CN103071436A - Preparation method for sustained release potassium permanganate microcapsule - Google Patents
Preparation method for sustained release potassium permanganate microcapsule Download PDFInfo
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- CN103071436A CN103071436A CN2013100476225A CN201310047622A CN103071436A CN 103071436 A CN103071436 A CN 103071436A CN 2013100476225 A CN2013100476225 A CN 2013100476225A CN 201310047622 A CN201310047622 A CN 201310047622A CN 103071436 A CN103071436 A CN 103071436A
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Abstract
The invention discloses a preparation method for a sustained release potassium permanganate microcapsule, comprising the following steps that (1), stearic acid is arranged in a reactor, absolute ethyl alcohol is added to the reactor, the reactor is heated in water bath, the solution in the reactor is sufficiently stirred until the stearic acid is completely dissolved; (2), polyethylene glycol 4000 and potassium permanganate are added to the reactor, potassium permanganate is homogeneously dispersed in the solution through ultrasound, the ultrasound is stopped, the solution is stirred and naturally cooled to the temperature of below 35 DEG C, and the reaction is finished after solid is completely dissolved out; and the mass ratio of potassium permanganate to stearic acid is 1:1-1:3. The preparation method for the sustained release potassium permanganate microcapsule solves the problems of low utilization rate of oxidant, high non-preference consumption and mass transfer of oxidant in the process of removing underground water pollutants by the in-situ chemical oxidation of liquid and powder potassium permanganate, and realizes the purposes of sustained release, effective transmission and efficient oxidation of the oxidant.
Description
[technical field]
The present invention relates to a kind of preparation method of the spacetabs type potassium permanganate microcapsules of repairing for underground water chloro-alkenes pollutant.
[background technology]
Along with socioeconomic development, a large amount of organic solvents are utilized by the mankind in practice, and these organic unreasonable discharging and inappropriate processing cause its entered environment and groundwater resources are polluted.Wherein chlorinated solvent (polyvinyl chloride-base) is because its density ratio water is large, belong to water-insoluble heavy-fluid (Dense Non-Aqueous Phase Liquid, DNAPL), easily to underground movement, thereby increased the contaminated depth ﹠ wideth of underground water and soil, so that the improvement reparation is very difficult, become the study hotspot that external soil and underground water pollution are repaired.Common dna PL pollutant has: the chlorohydrocarbon materials such as trichloro-ethylene (TCE), tetrachloro-ethylene (PCE), be widely used in the fields such as degreasing of aircraft engine, automobile component, electronic component and clothes, trichloro-ethylene (TCE), tetrachloro-ethylene (PCE) have the persistence characteristics in environment, very strong and have a carcinogenicity to the toxic action of biology, be put into EPA's priority pollutants, " blacklist " that Chinese environmental priority monitoring and control pollutant and European Union announce.
In situ chemical oxidation method (ISCO) is to think at present rehabilitating soil and the more effective technology of Organic Contamination of Groundwater, and when the contaminated site organic concentration was higher, its advantage was more obvious especially.Oxidant commonly used has H
2O
2, Fenton reagent, ozone and potassium permanganate.Wherein potassium permanganate is one of oxidant of mainly adopting of present original position repairing method, the strong (E of its oxidability
0=1.51V), cheap.Easy and simple to handle, its can oxidative degradation most of organic and inorganic pollution, and also the pH scope of using is wide.Studies show that permanganate can be used for the on the spot processing of chlorinated solvent (such as TCE, PCE) and petrochemical.There is on-the-spot TCE to pollute the case study of repairing in U.S. Kansas state (1996), Ohio state (1996,1997,1998).But potassium permanganate enters behind the soil nondirectional rapid dispersion with the form of the aqueous solution and consumes without selecting, so that the DNAPLs contaminated zone is the Oxidizer distribution of high oxidation agent demand band is not enough, thereby makes the utilization ratio of himself extremely low.Because the strong polarity in potassium permanganate surface makes it be difficult to spread out in non-polar solven, also cause the pollution repairing effect of DNAPLs poor in addition.For addressing this problem; some foreign study person adopts microcapsules technology; preparation spacetabs type potassium permanganate; on the one hand by increasing the time of contact of itself and DNAPLs the release time that prolongs oxidant; the potassium permanganate of microencapsulation is protected in the shell material on the other hand; reduce largely that other materials react in itself and the environment, improve its utilization rate.The oxidant particle type of service of microencapsulation is more extensive, can utilize fracturing to be pressed into the underground pollution district, also can be used as the reaction medium of in-situ chemical reaction wall.Therefore the introducing of microencapsulation technology is repaired the underground water chlorohydrocarbon for the Practical Project original position and is polluted significant.
