CN106433685A - Preparation method of soil remediation material on basis of acrylic resin - Google Patents
Preparation method of soil remediation material on basis of acrylic resin Download PDFInfo
- Publication number
- CN106433685A CN106433685A CN201610839559.2A CN201610839559A CN106433685A CN 106433685 A CN106433685 A CN 106433685A CN 201610839559 A CN201610839559 A CN 201610839559A CN 106433685 A CN106433685 A CN 106433685A
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- Prior art keywords
- acrylic resin
- preparation
- soil remediation
- montmorillonite
- remediation material
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K17/00—Soil-conditioning materials or soil-stabilising materials
- C09K17/40—Soil-conditioning materials or soil-stabilising materials containing mixtures of inorganic and organic compounds
- C09K17/42—Inorganic compounds mixed with organic active ingredients, e.g. accelerators
- C09K17/46—Inorganic compounds mixed with organic active ingredients, e.g. accelerators the inorganic compound being a water-soluble silicate
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having a double or triple bond to nitrogen, e.g. cyanates, cyanamides
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2101/00—Agricultural use
Abstract
The invention discloses a preparation method of a soil remediation material on the basis of acrylic resin. The preparation method comprises the specific steps as follows: Na-montmorillonite is taken, washed, dried, ground and added to octadecyl trimethyl ammonium chloride, organically modified montmorillonite is mixed with acetamiprid and the acrylic resin, the mixture is added to an acetonitrile solution, an inner oil-phase solution is obtained by adding triethyl citrate and polysorbate-80 to the solution and dropwise added to an outer oil-phase solution of light liquid paraffin mixed with Span-80, petroleum ether is added after emulsification performed for a period of time, and a precipitate is taken centrifugally, washed with an n-hexane solution and dried. The montmorillonite is organically modified with the octadecyl trimethyl ammonium chloride, the modified montmorillonite and the acrylic resin are taken as carriers of the acetamiprid as a pesticide, and drug-carrying microspheres are prepared with an O/O volatilization method and have the effect of adsorbing residual pollutants in soil while having soil sterilizing and insect killing functions on farming soil.
Description
Technical field
The invention belongs to technical field of pesticide, the system of more particularly to a kind of soil remediation material based on acrylic resin
Preparation Method.
Background technology
Medicine microspheres are a kind of novel pharmaceutical formulations, are using as the high molecular polymerization such as starch, shitosan, PLA, gelatin
Thing material, as carrier, solid or liquid medicine is wrapped up the solid skeletal thing of the microscopic, spherical entity being solidified to form, it is straight
Footpath is not of uniform size, typically at 1-300 μm, even more greatly, belongs to matrix type skeleton particulate.
Montmorillonite is the surface electronegative silicate lamella by nano thickness for the class, relies on the electrostatic interaction of interlayer and heap
The long-pending earthy mineral together constituting, the structure cell in its crystal structure is by one layer of alumina octahedral of folder in the middle of two-layer silicon-oxy tetrahedron
Body is constituted.There is one-dimensional layered nano-structure and the cation exchange characteristic of uniqueness, thus giving the many modifications of montmorillonite
May be with the expansion of application.The application of montmorillonite widely, makes it rich especially by inorganic and organically-modified
There is the performance of many uniquenesses, application further expands, and is described as " universal material ", is widely used in the absorption of Toxic
Agent, catalyst, coating agent, especially polymer-laminated nano composition, make mechanical properties of polymer, fire resistance, heat steady
The raising of qualitative energy, has a extensive future.
Content of the invention
It is an object of the invention to provide a kind of preparation method of the soil remediation material based on acrylic resin, with modification
Montmorillonite and acrylic resin, as agricultural chemicals Acetamiprid carrier, prepare drug bearing microsphere with O/O volatility process, the drug bearing microsphere being produced
Effect of residual contaminants in absorption soil is had concurrently while to cultivated soil sterilizing pesticide.
