjing Granule, isolates and purifies, and typical single bacterium colony is selected to be seeded in broth medium, 37 DEG C of cultures
After 24 hours, with the normal saline dilution of tryptone containing 1g/L at test bacteria suspension.
(2) sterilization test: test carries out under room temperature (20 DEG C~25 DEG C).100mL bacteria suspension and 900mL sterile water are mixed
It closes uniformly, forms 1L experimental liquid.Above-mentioned 5 kinds of slow-release oxones are knocked down respectively in above-mentioned 1L experimental liquid, are acted on
10 minutes.The experimental liquid 1.0mL after answering is negated, addition is equipped in 9.0mL neutralizer test tube and mixes, neutralization 10min.Through filling
Divide after mixing, sampling liquid inoculation, count plate culture calculates killing logarithm.Experiment is repeated 3 times, and is averaging and is killed logarithm.
(3) result: it is shown in Table 1.5 kinds of slow-release oxones are to Escherichia coli, staphylococcus aureus and molten
Hemorrhagic streptococcus has apparent bactericidal effect, and potassium hydrogen persulfate effective concentration is killed in the concentration range of 3g/L~6g/L
Bacterium better effect.
Table 1 averagely kills logarithm
| Test strain | Test serial number | Active constituent content (mg/L) | Averagely kill logarithm |
| Escherichia coli | Embodiment 1 | 500 | 4.02 |
| Escherichia coli | Embodiment 2 | 1000 | 5.08 |
| Escherichia coli | Embodiment 3 | 1500 | 5.79 |
| Escherichia coli | Embodiment 4 | 3000 | 6.34 |
| Escherichia coli | Embodiment 5 | 6000 | 6.69 |
| Staphylococcus aureus | Embodiment 1 | 500 | 4.09 |
| Staphylococcus aureus | Embodiment 2 | 1000 | 5.16 |
| Staphylococcus aureus | Embodiment 3 | 1500 | 5.87 |
| Staphylococcus aureus | Embodiment 4 | 3000 | 6.47 |
| Staphylococcus aureus | Embodiment 5 | 6000 | 6.79 |
| Hemolytic streptococcus | Embodiment 1 | 500 | 4.14 |
| Hemolytic streptococcus | Embodiment 2 | 1000 | 5.21 |
| Hemolytic streptococcus | Embodiment 3 | 1500 | 5.92 |
| Hemolytic streptococcus | Embodiment 4 | 3000 | 6.51 |
| Hemolytic streptococcus | Embodiment 5 | 6000 | 6.98 |
Two, the test of the burst size of the potassium hydrogen persulfate of slow-release oxone
The reaction kettle of the intelligent digestion instrument equipped with 1L water is placed according to slow-release oxone made from embodiment 5
It is interior, the dissolution rate of preparation is tested.Every taking out 5ml dissolution fluid in the corresponding time, its concentration is measured, and mend in time
Fill corresponding solvent.Each time point retest 4 times, until the dissolution rate detection in all time points terminates, it finally will be molten
Out-degree is scaled the burst size of potassium hydrogen persulfate.The results are shown in Table 2,4 parallel result differences of each time point measurement
Less, illustrate that the sustained release performance of this preparation is stablized, and along the propulsion of time, this preparation sustained release goes out potassium hydrogen persulfate, it is real
Now to effective sustained release of potassium hydrogen persulfate.
The burst size of 2 potassium hydrogen persulfate of table
Three, the sewage purification aptitude tests of slow-release oxone
It is placed in the beaker of the sewage equipped with 500mL according to slow-release oxone made from embodiment 5,10 points
The turbidity of solution is substantially reduced after clock, and in the subsequent sewage that 500mL was added into container every 30 minutes, and subsequent
Its turbidity is observed within 10 minutes, until sewage load reaches 2000mL and stops experiment.In this experiment, sewage is added every time
It is substantially reduced when 10 minutes its turbidities are more just added afterwards.Thus illustrate, this preparation can remain pair in a longer period of time
The detergent power of sewage.