[summary of the invention]
Technical problem to be solved by this invention is to provide a kind of preparation method of spacetabs type potassium permanganate microcapsules, has realized the slow release of oxidant, effectively transmission and the purpose such as efficient oxidation.
The present invention solves the problems of the technologies described above by the following technical programs: a kind of preparation method of spacetabs type potassium permanganate microcapsules may further comprise the steps:
(1) stearic acid is placed reactor, add absolute ethyl alcohol, heating water bath is stirred well to stearic acid and dissolves fully;
(2) add Macrogol 4000 and potassium permanganate, then the ultrasonic potassium permanganate Uniform Dispersion in solution that makes stops ultrasonicly and under agitation, naturally cools to below 35 ℃ again, treats that solid separates out fully, finishes reaction; Wherein, described potassium permanganate and stearic mass ratio are 1: 1-1: 3.
Further, described Macrogol 4000 and stearic mass ratio are 1: 2-1: 5.
Further, described absolute ethyl alcohol and stearic mass ratio are 1: 1.
Further, the temperature of described heating water bath is 70-80 ℃.
Further, the described ultrasonic time is 5-10min.
Further, electric blender is adopted in the stirring in the described step (2), and the speed that stirs is 150-350rpm.
Beneficial effect of the present invention is: the present invention passes through microcapsules technology, so that the potassium permanganate surface behind the microencapsulation becomes lipophile by hydrophily, make its easy dispersion in the organic solvents such as chlorohydrocarbon, increase the contact range of potassium permanganate oxidant and target contaminant, reduce without selecting and consume, improve the utilization of oxidant, thereby realize the slow release of oxidant, the effective purpose such as transmission and efficient oxidation.
[description of drawings]
The invention will be further described in conjunction with the embodiments with reference to the accompanying drawings.
Fig. 1 is the elution profiles of spacetabs type potassium permanganate microcapsules in water among the present invention.
Fig. 2 is that spacetabs type potassium permanganate microcapsules are illustrated to the continuation degraded situation of trichloro-ethylene among the present invention.
[specific embodiment]
1, a kind of preparation method of spacetabs type potassium permanganate microcapsules is characterized in that: may further comprise the steps:
(1) stearic acid is placed reactor, add absolute ethyl alcohol, at 70-80 ℃ of lower heating water bath, be stirred well to stearic acid and dissolve fully; With the shell material of stearic acid as spacetabs type potassium permanganate microcapsules.
(2) add again Macrogol 4000 and potassium permanganate, ultrasonic 5-10min makes potassium permanganate Uniform Dispersion in solution, then stop ultrasonic and under agitation, naturally cool to below 35 ℃, stearic acid solubility is reduced, condense take potassium permanganate as core and separate out, namely get spacetabs type potassium permanganate microcapsules, treat that solid separates out fully, finish reaction; Wherein, electric blender is adopted in the stirring in the described step (2), and the speed that stirs is 150-350rpm; Described potassium permanganate and stearic mass ratio are 1: 1-1: 3; Described Macrogol 4000 and stearic mass ratio are 1: 2-1: 5; Described absolute ethyl alcohol and stearic mass ratio are 1: 1.
Embodiment 1
Get the shell material stearic acid and place there-necked flask, add absolute ethyl alcohol, described absolute ethyl alcohol and stearic mass ratio are 1: 1; Fully stir with 350rpm, ℃ heating of control bath temperature to 70 is fully dissolved stearic acid; Macrogol 4000 in mass ratio again: stearic acid=1: 3, add Macrogol 4000 (PEG4000), then potassium permanganate in mass ratio: stearic acid=1: 1, add potassium permanganate, ultrasonic 10min makes potassium permanganate Uniform Dispersion in shell material solution, stop ultrasonic, stir with the speed of 150rpm and to reduce simultaneously below the temperature of reaction system to 35 ℃, treat that solid separates out fully, finish to react.