The present invention is achieved by the following technical solutions：
A kind of preparation method of the soil remediation material based on acrylic resin, comprises the following specific steps that：
S1, take sodium-based montmorillonite washing and drying after, be milled to particle diameter be 2.25-3.3mm, obtain montmorillonite particle；
S2, the montmorillonite particle obtaining in S1 is added in OTAC, solid-to-liquid ratio is 1:4, obtain
To modified montmorillonoid suspension；
This modified montmorillonoid suspension centrifuging and taking is precipitated vacuum drying, milled 200 mesh sieves obtain modified montmorillonoid powder；
S3, weigh Acetamiprid and acrylic resin with S2 preparation modified montmorillonoid powder mix after add molten to acetonitrile
In liquid, solid-to-liquid ratio is 1:15, obtain interior oil-phase solution；
In oil-phase solution in adding after triethyl citrate is mixed with Tween-80, solid-to-liquid ratio is 1:5, magnetic force stirs
Mix device stirring 30min；
S4, in liquid paraffin,light add Arlacel-80, solid-to-liquid ratio be 1:100, obtain outer oil-phase solution；
Under the conditions of 10 DEG C of ice-water baths, interior oil-phase solution is added dropwise in outer oil-phase solution, interior oil phase and outer oil phase
Volume ratio be 1:2, with 800r/min mechanical agitation 10min after ultrasonic 10-20min；
With volume ratio for 1 after standing 1-2h:1 addition petroleum ether, topples over supernatant liquor after standing, centrifuging and taking precipitation is used just own
The washing of alkane solution is simultaneously dried under room temperature condition.
Further, in described S1, drying temperature is 105 DEG C, and drying time is 1-2h.
Further, OTAC solution concentration described in S2 is 8g/L.
Further, in described S2, bath temperature is 65-80 DEG C, and the water-bath concussion time is 4-6h.
Further, in described S2, centrifugation rate is 4000-5000r/min, and centrifugation time is 20min.
Further, the mass ratio of Acetamiprid described in S3, acrylic resin and modified montmorillonoid powder is 2:7:10.
Further, triethyl citrate described in S3 and Tween-80 mass ratio are 20:1.
Further, in described S4, mechanical agitation speed is 300r/min, and the mechanical agitation time is 10min.
Further, in described S4, centrifugation rate is 3000r/min, and centrifugation time is 30min.
The invention has the advantages that：
The present invention passes through to add OTAC organically-modified to montmorillonite, and with modified montmorillonoid and third
Olefin(e) acid resin, as agricultural chemicals Acetamiprid carrier, prepares drug bearing microsphere with O/O volatility process, and the drug bearing microsphere being produced is to cultivated soil
Effect of residual contaminants in absorption soil is had concurrently while sterilizing pesticide.
Specific embodiment
Technical scheme in the embodiment of the present invention is clearly and completely described it is clear that described embodiment is only
The a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art
The all other embodiment being obtained under the premise of not making creative work, broadly falls into the scope of protection of the invention.
Embodiment 1
S1, take sodium-based montmorillonite after being washed with deionized 2 times, to put in 105 DEG C of baking ovens drying 1h, the illiteracy of drying is taken off
It is 2.25mm that soil is milled to particle diameter, obtains montmorillonite particle；
OTAC is added to be configured to 8g/L solution, by the montmorillonite obtaining in S1 in S2, distilled water
Particle is added in this organic solution, and solid-to-liquid ratio is 1:4-6h is shaken in 4,65 DEG C of water-baths, obtains modified montmorillonoid suspension；
This modified montmorillonoid suspension is centrifuged 20min in 4000r/min, takes milled 200 mesh after precipitation vacuum drying 24h
Sieve obtains modified montmorillonoid powder；
S3, weigh Acetamiprid and acrylic resin with S2 preparation modified montmorillonoid powder mix after add molten to acetonitrile
In liquid, solid-to-liquid ratio is 1:15, obtain interior oil-phase solution, the wherein quality of Acetamiprid, acrylic resin and modified montmorillonoid powder
Than for 2:7:10；
In oil-phase solution in adding after triethyl citrate is mixed with Tween-80, solid-to-liquid ratio is 1:5, magnetic force stirs
Mix device stirring 30min, wherein triethyl citrate and Tween-80 mass ratio is 20:1；
S4, in liquid paraffin,light add Arlacel-80, solid-to-liquid ratio be 1:100, obtain outer oil-phase solution；
Under the conditions of 10 DEG C of ice-water baths, interior oil-phase solution is added dropwise in outer oil-phase solution, interior oil phase and outer oil phase
Volume ratio be 1:2, with 800r/min mechanical agitation 10min after ultrasonic 10min；
With volume ratio for 1 after standing 1-2h:1 addition petroleum ether, 300r/min mechanical agitation 10min, stand 30min-
Solution layering after 60min, topples over supernatant liquor and is centrifuged 30min in 3000r/min, take precipitation hexane solution to wash 3 times
Afterwards, it is placed in 20 DEG C and 4h is dried.