The present invention provides a kind of slow-release oxone, as shown in Figure 1, from the inside to the outside successively including carrying pill core
1, inner layer film clothing 2 and outer membrane clothing 3；The thickness of inner layer film clothing 2 is greater than 0.1mm, and outer membrane clothing 3 accounts for slow-release potassium hydrogen persulfate system
Agent gross mass percentage 0.1%~0.5%；
Carry pill core 1 raw material components include potassium hydrogen persulfate, filler, No.1 plasticizer, sodium carboxymethylcellulose and
Water carries the mass ratio of 1 each raw material component of pill core are as follows: potassium hydrogen persulfate 3~7: filler 14~16: No.1 plasticizer 3~5:
Sodium carboxymethylcellulose 0.01~0.1: water 4~8, No.1 plasticizer are water-soluble plasticizer；
The raw material components of inner layer film clothing 2 include ethyl cellulose, No. two plasticizer, pore-foaming agent and organic solvent, inner layer film
The mass ratio of 2 each raw material component of clothing are as follows: 12~18: No. two plasticizer 2~4 of ethyl cellulose: pore-foaming agent 3~5: organic solvent 75
~85, No. two plasticizer are fat-soluble plasticizer；
The raw material components of outer membrane clothing 3 include hydroxypropyl methyl cellulose, No. three plasticizer, potassium hydrogen persulfate and water, outside
The mass ratio of 3 each raw material component of tunic clothing are as follows: 4~6: No. three plasticizer 4~6 of hydroxypropyl methyl cellulose: potassium hydrogen persulfate 1~
3: water 80~120, No. three plasticizer are water-soluble plasticizer.
Potassium hydrogen persulfate is made load pill core 1 and wraps up two different coatings by the present invention, to achieve the purpose that sustained release.It is interior
Tunic clothing 2 adds No. two plasticizer, pore-foaming agent and organic solvent using ethyl cellulose as slow-release material, is made with one
Determine the fat-soluble coating in duct；Outer membrane clothing 3 adds No. three plasticizer, mistakes using hydroxypropyl methyl cellulose as slow-release material
The water-soluble coating containing potassium hydrogen persulfate is made in potassium acid sulfate and water.
The thickness of inner layer film clothing 2 is too thin, and inner layer film clothing 2 can rupture in disintegration in a short time, and the slow releasing function time is too short,
Thus setting inner layer film clothing 2 thickness be greater than 0.1mm, can slow release potassium hydrogen persulfate and extend its sustained release time；
Outer membrane clothing 3 only accounts for the 0.1%~0.5% of this slow-release oxone gross mass percentage, and very thin thickness allows this
Slow-release oxone, which is not knocked down, to be played the role of before water body maintaining preparation stability, also allows this slow-release persulfuric acid
Hydrogen potassium preparation can dissolve in a short time after knocking down water body, and exposure inner layer film clothing 2 realizes the sustained release of effective component.
Ethyl cellulose, have it is fat-soluble, have the effects that film forming, bonding, fill.Because ethyl cellulose dissolves in nothing
Water-ethanol avoids the residual of toxic solvent from causing secondary pollution to water body without using volatility and hypertoxicity solvent.It is not
It is dissolved in water, property is stablized, is unlikely to deteriorate, cold resistance, salt tolerant, resistance to good hygroscopicity, is not had to worry that it is rotten with the preparation of its package
The problem of, less with the potassium hydrogen persulfate problem apt to deteriorate for worrying to carry in pill core 1, slow-release material can be worked as, and can be with
Protection carries pill core 1, dual-purpose at one stroke.
Hydroxypropyl methyl cellulose has water solubility, is readily dispersed in hot water but is not directly dissolved in hot water, and water is slow to the cold
Slow swelling.Since it has relatively good thickening capabilities, stability, film forming, water-retaining property is water-soluble under given conditions,
It is improved well by the stability for the preparation that it is wrapped up, preparation is made to be easy to store.
