CN106614553A - Pesticide slow-release agent and preparation method thereof - Google Patents
Pesticide slow-release agent and preparation method thereof Download PDFInfo
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- CN106614553A CN106614553A CN201610981077.0A CN201610981077A CN106614553A CN 106614553 A CN106614553 A CN 106614553A CN 201610981077 A CN201610981077 A CN 201610981077A CN 106614553 A CN106614553 A CN 106614553A
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- phytic acid
- pesticide
- releasing agent
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- 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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
-
- 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
- A01N51/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds having the sequences of atoms O—N—S, X—O—S, N—N—S, O—N—N or O-halogen, regardless of the number of bonds each atom has and with no atom of these sequences forming part of a heterocyclic ring
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- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention provides a pesticide slow-release agent and a preparation method thereof. The preparation method includes the steps: firstly, performing phytic acid modification for straws; secondly, enabling pesticides to adsorb on phytic acid modified straws. A preparation process of the phytic acid modified straws includes the steps: crushing the straws; performing acidification for the crushed straws; washing; cleaning to obtain preset straws; mixing and reacting 75%-90% of N, N-dimethyl formamide, 3%-10% of preset straws, 2%-6% of urea and 3%-10% of phytic acid to obtain the phytic acid modified straws. According to the pesticide slow-release agent, by the aid of modified products of the straws, imidacloprid pesticide can be effectively adsorbed, release of the imidacloprid pesticide is effectively controlled, and the pesticide slow-release agent is wide in raw material resource, simple in preparation process, short in period, high in adsorbing capacity and excellent in controlled release performance.
Description
Technical field
The invention belongs to pesticide field, is related to pesticide slow-releasing agent, and in particular to a kind of pesticide slow-releasing agent and preparation method thereof.
Background technology
Imidacloprid is nitro-methylene-type systemic insecticide, is the acting body of nAChR, interference insect fortune
Dynamic nervous system makes chemical signal transmit failure, no interactions resistance problem.It is mainly used in preventing and treating sucking pest.Imidacloprid
Chloro nicotine insecticide of new generation, because its have wide spectrum, efficiently, low toxicity, low-residual, insect is not likely to produce resistance, to people,
Poultry, plant and natural enemies security, and have tag, stomach toxicity and the multiple drug effect of interior suction, quick-acting is good, has higher preventive effect within 1 day after medicine,
Residual life, is up to 25 days or so.Drug effect and temperature are proportionate, and temperature is high, are extensively welcome by peasant the characteristics of good disinsection effect,
Become the maximum insecticide variety of global marketing volume.About 2.2 ten thousand tons of 2012 annual productions and apparent demand amount, and domestic imidacloprid is produced
About 1.8 ten thousand tons of amount, global all production capacities are in advance in respect of 40,000 tons/year.
The traditional processing formulation of imidacloprid mainly has missible oil, wettable powder, suspending agent, water dispersible granules, tablet etc..This
An a little common problems of the formulation using in be apply after due to photodissociation (especially ultraviolet), hydrolysis, it is biodegradable, volatilize and
The reasons such as loss, cause its utilization rate substantially to reduce, and have quite a few not act on target, and are wasted, while making
Into environmental pollution.Developing imidacloprid slow-releasing granules in recent years becomes the focus of research.
One kind is disclosed in prior art with imidacloprid etc. as active component, modified starch and clay are filler, with tung oil,
Peanut oil etc. for coating agent new sustained release granular pesticide, had good sustained release effect, but all oils limited sources.
A kind of imidacloprid/hydrotalcite-like compounds nano hybrid is disclosed in prior art, by with surfactant-modified class
Hydrotalcite and the imidacloprid being inserted with intercalated form are made, and imidacloprid/HTLC nano hybrids are by surfactant (SAA)
Modified HTLC and the toluene/ethanol solution hybrid reaction of imidacloprid and synthesize, synthetic method is simple, and drugloading rate is big, with
Imidacloprid bulk drug is compared with obvious slow release effect.But the method production time is slower, the reaction time needs 4 days.Can
To find out, so far, imidacloprid sustained release agent also has very big room for improvement, particularly in raw material sources, adsorbance, and sustained release effect
Really, the aspect such as preparation technology and cycle.