Embodiment 2
S1, sodium-based montmorillonite is taken after being washed with deionized 3 times, to put in 105 DEG C of baking ovens drying 1-2h, the illiteracy that will dry
It is 3.3mm that de- soil is milled to particle diameter, obtains montmorillonite particle；
OTAC is added to be configured to 8g/L solution, by the montmorillonite obtaining in S1 in S2, distilled water
Particle is added in this organic solution, and solid-to-liquid ratio is 1:6h is shaken in 4,80 DEG C of water-baths, obtains modified montmorillonoid suspension；
This modified montmorillonoid suspension is centrifuged 20min in 5000r/min, takes milled 200 mesh after precipitation vacuum drying 24h
Sieve obtains modified montmorillonoid powder；
S3, weigh Acetamiprid and acrylic resin with S2 preparation modified montmorillonoid powder mix after add molten to acetonitrile
In liquid, solid-to-liquid ratio is 1:15, obtain interior oil-phase solution, the wherein quality of Acetamiprid, acrylic resin and modified montmorillonoid powder
Than for 2:7:10；
In oil-phase solution in adding after triethyl citrate is mixed with Tween-80, solid-to-liquid ratio is 1:5, magnetic force stirs
Mix device stirring 30min, wherein triethyl citrate and Tween-80 mass ratio is 20:1；
S4, in liquid paraffin,light add Arlacel-80, solid-to-liquid ratio be 1:100, obtain outer oil-phase solution；
Under the conditions of 10 DEG C of ice-water baths, interior oil-phase solution is added dropwise in outer oil-phase solution, interior oil phase and outer oil phase
Volume ratio be 1:2, with 800r/min mechanical agitation 10min after ultrasonic 20min；
With volume ratio for 1 after standing 1-2h:1 addition petroleum ether, 300r/min mechanical agitation 10min, molten after standing 60min
Liquid is layered, and topples over supernatant liquor and is centrifuged 30min in 3000r/min, after taking precipitation hexane solution to wash 5 times, is placed in 30
DEG C 8h is dried.
Embodiment 3
S1, sodium-based montmorillonite is taken after being washed with deionized 3 times, to put in 105 DEG C of baking ovens drying 1.5h, the illiteracy that will dry
It is 2.75mm that de- soil is milled to particle diameter, obtains montmorillonite particle；
OTAC is added to be configured to 8g/L solution, by the montmorillonite obtaining in S1 in S2, distilled water
Particle is added in this organic solution, and solid-to-liquid ratio is 1:4-6h is shaken in 4,70 DEG C of water-baths, obtains modified montmorillonoid suspension；
This modified montmorillonoid suspension is centrifuged 20min in 4500r/min, takes milled 200 mesh after precipitation vacuum drying 24h
Sieve obtains modified montmorillonoid powder；
S3, weigh Acetamiprid and acrylic resin with S2 preparation modified montmorillonoid powder mix after add molten to acetonitrile
In liquid, solid-to-liquid ratio is 1:15, obtain interior oil-phase solution, the wherein quality of Acetamiprid, acrylic resin and modified montmorillonoid powder
Than for 2:7:10；
In oil-phase solution in adding after triethyl citrate is mixed with Tween-80, solid-to-liquid ratio is 1:5, magnetic force stirs
Mix device stirring 30min, wherein triethyl citrate and Tween-80 mass ratio is 20:1；
S4, in liquid paraffin,light add Arlacel-80, solid-to-liquid ratio be 1:100, obtain outer oil-phase solution；
Under the conditions of 10 DEG C of ice-water baths, interior oil-phase solution is added dropwise in outer oil-phase solution, interior oil phase and outer oil phase
Volume ratio be 1:2, with 800r/min mechanical agitation 10min after ultrasonic 15min；
With volume ratio for 1 after standing 1-2h:1 addition petroleum ether, 300r/min mechanical agitation 10min, molten after standing 45min
Liquid is layered, and topples over supernatant liquor and is centrifuged 30min in 3000r/min, after taking precipitation hexane solution to wash 4 times, is placed in 25
DEG C 6h is dried.