Hydroxypropyl methyl cellulose has been selected in outer membrane clothing 3, has selected ethyl cellulose in inner layer film clothing 2, so that carrying
After pill core 1 is wrapped up via above-mentioned outer membrane clothing 3 and inner layer film clothing 2, the stability of preparation entirety is improved, and is solved conventional
Oxone problem apt to deteriorate.
It being placed in water after potassium hydrogen persulfate is by above two coating package, outer membrane clothing 3 is contacted with water at first, due to
Outer membrane clothing 3 has water solubility, meets water dissolution, releases the potassium hydrogen persulfate contained in outer membrane clothing 3, can play to water body
Disinfection, purification the effects of.After outer membrane clothing 3 is completely dissolved, inner layer film clothing 2 is contacted with water, due to the ethyl of inner layer film clothing 2
Cellulose is fat soluble materials, and it is insoluble to meet water, and the pore-foaming agent in inner layer film clothing 2 is water-soluble material, meets water dissolution, thus energy
Duct is formed in inner layer film clothing 2, the potassium hydrogen persulfate carried in pill core 1 was gradually released by the duct of inner layer film clothing 2
Potassium acid sulfate achievees the purpose that be sustained potassium hydrogen persulfate.On the basis of the selection of above-mentioned slow-release oxone, adjustment
The content of core material potassium hydrogen persulfate, the concentration of pore-foaming agent, the thickness of inner layer film clothing 2, outer membrane clothing 3 account for gross mass percentage,
The content of 3 potassium hydrogen persulfate of outer membrane clothing, can achieve effective control the rate of release of potassium hydrogen persulfate.It is existing to solve
Oxone the problem of being unable to control activity and action time.
And since this slow-release oxone can control the rate of release of potassium hydrogen persulfate, control hydrogen persulfate
Potassium release concentration can persistently play the effects of disinfection to water body, purification whithin a period of time, to extend potassium hydrogen persulfate
Effective reaction time, not only can maximum save the cost, but also good treatment effect can be played；So that treatment process
In, without going the amount for launching potassium hydrogen persulfate in control water in the time that said preparation also can more be grown at one to be on time daily
The state for reacting balance, solves the problems, such as that the cumbersome of conventional formulation, treatment effect are bad, processing cost is high.
As the mass ratio of pore-foaming agent in inner layer film clothing 2 increases in a certain range, the aperture in 2 duct of inner layer film clothing increases
Greatly, the number in duct increases, and the burst size of potassium hydrogen persulfate will be more in same time, whole hydrogen persulfate Potassium release speed
Rate will be faster；For the mass ratio of pore-foaming agent beyond after certain range, pore-foaming agent is excessive in inner layer film clothing 2, and inner layer film clothing 2 is easy
Disintegration rupture.When mass ratio of the pore-foaming agent in inner layer film clothing 2 is greater than 3, the diameter in the duct that inner layer film clothing 2 is formed is obvious
Increase, the rate of release of potassium hydrogen persulfate is obviously accelerated；When mass ratio of the pore-foaming agent in inner layer film clothing 2 is greater than 5, it is no more than
The disintegration rupture of inner layer film clothing 2 in 10 hours, therefore mass ratio of the pore-foaming agent in inner layer film clothing 2 selects between 3~5.
Preferably, No.1 plasticizer is sucrose, and No. two plasticizer are triethyl citrate, and No. three plasticizer are poly- second two
Alcohol -400.
Sucrose is a kind of low voc compounds, has good water solubility, as the plasticizer for carrying pill core 1, uses water
It after being dissolved into sucrose solution, comes into full contact with and mixes with the bulk composition for carrying pill core 1, can increase the body force for carrying pill core 1
Learn performance, permeance property.
Triethyl citrate has fat-soluble, has good fungus resistance and an oil resistivity, less toxic environmental sound, as
The plasticizer of inner layer film clothing 2 improves the flexibility of inner layer film clothing 2, and ethyl cellulose can be assisted to form one layer of more stable packet
Clothing, it is ensured that the sustained release performance of inner layer film clothing 2.