Embodiment 2
Get the shell material stearic acid and place there-necked flask, add absolute ethyl alcohol, described absolute ethyl alcohol and stearic mass ratio are 1: 1; Fully stir with 350rpm, ℃ heating of control bath temperature to 80 is fully dissolved stearic acid; Macrogol 4000 in mass ratio again: stearic acid=1: 2, add PEG4000, then potassium permanganate in mass ratio: stearic acid=1: 2, add potassium permanganate, ultrasonic 5min makes potassium permanganate Uniform Dispersion in shell material solution, stop ultrasonic, stir with the speed of 250rpm and to reduce simultaneously below the temperature of reaction system to 35 ℃, treat that solid separates out fully, finish to react.
Embodiment 3
Get the shell material stearic acid and place there-necked flask, add absolute ethyl alcohol, described absolute ethyl alcohol and stearic mass ratio are 1: 1; Fully stir with 350rpm, ℃ heating of control bath temperature to 75 is fully dissolved stearic acid; Macrogol 4000 in mass ratio again: stearic acid=1: 5, add PEG4000, then potassium permanganate in mass ratio: stearic acid=1: 3, add potassium permanganate, ultrasonic 8min makes potassium permanganate Uniform Dispersion in shell material solution, stop ultrasonic, stir with the speed of 350rpm and to reduce simultaneously below the temperature of reaction system to 35 ℃, treat that solid separates out fully, finish to react.
Experimental result shows, along with the increase of nucleocapsid ratio (being potassium permanganate and stearic ratio), the particle diameter of sustained release agent also changes, when potassium permanganate and stearic acid (nucleocapsid ratio) when being 1: 1, the particle diameter of the product that makes is minimum, is about 0.5mm～2mm; When potassium permanganate and stearic acid (nucleocapsid ratio) were 1: 2 and 1: 3, particle diameter was more or less the same, and all is about 2mm～5mm.The clad ratio of the spacetabs type potassium permanganate microcapsules under three kinds of nucleocapsids (being that potassium permanganate and stearic proportioning are 1: 1,1: 2,1: 3) ratio is respectively 33.8%, 58.5%, 129.0%, and the release percentage in water behind the placement 240h is respectively 60.1%, 54.2%, 30.9%.
Wherein, the computing formula of the clad ratio of spacetabs type potassium permanganate microcapsules is as follows:
E=(the actual potassium permanganate content that coats)/(the theoretical potassium permanganate content that coats) * 100%
Actual coating potassium permanganate content refers to the mass percent of actual contained potassium permanganate in the spacetabs type potassium permanganate microcapsules;
Theory coats potassium permanganate content and refers in the microencapsulation process, and the potassium permanganate of adding accounts for potassium permanganate and stearic acid total content percentage.
The spacetabs type potassium permanganate microcapsules that above-described embodiment is made carry out the slowly-releasing experiment, get spacetabs type potassium permanganate microcapsules 0.2～0.5g, place the conical flask that contains 150～500ml distilled water, and (22～24 ℃) are preserved under the shady place room temperature.Front 3 hours, per hour sampling once; Then sampling every day once, measure its absorbance in wavelength 525nm place with ultraviolet specrophotometer, get the concentration of corresponding potassium permanganate according to potassium permanganate calibration curve Solving Equations, according to formula Q=potassium permanganate Cumulative release amount/potassium permanganate total content, calculate high potassium permanganate accumulative total and discharge percentage Q again.Fig. 1 is the elution profiles of spacetabs type potassium permanganate microcapsules in water, and the abscissa among Fig. 1 is slow-release time, and ordinate is that potassium permanganate discharges percentage.Wherein, the experimental data of Fig. 1 equation Q=kt
n(wherein, Q-potassium permanganate accumulative total discharges percentage; K-discharges constant; T-release time, h; N-discharges progression) simulate (artificial line as shown in Figure 1), the release dynamics equation that obtains is Q=0.352t
0.6112, (R
2=0.967), and can be in the hope of discharging the required time t of 50% potassium permanganate
0.5=138.5d, theoretical slow-release time reaches 430.5d.