Medicine microspheres are a kind of novel pharmaceutical formulations, are using as the high molecular polymerization such as starch, shitosan, PLA, gelatin
Thing material, as carrier, solid or liquid medicine is wrapped up the solid skeletal thing of the microscopic, spherical entity being solidified to form, it is straight
Footpath is not of uniform size, typically at 1-300 μm, even more greatly, belongs to matrix type skeleton particulate.The present invention passes through to add octadecyl three
Ammonio methacrylate is organically-modified to montmorillonite, and using modified montmorillonoid and acrylic resin as agricultural chemicals Acetamiprid carrier, with O/O
Volatility process prepares drug bearing microsphere, has concurrently in absorption soil and remain while the drug bearing microsphere being produced is to cultivated soil sterilizing pesticide
Effect of pollutant.
Above content is only citing made for the present invention and illustrates, affiliated those skilled in the art are to being retouched
The specific embodiment stated is made various modifications or supplements or substituted using similar mode, without departing from invention or super
More scope defined in the claims, all should belong to protection scope of the present invention.
Claims (9)
1. a kind of preparation method of the soil remediation material based on acrylic resin is it is characterised in that comprise the following specific steps that：
S1, take sodium-based montmorillonite washing and drying after, be milled to particle diameter be 2.25-3.3mm, obtain montmorillonite particle；
S2, the montmorillonite particle obtaining in S1 is added in OTAC, solid-to-liquid ratio is 1:4, changed
Property montmorillonite suspension；
This modified montmorillonoid suspension centrifuging and taking is precipitated vacuum drying, milled 200 mesh sieves obtain modified montmorillonoid powder；
S3, weigh Acetamiprid and acrylic resin with S2 preparation modified montmorillonoid powder mix after add to acetonitrile solution
In, solid-to-liquid ratio is 1:15, obtain interior oil-phase solution；
In oil-phase solution in adding after triethyl citrate is mixed with Tween-80, solid-to-liquid ratio is 1:5, magnetic stirring apparatus
Stirring 30min；
S4, in liquid paraffin,light add Arlacel-80, solid-to-liquid ratio be 1:100, obtain outer oil-phase solution；
Under the conditions of 10 DEG C of ice-water baths, interior oil-phase solution is added dropwise in outer oil-phase solution, the body of interior oil phase and outer oil phase
Long-pending ratio is 1:2, with 800r/min mechanical agitation 10min after ultrasonic 10-20min；
With volume ratio for 1 after standing 1-2h:1 addition petroleum ether, topples over supernatant liquor after standing, centrifuging and taking precipitation is molten with n-hexane
Liquid washing is simultaneously dried under room temperature condition.
2. the preparation method of a kind of soil remediation material based on acrylic resin according to claim 1, its feature exists
In：In described S1, drying temperature is 105 DEG C, and drying time is 1-2h.
3. the preparation method of a kind of soil remediation material based on acrylic resin according to claim 1, its feature exists
In：OTAC solution concentration described in S2 is 8g/L.
4. the preparation method of a kind of soil remediation material based on acrylic resin according to claim 1, its feature exists
In：In described S2, bath temperature is 65-80 DEG C, and the water-bath concussion time is 4-6h.
5. the preparation method of a kind of soil remediation material based on acrylic resin according to claim 1, its feature exists
In：In described S2, centrifugation rate is 4000-5000r/min, and centrifugation time is 20min.
6. the preparation method of a kind of soil remediation material based on acrylic resin according to claim 1, its feature exists
In：The mass ratio of Acetamiprid described in S3, acrylic resin and modified montmorillonoid powder is 2:7:10.
7. the preparation method of a kind of soil remediation material based on acrylic resin according to claim 1, its feature exists
In：Triethyl citrate described in S3 and Tween-80 mass ratio are 20:1.
8. the preparation method of a kind of soil remediation material based on acrylic resin according to claim 1, its feature exists
In：In described S4, mechanical agitation speed is 300r/min, and the mechanical agitation time is 10min.
9. the preparation method of a kind of soil remediation material based on acrylic resin according to claim 1, its feature exists
In：In described S4, centrifugation rate is 3000r/min, and centrifugation time is 30min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107941964A (en) * | 2018-01-05 | 2018-04-20 | 江苏中宜金大分析检测有限公司 | A kind of method of pendimethalin content in agricultural product using liquid chromatography for measuring |
| CN111886956A (en) * | 2020-07-10 | 2020-11-06 | 西藏自治区农牧科学院农业质量标准与检测研究所 | Method for repairing salinization of farming soil |
| CN113575608A (en) * | 2021-08-27 | 2021-11-02 | 广东中迅农科股份有限公司 | Insecticidal composition and application thereof |
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| CN113575608A (en) * | 2021-08-27 | 2021-11-02 | 广东中迅农科股份有限公司 | Insecticidal composition and application thereof |
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