Polyethylene glycol-400 has water-soluble and fixedness, less toxic environmental sound, the plasticising as outer membrane clothing 3
Agent can properly increase the mechanical property of outer membrane clothing 3, effectively hydroxypropyl methyl cellulose is assisted to form stable coating, make to carry
Pill core 1 is not easily susceptible to steam interference, improves preparation overall stability.
Preferably, pore-foaming agent is Polyethylene glycol-2000, and organic solvent is dehydrated alcohol, and filler is starch.
Contain water-soluble pore-foaming agent particle in fat-soluble inner layer film clothing 2, is wrapped up when carrying pill core 1 by inner layer film clothing 2
It is contacted afterwards with water, since inner layer film clothing 2 is not soluble in water, and pore-foaming agent can be dissolved in water and leave aperture, carry pill core 1 to realize
Potassium hydrogen persulfate be gradually released into water by duct.And water-soluble pore-foaming agent can preferably cause micro hole, solid
Grain is easily dispersed uniformly, by forming the Polyethylene glycol-2000 in certain duct in stirring, be soluble in ethyl cellulose
Water does not dissolve in organic solvent, and function and effect are good, and cheap.
Organic solvent for dissolving fat-soluble ethyl cellulose, in order to enable this preparation using it is safer, avoid to water
Inner layer film clothing is made after promoting ethyl cellulose to dissolve as organic solvent in the secondary pollution of body, preferably nontoxic dehydrated alcohol
2。
Filler is the main material for carrying pill core 1 other than potassium hydrogen persulfate, is the skeleton for supporting this load pill core 1
Material is preferably starch, and starch is readily available materials, cheap, is a kind of good harmless filler.It will
Starch and hydrogen persulfate k particle mix, and potassium hydrogen persulfate is distributed in around starch, pass through inner layer film clothing 2 when carrying pill core 1
Duct and water when contacting, starch is gradually dissolved in the water, while gradually exposing hydrogen persulfate k particle, hydrogen persulfate k particle
Water dissolution is met, the stress efficacy of this preparation is played.
Preferably, inner layer film clothing 2 with a thickness of 0.2mm, outer membrane clothing 3 accounts for slow-release oxone gross mass hundred
Divide ratio 0.2%.
The thickness of inner layer film clothing 2 is higher, and the burst size of potassium hydrogen persulfate is fewer in same time, hydrogen persulfate Potassium release
Rate is slower.When the thickness of the inner layer film clothing 2 of this preparation is less than 0.2mm, thickness is too thin, is no more than 10 hours inner layer film clothing 2
Disintegration rupture；The inner layer film clothing 2 of this preparation with a thickness of 0.2mm when, effect is not disintegrated for 50 hours, and hydrogen persulfate K released
Amount is all big compared to the burst size of other thickness of inner layer film clothing 2.
Outer membrane clothing 3 only accounts for the 0.2% of this slow-release oxone gross mass percentage, and very thin thickness allows
This slow-release oxone, which is not knocked down, to be played the role of before water body maintaining preparation stability, also allows this slow-release over cure
Potassium hydrogen phthalate preparation can dissolve in a short time after knocking down water body, and exposure inner layer film clothing 2 realizes the sustained release of effective component.
Preferably, the raw material components for carrying pill core 1 include potassium hydrogen persulfate, filler, No.1 plasticizer, carboxymethyl cellulose
Plain sodium and water carry the mass ratio of 1 each raw material component of pill core are as follows: potassium hydrogen persulfate 6: filler 15: No.1 plasticizer 4: carboxylic first
Base sodium cellulosate 0.05: water 5；
The raw material components of inner layer film clothing 2 include ethyl cellulose, No. two plasticizer, pore-foaming agent and organic solvent, inner layer film
The mass ratio of 2 each raw material component of clothing are as follows: 15: No. two plasticizer 3 of ethyl cellulose: pore-foaming agent 4: organic solvent 80；
The raw material components of outer membrane clothing 3 include hydroxypropyl methyl cellulose, No. three plasticizer, potassium hydrogen persulfate and water, outside
The mass ratio of 3 each component of tunic clothing are as follows: 5: No. three plasticizer 5 of hydroxypropyl methyl cellulose: potassium hydrogen persulfate 2: water 100.