The content of the invention
For shortcomings and deficiencies present in prior art, this it is an object of the invention to, there is provided a kind of pesticide slow-releasing agent
And preparation method thereof, for imidacloprid pesticide, can preferably realize adsorbing imidacloprid pesticide and control release.
In order to solve above-mentioned technical problem, the present invention is adopted the following technical scheme that and is achieved:
A kind of preparation method of pesticide slow-releasing agent, the method first carries out phytic acid to stalk and is modified, and is then adsorbed onto in agricultural chemicals
On phytic acid modified straw.
The present invention also has following distinguishing feature:
Specifically, the preparation process of described phytic acid modified straw is comprised the following steps:
Step one, dry crushed stalk is acidified in acid solution, is then washed till neutrality, is dried, and obtains pre- place
Stalk after reason;
Step 2, is well mixed raw material by following percentage by weight:
30mLN is added to per the pretreated stalks of 2g, in dinethylformamide and is stirred, then sequentially added
The phytic acid of 2.1mL and the urea of 1.2g;
The raw material being well mixed is transferred in reactor, temperature control is fully reacted at 80 DEG C, is taken out, washing,
It is dried, obtains final product phytic acid modified straw.
In step one, by dry crushed stalk to 100~200 mesh.
In step one, the pH of described acid solution is less than 3;Preferably, the pH of described acid solution is 1~2;Preferably,
Described acid solution is the hydrochloric acid of 0.1mol/L.
In step 2, fully reaction is referred to as far as possible that raw material reaction is complete.The fully reaction time of reaction is 4~7 little
When, preferably 5~6 hours.
Specifically, it is by the process that agricultural chemicals is adsorbed onto on phytic acid modified straw:Phytic acid modified straw is taken, is added to excessive
In the pesticide solution, after fully absorption, filter, after solid content is dried, obtain final product pesticide slow-releasing agent.
Preferably, described stalk is wheat stalk, rice straw or maize straw.
Preferably, described agricultural chemicals is nicotinic insecticide, it is furthermore preferred that described agricultural chemicals is imidacloprid.The agricultural chemicals
For imidacloprid when, it is above-mentioned agricultural chemicals is adsorbed onto on phytic acid modified straw during, the pH of the pesticide solution is 5~10, further
Preferably, the pH of the pesticide solution is 7~9.
A kind of pesticide slow-releasing agent, the agricultural chemicals corrosion inhibiter is by made by agricultural chemicals is adsorbed onto on phytic acid modified straw.Institute
The agricultural chemicals corrosion inhibiter stated is made using preparation method as above.
The present invention compared with prior art, has the following technical effect that:
The present invention can not only preferably realize adsorbing imidacloprid pesticide and controlled-release is released using the modified product of stalk
Put, and with raw material sources extensively, preparation process is simple, cycle is short, adsorbance be big, control release function admirable characteristic.
Wheat stalk surface hydroxyl groups are esterified with the electronegative phosphate group of phytate molecule after pretreatment
Reaction, is prepared into imidacloprid pesticide sustained release agent.Wheat stalk surface carries stronger elecrtonegativity, enhances to imidacloprid pesticide
Suction-operated, adjusts pH value, changes wheat stalk surface electrical behavior, so as to reach the purpose of sustained-release pesticides.With existing technology phase
Than the invention has extensive, big, the control release function admirable of preparation process is simple, cycle is short, adsorbance of raw material sources etc. excellent
Point, effectively improves imidacloprid utilization rate, reduces the usage amount of imidacloprid, and then mitigation is excessively used imidacloprid pesticide or pyrrole
Worm quinoline is lost in the pollution to environment, while the comprehensive utilization of wheat stalk can be realized.
Description of the drawings
Fig. 1 is to prepare the wheat stalk powder obtained during the imidacloprid pesticide sustained release agent based on wheat stalk to carry out light
Microscope phenogram is learned, that is, schemes a.