Trichloro-ethylene (TCE) solution that 100mL concentration is about 10mg/L, drop in the 250mL reaction bulb, then disposable 75mg spacetabs type potassium permanganate microcapsules that add, the pH value of regulating trichloro-ethylene solution with the NaOH of the HCl of 0.1mol/L and 0.1mol/L is 7.0, oscillating reactions in constant temperature oscillator under the room temperature, speed setting is 250rpm, and the trichloro-ethylene change in concentration is measured in certain hour sampling in interval; When the concentration of trichloro-ethylene is lower than 1.0mg/L, finish reaction, solution in the bottle is discharged, with distilled water spacetabs type potassium permanganate microcapsules are washed repeatedly fast, oven dry, then it is dropped into again in trichloro-ethylene (TCE) solution that another part 100mL concentration is about 10mg/L, carry out reaction second round, so circulation, until the concentration of remaining trichloro-ethylene does not satisfy three grades of discharge standards (being 1.0mg/L) in the solution, think that spacetabs type potassium permanganate microcapsules lost efficacy, estimate the lasting effectiveness of spacetabs type potassium permanganate microcapsules degrade trichloro-ethylene (TCE), the result as shown in Figure 2.Seven cycles are experienced altogether in the slowly-releasing experiment of spacetabs type potassium permanganate microcapsules in trichloro-ethylene solution.Period 1, spacetabs type potassium permanganate microcapsules are the fastest to the removal speed of trichloro-ethylene (TCE), and the trichloro-ethylene clearance approximately 95% in 8 hours.This is because the potassium permanganate of sustained release agent adsorption takes the lead in water-solublely, makes that potassium permanganate concentration increases rapidly in the solution, thus trichloro-ethylene to remove speed very fast.Along with injecting increasing of trichloro-ethylene solution number of times, potassium permanganate constantly is consumed, so spacetabs type potassium permanganate microcapsules reduce gradually to the removal speed of trichloro-ethylene.Second～period 6, pass through respectively 13h, 14h, 27h, 32h, 36h, the trichloro-ethylene residual concentration reaches three grades of discharge standards.Through seven all after dates, spacetabs type potassium permanganate microcapsules lost efficacy.
In two parts of 100mL concentration trichloro-ethylene solution that is 9.8mg/L, throw in respectively spacetabs type potassium permanganate microcapsules 7.1mg and 17.5mg, then the regulation system original ph is 7.0, before the assaying reaction with reaction 24h after the Chlorine in Solution ion concentration, investigate the dechlorination degree of spacetabs type potassium permanganate microcapsules oxidative degradation trichloro-ethylenes (TCE).The initial trichloro-ethylene concentration of reaction system is 9.8mg/L, and when spacetabs type potassium permanganate microcapsules dosage was 7.1mg, behind the reaction 24h, the clearance of trichloro-ethylene was 90%, still has 10% trichloro-ethylene not to be removed; Dechlorination rate is 69%, and this explanation only has 69% the complete dechlorination of trichloro-ethylene in 90% trichloro-ethylene of removing.When spacetabs type potassium permanganate microcapsules dosage to 17.5mg, behind the reaction 24h, the clearance of trichloro-ethylene is 100%, simultaneously dechlorination rate also reaches 93.7%.
The present invention is directed to the potassium permanganate in situ chemical oxidation and remove that the oxidant utilization rate that exists in the groundwater pollutant process is low, non-selectivity consumption large, the problems such as mass transfer of oxidant, pass through microcapsules technology, so that the potassium permanganate surface behind the microencapsulation becomes lipophile by hydrophily, make its easy dispersion in the organic solvents such as chlorohydrocarbon, increase the contact range of potassium permanganate oxidant and target contaminant, reduce without selecting and consume, improve the utilization of oxidant, thereby realize the slow release of oxidant, the effective purpose such as transmission and efficient oxidation.
Claims (6)
1. the preparation method of spacetabs type potassium permanganate microcapsules is characterized in that: may further comprise the steps:
(1) stearic acid is placed reactor, add absolute ethyl alcohol, heating water bath is stirred well to stearic acid and dissolves fully;
(2) add Macrogol 4000 and potassium permanganate, then the ultrasonic potassium permanganate Uniform Dispersion in solution that makes stops ultrasonicly and under agitation, naturally cools to below 35 ℃ again, treats that solid separates out fully, finishes reaction; Wherein, described potassium permanganate and stearic mass ratio are 1: 1-1: 3.
2. the preparation method of spacetabs type potassium permanganate microcapsules as claimed in claim 1, it is characterized in that: described Macrogol 4000 and stearic mass ratio are 1: 2-1: 5.