As the mass ratio of pore-foaming agent in inner layer film clothing 2 increases in a certain range, the aperture in 2 duct of inner layer film clothing increases
Greatly, the number in duct increases, and the burst size of potassium hydrogen persulfate will be more in same time, whole hydrogen persulfate Potassium release speed
Rate will be faster.When mass ratio of the pore-foaming agent in inner layer film clothing 2 is 4, under the premise of effect is not disintegrated for 50 hours, over cure
The burst size of potassium hydrogen phthalate is maximum.
The present invention also provides a kind of preparation methods of slow-release oxone, comprising the following steps:
(1) production carries pill core 1: No.1 plasticizer and sodium carboxymethylcellulose is soluble in water, mixed liquor A is obtained, and it will
After potassium hydrogen persulfate and filler mixing, it is dried after sufficiently being mixed with mixed liquor A, obtains and carry pill core 1；
(2) it synthesizes inner layer film clothing solution: ethyl cellulose is added in organic solvent, carry out heating water bath, stir, be added
No. two plasticizer and pore-foaming agent, stirring to ethyl cellulose are dissolved, and inner layer film clothing solution is obtained；
(3) it synthesizes outer membrane clothing solution: hydroxypropyl methyl cellulose and potassium hydrogen persulfate is added to the water, carry out water-bath and add
Heat adds No. three plasticizer, and stirring to hydroxypropyl methyl cellulose is dissolved, and obtains outer membrane clothing solution；
(4) coating: being repeatedly dipped to load pill core 1 in inner layer film clothing solution, takes out, then be dipped to outer membrane clothing repeatedly
It in solution, shakes, filter after taking-up, carry out vacuum drying treatment to constant weight, obtain slow-release oxone.
It carries potassium hydrogen persulfate and filler in pill core 1 to mix, skeleton structure of the filler as load pill core 1, so that
Potassium hydrogen persulfate distribution of particles meets water and gradually releases potassium hydrogen persulfate around filler；And mix No.1 plasticizer, carboxylic
Sodium carboxymethylcellulose pyce and water, enhancing carry the mechanical strength of pill core 1, are easy to moulding.
Sustained release material ethyl cellulose and No. two plasticizer in inner layer film clothing 2 are liposoluble substance, are needed using having
Solvent is dissolved, and heating stirring is needed in course of dissolution, promotes ethyl cellulose sufficiently to dissolve, the pore being added thereafter
Agent is water-soluble substances, does not dissolve in organic solvent, and retains its original solid particle forms and be distributed in liquid, to compared with indissoluble
The ethyl cellulose of solution sufficiently dissolves.
Sustained release material hydroxypropyl methyl cellulose in outer membrane clothing 3 is water-soluble substances, can be in the condition of heating stirring
Under be dissolved in water；And water-soluble No. three plasticizer are added and increase the whole mechanical strength of outer membrane clothing 3, it is easy to moulding；It is added
Suitable potassium hydrogen persulfate provides starting burst size, the effect effect at stabilization formulations initial stage before contacting for this load pill core 1 with water
Can, it is sufficiently dissolved to less soluble hydroxypropyl methyl cellulose.
It by above-mentioned steps, obtains and carries pill core 1, inner layer film clothing solution and outer membrane clothing solution, carry pill core 1 first repeatedly
It is dipped in inner layer film clothing solution, adjusts the thickness of inner layer film clothing 2 by controlling the number of its immersion, then will be enclosed with interior
The load pill core 1 of tunic clothing 2 is dipped to repeatedly in outer membrane clothing solution, adjusts outer membrane clothing by controlling the number of its immersion
3 account for the percentage of this slow-release oxone gross mass, then shake, to be filtered to remove 3 outer surface of outer membrane clothing extra
Solution, drying and dehydrating avoid this preparation from leading to rotten problem since moisture is high.