Fig. 2 is to prepare the wheat stalk powder obtained during the imidacloprid pesticide sustained release agent based on wheat stalk to be swept
Electron microscope phenogram is retouched, that is, schemes b.
Fig. 3 is to prepare the phytic acid modified wheat stalk obtained during the imidacloprid pesticide sustained release agent based on wheat stalk to enter
Row light microscope phenogram, that is, scheme c.
Fig. 4 is to prepare the phytic acid modified wheat stalk obtained during the imidacloprid pesticide sustained release agent based on wheat stalk to enter
Row SEM phenogram, that is, scheme d.
Fig. 5 is to prepare the imidacloprid pesticide sustained release agent obtained during the imidacloprid pesticide sustained release agent based on wheat stalk to enter
Row light microscope phenogram, that is, scheme e.
Fig. 6 is to prepare the imidacloprid pesticide sustained release agent obtained during the imidacloprid pesticide sustained release agent based on wheat stalk to enter
Row SEM phenogram, that is, scheme f.
With reference to embodiments explanation is further explained in detail to the particular content of the present invention.
Specific embodiment
The specific embodiment of the present invention given below, implement in detail below it should be noted that the invention is not limited in
Example, all equivalents done on the basis of technical scheme each fall within protection scope of the present invention.
Embodiment 1:
The present embodiment provides a kind of preparation method of pesticide slow-releasing agent, and the method first carries out phytic acid to wheat stalk and is modified,
Then agricultural chemicals is adsorbed onto on phytic acid modified wheat stalk, specifically includes following steps:
Step one, wheat stalk pretreatment:Wheat stalk is cleaned up, in 50 DEG C of drying, 100~200 mesh is ground into
Powder wheat stalk, then with distillation water washing wheat stalk powder end, filter afterwards, by screening 0.1mol/L hydrochloric acid
In greenhouse, soaking and stirring 2h is acidified, and then ultrasonic bath washes 30min (40kHz, 300W), and absolute ethanol washing is used after filtration
To neutral, in 50 DEG C of drying, pretreated wheat stalk is obtained.Light microscope phenogram such as Fig. 1 of wheat stalk powder
Shown, the SEM phenogram of wheat stalk powder is as shown in Figure 2.
It is prepared by step 2, phytic acid modified wheat stalk:Precise wheat stalk powder 2g, is added to 30mLN, N- diformazans
In base formamide and stir, then sequentially add the phytic acid of 2.1mL and the urea of 1.2g, pour into after stirring at normal temperature 30min
Reactor, reacts 5h in the baking oven for putting into 80 DEG C, taking-up is cooled to room temperature, and deionized water is centrifuged repeatedly washing 3 times, will produce
Thing is put in 50 DEG C of baking ovens and is dried, that is, obtain phytic acid modified wheat stalk.The light microscope of phytic acid modified wheat stalk is characterized
Figure is as shown in figure 3, the SEM phenogram of phytic acid modified wheat stalk is as shown in Figure 4.
It is prepared by step 3, imidacloprid pesticide sustained release agent:Precise 1g phytic acid modified wheat stalks, are added to 100mL's
The imidacloprid pesticide of 100mg/L.In view of the absorption for being conducive to modified wheat stalk and imidacloprid in the basic conditions, i.e. alkalescence
Stronger adsorbance is bigger.But the too strong unavoidable soil ph of alkaline subsequent applications process brings impact.Therefore it is selectable molten
Liquid alkaline range is 7~10, and experiment preferable ph is between 7.5~8.5.Stirring at normal temperature 2h, filters, and dries at 50~60 DEG C,
Obtain imidacloprid pesticide sustained release agent.The light microscope phenogram of imidacloprid pesticide sustained release agent is as shown in figure 5, imidacloprid pesticide
The SEM phenogram of sustained release agent is as shown in Figure 6.
The concentration of the imidacloprid in filtrate is measured using ultra-violet and visible spectrophotometer, phytic acid modified wheat stalk is calculated
Adsorbance to imidacloprid.As a result it is as shown in table 1.