3. the preparation method of spacetabs type potassium permanganate microcapsules as claimed in claim 1, it is characterized in that: described absolute ethyl alcohol and stearic mass ratio are 1: 1.
4. the preparation method of spacetabs type potassium permanganate microcapsules as claimed in claim 1, it is characterized in that: the temperature of described heating water bath is 70-80 ℃.
5. the preparation method of spacetabs type potassium permanganate microcapsules as claimed in claim 1, it is characterized in that: the described ultrasonic time is 5-10min.
6. the preparation method of spacetabs type potassium permanganate microcapsules as claimed in claim 1 is characterized in that: electric blender is adopted in the stirring in the described step (2), and the speed that stirs is 150-350rpm.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103896389A (en) * | 2014-03-26 | 2014-07-02 | 华南师范大学 | Controlled release type potassium ferrate composite as well as preparation method and application thereof |
| CN109127714A (en) * | 2018-09-28 | 2019-01-04 | 昆明理工大学 | A kind of soil remediation medicament high-pressure jet injected system and method |
| CN109970162A (en) * | 2019-03-28 | 2019-07-05 | 浙江大学 | A kind of novel dephosphorization sustained release agent and preparation method thereof |
| CN110294773A (en) * | 2019-07-29 | 2019-10-01 | 北京德美科创科技有限公司 | TCPP fire retardant preparation method and thus obtained TCPP fire retardant |
| CN110387242A (en) * | 2019-06-27 | 2019-10-29 | 浙江工商大学 | A kind of potassium permanganate sustained-release agent and its preparation method and application |
| CN110639339A (en) * | 2019-09-29 | 2020-01-03 | 华晋瑞海科技有限公司 | Novel denitration agent and preparation method thereof |
| CN110845076A (en) * | 2019-11-13 | 2020-02-28 | 沈阳大学 | Combined remediation method for atrazine-polluted water body |
| CN110899319A (en) * | 2019-10-18 | 2020-03-24 | 沈阳大学 | Method for restoring atrazine-polluted farmland soil |
| CN111892155A (en) * | 2020-08-20 | 2020-11-06 | 江苏苏美达成套设备工程有限公司 | Slow-release oxidizing agent for removing underground water polluted organic matter and process thereof |
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2013
- 2013-02-05 CN CN2013100476225A patent/CN103071436A/en active Pending
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896389A (en) * | 2014-03-26 | 2014-07-02 | 华南师范大学 | Controlled release type potassium ferrate composite as well as preparation method and application thereof |
| CN103896389B (en) * | 2014-03-26 | 2016-01-20 | 华南师范大学 | Control release type potassium ferrate complex body and Synthesis and applications thereof |
| CN109127714A (en) * | 2018-09-28 | 2019-01-04 | 昆明理工大学 | A kind of soil remediation medicament high-pressure jet injected system and method |
| CN109970162A (en) * | 2019-03-28 | 2019-07-05 | 浙江大学 | A kind of novel dephosphorization sustained release agent and preparation method thereof |
| CN110387242A (en) * | 2019-06-27 | 2019-10-29 | 浙江工商大学 | A kind of potassium permanganate sustained-release agent and its preparation method and application |
| CN110294773A (en) * | 2019-07-29 | 2019-10-01 | 北京德美科创科技有限公司 | TCPP fire retardant preparation method and thus obtained TCPP fire retardant |
| CN110294773B (en) * | 2019-07-29 | 2022-08-23 | 北京德美科创科技有限公司 | TCPP flame retardant preparation method and TCPP flame retardant prepared by same |
| CN110639339A (en) * | 2019-09-29 | 2020-01-03 | 华晋瑞海科技有限公司 | Novel denitration agent and preparation method thereof |
| CN110899319A (en) * | 2019-10-18 | 2020-03-24 | 沈阳大学 | Method for restoring atrazine-polluted farmland soil |
| CN110845076A (en) * | 2019-11-13 | 2020-02-28 | 沈阳大学 | Combined remediation method for atrazine-polluted water body |
| CN111892155A (en) * | 2020-08-20 | 2020-11-06 | 江苏苏美达成套设备工程有限公司 | Slow-release oxidizing agent for removing underground water polluted organic matter and process thereof |
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Application publication date: 20130501 |