Preferably, step (2) synthesizes inner layer film clothing solution: ethyl cellulose being added in organic solvent, water-bath is carried out and adds
No. two plasticizer are added in heat while stirring, after stirring 30 minutes, pore-foaming agent are added, after stirring is completely dissolved to ethyl cellulose
It keeps standing 10 minutes under heating water bath state, obtains inner layer film clothing solution；
Step (3) synthesizes outer membrane clothing solution: hydroxypropyl methyl cellulose and potassium hydrogen persulfate being added to the water, water is carried out
Bath heating, adds No. three plasticizer, keeps heating water bath to stir 30 minutes, is stirred under room temperature to hydroxypropyl methyl fiber
Element is completely dissolved, and stands 10 minutes under room temperature, obtains outer membrane clothing solution.
By experiment repeatedly, ethyl cellulose persistently stirs 30 minutes in warm water and is just easy dissolution sufficiently；Hydroxypropyl
Methylcellulose persistently stirs 30 minutes in warm water, is then cooled to after room temperature under conditions of continuing stirring, is just easy dissolution
Sufficiently.Ethyl cellulose and hydroxypropyl methyl cellulose can generate bubble, the presence of bubble during lasting stirring and dissolving
It will affect the inner layer film clothing 2 of synthesis and the quality of outer membrane clothing 3, thus, it is filled in ethyl cellulose and hydroxypropyl methyl cellulose
After dividing dissolution, 10 minutes will be stood under the conditions of original temperature, bubble is allowed to naturally drain, improve the inner layer film clothing 2 of synthesis
With the quality of outer membrane clothing 3.
Preferably, it is 2~6 times that pill core 1 is carried in step (4) to impregnate the number of inner layer film clothing solution, package in step (4)
The number for carrying the immersion outer membrane clothing solution of pill core 1 for having inner layer film clothing 2 is 2~3 times.
It carries pill core 1 to be first dipped to repeatedly in inner layer film clothing solution, the number that pill core 1 impregnates is carried by control to adjust
Then the load pill core 1 for being enclosed with inner layer film clothing 2 is dipped in outer membrane clothing solution repeatedly, passes through by the thickness of inner layer film clothing 2
The number of its immersion is controlled to adjust the percentage that outer membrane clothing 3 accounts for this slow-release oxone gross mass.
Measured, carry inner layer film clothing solution of the every immersion of pill core 1, increased inner layer film clothing 2 with a thickness of
0.10mm impregnates 2~6 times, then obtains 0.2mm~0.60mm thickness inner layer film clothing 2；When the thickness of inner layer film clothing 2 is less than 0.2mm
When, thickness is too thin, is no more than the disintegration rupture of inner layer film clothing 2 in 10 hours；When the thickness of inner layer film clothing 2 is greater than 0.60mm,
Thickness is too thick, and hydrogen persulfate K released is too slow, and effect obviously weakens, therefore carries pill core 1 and be dipped to inner layer film clothing solution 2~6 times
It is advisable.
Through measuring, the load pill core 1 for being enclosed with inner layer film clothing 2 is impregnated into 2~3 outer membrane clothing solution, outer membrane clothing 3 accounts for
The 0.2%~0.3% of this slow-release oxone gross mass percentage, very thin thickness allow this slow-release persulfuric acid
Hydrogen potassium preparation plays the role of maintaining preparation stability before not knocking down water body, this slow-release oxone is also allowed to be knocked down
It can be dissolved in a short time after water body, exposure inner layer film clothing 2 realizes the sustained release of effective component.
Preferably, it is 2 times that pill core 1 is carried in step (4) to impregnate the number of inner layer film clothing solution, and step is enclosed in (4)
The number for carrying the immersion outer membrane clothing solution of pill core 1 of inner layer film clothing 2 is 2 times.