Using method:After applying pesticides sustained release agent, by adjusting the pH to 4~10 of planting environment farm chemical release is controlled;
Preferably, farm chemical release is controlled by adjusting the pH to 5~10 of planting environment.Improve planting environment pH, farm chemical release speed
Slow down;Planting environment pH is reduced, pesticide slow-release speed increases.Certainly, specific planting environment pH can also be according to the suitable of agricultural chemicals
It is adjusted with pH scopes, such as imidacloprid is 5~11 relatively stable in pH, then, in concrete operations, can select to adjust and plant
It is 5~10 to plant environment pH.The pesticide slow-releasing agent that i.e. present invention is provided, after application, can be adjusted by adjusting planting environment pH
The rate of release of whole agricultural chemicals, it is actually used during, can according to real needs adjustment obtain corresponding farm chemical release speed.
Imidacloprid pesticide sustained release agent sustained release is determined:The imidacloprid pesticide sustained release agent of precise 0.1g, is added to regulation pH
Value is respectively in the deionized water of 8 and 10 100mL and stirs, and is measured under different time using ultra-violet and visible spectrophotometer
The concentration of the imidacloprid in solution.As a result it is as shown in table 1.
Embodiment 2:
The present embodiment provides a kind of preparation method of pesticide slow-releasing agent, and the method first carries out phytic acid to wheat stalk and is modified,
Then agricultural chemicals is adsorbed onto on phytic acid modified wheat stalk, specifically includes following steps:
Step one, wheat stalk pretreatment:It is identical with the step of embodiment 1 one.
It is prepared by step 2, phytic acid modified wheat stalk:It is identical with the step of embodiment 1 two.
It is prepared by step 3, imidacloprid pesticide sustained release agent:It is identical with the step of embodiment 1 three.
The concentration of the imidacloprid in filtrate is measured using ultra-violet and visible spectrophotometer, phytic acid modified wheat stalk is calculated
Adsorbance to imidacloprid.As a result it is as shown in table 1.
Imidacloprid pesticide sustained release agent sustained release is determined:The imidacloprid pesticide sustained release agent of precise 0.1g, is added to regulation pH
It is worth in the deionized water for 7 100mL and stirs, is measured under different time in solution using ultra-violet and visible spectrophotometer
The concentration of imidacloprid.As a result it is as shown in table 1.
Embodiment 3:
The present embodiment provides a kind of preparation method of pesticide slow-releasing agent, and the method first carries out phytic acid to wheat stalk and is modified,
Then agricultural chemicals is adsorbed onto on phytic acid modified wheat stalk, specifically includes following steps:
Step one, wheat stalk pretreatment:It is identical with the step of embodiment 1 one.
It is prepared by step 2, phytic acid modified wheat stalk:It is identical with the step of embodiment 1 two.
It is prepared by step 3, imidacloprid pesticide sustained release agent:It is identical with the step of embodiment 1 three.
The concentration of the imidacloprid in filtrate is measured using ultra-violet and visible spectrophotometer, phytic acid modified wheat stalk is calculated
Adsorbance to imidacloprid.As a result it is as shown in table 1.
Imidacloprid pesticide sustained release agent sustained release is determined:The imidacloprid pesticide sustained release agent of precise 0.1g, is added to regulation pH
Value is respectively in the deionized water of 4 and 6 100mL and stirs, and is measured under different time using ultra-violet and visible spectrophotometer
The concentration of the imidacloprid in solution.As a result it is as shown in table 1.
Embodiment 4:
The present embodiment provides a kind of preparation method of pesticide slow-releasing agent, and other steps of the method are same as Example 1, area
It is not only in that, the wheat stalk in embodiment 1 is replaced by into rice straw.
Embodiment 5:
The present embodiment provides a kind of preparation method of pesticide slow-releasing agent, and other steps of the method are same as Example 1, area
It is not only in that, the wheat stalk in embodiment 1 is replaced by into maize straw.
Table 1 with solution ph change, slow-release capability of the imidacloprid pesticide sustained release agent to imidacloprid pesticide
Claims (10)
1. a kind of preparation method of pesticide slow-releasing agent, it is characterised in that the method first carries out phytic acid to stalk and is modified, then by agriculture
Medicine is adsorbed onto on phytic acid modified straw.