Carrying pill core 1 to impregnate the number of inner layer film clothing solution is 2 times, then the inner layer film clothing 2 obtained with a thickness of 0.2mm,
Effect is not disintegrated for 50 hours, and potassium hydrogen persulfate burst size is all big compared to the burst size of other thickness of inner layer film clothing 2.It is enclosed with
The number for carrying the immersion outer membrane clothing solution of pill core 1 of inner layer film clothing 2 is 2 times, then the outer membrane clothing 3 obtained accounts for this slow-release mistake
The 0.2% of potassium acid sulfate preparation gross mass percentage, very thin thickness can combine the stability of this preparation and realize sustained release
Effect.
Preferably, step (2) and the condition of the heating water bath in step (3) are not higher than 60 DEG C, step (1) and step
(4) drying temperature in is not higher than 30 degrees Celsius.
Ethyl cellulose and hydroxypropyl methyl cellulose only will disperse in the hot water higher than 60 DEG C, but solubility property becomes
Difference influences the abundant dissolution of ethyl cellulose and hydroxypropyl methyl cellulose, therefore the condition of heating water bath is not higher than 60 DEG C.It crosses
Potassium acid sulfate will resolve into potassium sulfate and potassium acid sulfate at 30 DEG C or more, not divide yet in 20 DEG C~30 DEG C or so potassium hydrogen persulfates
Solution, starts slowly to decompose at 40 DEG C, decomposes at 60 DEG C and slows down, and decomposes close to complete, so this slow-release potassium hydrogen persulfate
The drying temperature of preparation should not be higher than 30 DEG C.
The technical principle of the invention is described above in combination with a specific embodiment.These descriptions are intended merely to explain of the invention
Principle, and shall not be construed in any way as a limitation of the scope of protection of the invention.Based on the explanation herein, the technology of this field
Personnel can associate with other specific embodiments of the invention without creative labor, these modes are fallen within
Within protection scope of the present invention.
Claims (10)
1. a kind of slow-release oxone, which is characterized in that from the inside to the outside successively include carry pill core, inner layer film clothing and
Outer membrane clothing；The thickness of the inner layer film clothing is greater than 0.1mm, and it is total that the outer membrane clothing accounts for the slow-release oxone
Mass percent 0.1%~0.5%；
It is described carry pill core raw material components include potassium hydrogen persulfate, filler, No.1 plasticizer, sodium carboxymethylcellulose and
Water, the mass ratio for carrying pill core each raw material component are as follows: potassium hydrogen persulfate 3~7: filler 14~16: No.1 plasticizer 3~
5: sodium carboxymethylcellulose 0.01~0.1: water 4~8, the No.1 plasticizer are water-soluble plasticizer；
The raw material components of the inner layer film clothing include ethyl cellulose, No. two plasticizer, pore-foaming agent and organic solvent, the internal layer
The mass ratio of film clothing each raw material component are as follows: 12~18: No. two plasticizer 2~4 of ethyl cellulose: pore-foaming agent 3~5: organic solvent
75~85, No. two plasticizer are fat-soluble plasticizer；
The raw material components of the outer membrane clothing include hydroxypropyl methyl cellulose, No. three plasticizer, potassium hydrogen persulfate and water, described
The mass ratio of outer membrane clothing each raw material component are as follows: 4~6: No. three plasticizer 4~6 of hydroxypropyl methyl cellulose: potassium hydrogen persulfate 1
~3: water 80~120, No. three plasticizer are water-soluble plasticizer.
2. slow-release oxone according to claim 1, which is characterized in that the No.1 plasticizer is sugarcane
Sugar, No. two plasticizer are triethyl citrate, and No. three plasticizer are polyethylene glycol-400.
3. slow-release oxone according to claim 1, which is characterized in that the pore-foaming agent is poly- second two
Alcohol -2000, the organic solvent are dehydrated alcohol, and the filler is starch.
4. slow-release oxone according to claim 1, which is characterized in that the inner layer film clothing with a thickness of
0.2mm, the outer membrane clothing account for the slow-release oxone gross mass percentage 0.2%.
5. slow-release oxone according to claim 1, which is characterized in that the raw material group for carrying pill core
Divide includes potassium hydrogen persulfate, filler, No.1 plasticizer, sodium carboxymethylcellulose and water, the load pill core each raw material component
Mass ratio are as follows: potassium hydrogen persulfate 6: filler 15: No.1 plasticizer 4: sodium carboxymethylcellulose 0.05: water 5；
The raw material components of the inner layer film clothing include ethyl cellulose, No. two plasticizer, pore-foaming agent and organic solvent, the internal layer
The mass ratio of film clothing each raw material component are as follows: 15: No. two plasticizer 3 of ethyl cellulose: pore-foaming agent 4: organic solvent 80；
The raw material components of the outer membrane clothing include hydroxypropyl methyl cellulose, No. three plasticizer, potassium hydrogen persulfate and water, described
The mass ratio of outer membrane clothing each component are as follows: 5: No. three plasticizer 5 of hydroxypropyl methyl cellulose: potassium hydrogen persulfate 2: water 100.
6. a kind of preparation method of slow-release oxone described in -5 any bars according to claim 1, feature exist
In, comprising the following steps:
(1) production carries pill core: No.1 plasticizer and sodium carboxymethylcellulose is soluble in water, mixed liquor A is obtained, by persulfuric acid
After hydrogen potassium and filler mixing, it is dried after sufficiently being mixed with mixed liquor A, obtains and carry pill core；
(2) it synthesizes inner layer film clothing solution: ethyl cellulose is added in organic solvent, carry out heating water bath, stirring is added No. two
Plasticizer and pore-foaming agent, stirring to ethyl cellulose are dissolved, and inner layer film clothing solution is obtained；
(3) it synthesizes outer membrane clothing solution: hydroxypropyl methyl cellulose and potassium hydrogen persulfate is added to the water, carry out heating water bath,
No. three plasticizer are added, stirring to hydroxypropyl methyl cellulose is dissolved, and outer membrane clothing solution is obtained；
(4) coating: being repeatedly dipped to load pill core in inner layer film clothing solution, takes out, then be dipped to outer membrane clothing solution repeatedly
In, it shakes, filter after taking-up, carry out vacuum drying treatment to constant weight, obtain slow-release oxone.
7. the preparation method of slow-release oxone according to claim 6, which is characterized in that the step
(2) it synthesizes inner layer film clothing solution: ethyl cellulose is added in organic solvent, carry out heating water bath, No. two are added while stirring
After stirring 30 minutes, pore-foaming agent is added in plasticizer, and stirring keeps quiet under heating water bath state after being completely dissolved to ethyl cellulose
It sets 10 minutes, obtains inner layer film clothing solution；
The step (3) synthesizes outer membrane clothing solution: hydroxypropyl methyl cellulose and potassium hydrogen persulfate being added to the water, water is carried out
Bath heating, adds No. three plasticizer, keeps heating water bath to stir 30 minutes, is stirred under room temperature to hydroxypropyl methyl fiber
Element is completely dissolved, and stands 10 minutes under room temperature, obtains outer membrane clothing solution.
8. the preparation method of slow-release oxone according to claim 6, which is characterized in that the step
(4) carrying pill core in impregnate the number of inner layer film clothing solution is 2~6 times, and the load medicine of inner layer film clothing is enclosed in the step (4)
The number that capsule core impregnates outer membrane clothing solution is 2~3 times.
9. the preparation method of slow-release oxone according to claim 8, which is characterized in that the step
(4) carrying pill core in impregnate the number of inner layer film clothing solution is 2 times, and the load pill of inner layer film clothing is enclosed in the step (4)
The number that core impregnates outer membrane clothing solution is 2 times.
10. the preparation method of slow-release oxone according to claim 6, which is characterized in that the step
(2) condition of the heating water bath and in the step (3) is not higher than 60 DEG C, dry in the step (1) and the step (4)
Dry temperature is not higher than 30 degrees Celsius.
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