2. the preparation method of pesticide slow-releasing agent as claimed in claim 1, it is characterised in that the system of described phytic acid modified straw
Standby process is comprised the following steps:
Step one, dry crushed stalk is acidified in acid solution, is then washed till neutrality, is dried, after being pre-processed
Stalk;
Step 2, is well mixed raw material by following percentage by weight:
30mLN is added to per the pretreated stalks of 2g, in dinethylformamide and is stirred, then sequentially added
The phytic acid of 2.1mL and the urea of 1.2g;
The raw material being well mixed is transferred in reactor, temperature control is fully reacted at 80 DEG C, is taken out, washed, be dried,
Obtain final product phytic acid modified straw.
3. the preparation method of pesticide slow-releasing agent as claimed in claim 2, it is characterised in that in step one, described acid solution
PH be less than 3.
4. the preparation method of pesticide slow-releasing agent as claimed in claim 2, it is characterised in that in step one, described acid solution
For the hydrochloric acid of 0.1mol/L.
5. the preparation method of pesticide slow-releasing agent as claimed in claim 1, it is characterised in that agricultural chemicals is adsorbed onto into the modified straw of phytic acid
Process on stalk is:Phytic acid modified straw is taken, in being added to excessive the pesticide solution, after fully absorption, is filtered, by solid content
After drying, pesticide slow-releasing agent is obtained final product.
6. the preparation method of pesticide slow-releasing agent as claimed in claim 1, it is characterised in that described stalk be wheat stalk,
Rice straw or maize straw.
7. the preparation method of the pesticide slow-releasing agent as described in claim 1 to 6 any claim, it is characterised in that described
Agricultural chemicals is nicotinic insecticide.
8. the preparation method of pesticide slow-releasing agent as claimed in claim 7, it is characterised in that described agricultural chemicals is imidacloprid.
9. a kind of pesticide slow-releasing agent, it is characterised in that the agricultural chemicals corrosion inhibiter is by the way that agricultural chemicals is adsorbed onto on phytic acid modified straw
Made by.
10. pesticide slow-releasing agent as claimed in claim 9, it is characterised in that described agricultural chemicals corrosion inhibiter is using such as claim 1
Make to the preparation method described in 8 any claims.
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Citations (5)
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---|---|---|---|---|
CN102823619A (en) * | 2012-09-20 | 2012-12-19 | 贵州大学 | Imidacloprid sustained-release granules and preparation and application thereof |
CN103461325A (en) * | 2013-06-06 | 2013-12-25 | 黄山市迎客松生物科技有限公司 | Straw-based drug liquid controlled release agent and preparation method thereof |
CN103881033A (en) * | 2014-02-26 | 2014-06-25 | 成都理工大学 | Preparation method of crop straw dye adsorption material |
CN104430323A (en) * | 2014-11-26 | 2015-03-25 | 北京农学院 | Controlled-release pesticide granules |
CN105622298A (en) * | 2014-11-28 | 2016-06-01 | 江阴市联业生物科技有限公司 | Production technology of corn straw composite water absorbing resin slow release urea |
-
2016
- 2016-11-08 CN CN201610981077.0A patent/CN106614553A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102823619A (en) * | 2012-09-20 | 2012-12-19 | 贵州大学 | Imidacloprid sustained-release granules and preparation and application thereof |
CN103461325A (en) * | 2013-06-06 | 2013-12-25 | 黄山市迎客松生物科技有限公司 | Straw-based drug liquid controlled release agent and preparation method thereof |
CN103881033A (en) * | 2014-02-26 | 2014-06-25 | 成都理工大学 | Preparation method of crop straw dye adsorption material |
CN104430323A (en) * | 2014-11-26 | 2015-03-25 | 北京农学院 | Controlled-release pesticide granules |
CN105622298A (en) * | 2014-11-28 | 2016-06-01 | 江阴市联业生物科技有限公司 | Production technology of corn straw composite water absorbing resin slow release urea |
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Title |
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