CN101438701B - Film-forming agent for seed-coating containing polyvinyl alcohol and oxidized starch-acrylamide copolymer - Google Patents
Film-forming agent for seed-coating containing polyvinyl alcohol and oxidized starch-acrylamide copolymer Download PDFInfo
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- CN101438701B CN101438701B CN2008100801095A CN200810080109A CN101438701B CN 101438701 B CN101438701 B CN 101438701B CN 2008100801095 A CN2008100801095 A CN 2008100801095A CN 200810080109 A CN200810080109 A CN 200810080109A CN 101438701 B CN101438701 B CN 101438701B
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- polyvinyl alcohol
- oxidized starch
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Abstract
The invention relates to a polyvinyl alcohol-containing and oxidized starch-acrylamide copolymer-containing film agent in seed coating formulation which comprises: 0.2 to 1.2 percent of polyvinyl alcohol, oxidized starch-acrylamide copolymer which is obtained by polymerizing 5 percent of oxidized starch and 3.8 percent to 4.8 percent of acrylamide under the existence of 0.1 percent of ammonium persulfate, and water 100 percent of compensation. The preparation method thereof comprises the following steps: firstly, the polyvinyl alcohol is soaked by part of the water for 60 min to 90 min, then is added with the oxidized starch, the acrylamide and the ammonium persulfate by stirring, evenly mixed, heated to a temperature of 80 DEG C to 90 DEG C to react for 30 min to 60 min, then is added with the residual water, evenly stirred and is cooled to the room temperature to obtain the film agent in seed coating formulation. The film agent has the advantages of firm sticking, remarkably enhanced uniformity, low production cost, easy degrading and small harm to the environment.
Description
Technical field
The present invention relates to a kind of suspension seed-coating agent film forming agent, relate in particular to a kind of kind clothing agent film forming agent, the invention still further relates to the preparation method of this kind clothing agent film forming agent to make behind oxidized starch-acrylamide copolymer and the polyvinyl alcohol blending.
Background technology
The agent of kind of clothing is a kind of pesticidal preparations that is used for crop or other plant seed Cotton seeds, has film forming characteristics.Its composition mainly is divided into two parts, the one, agricultural chemicals, little fertilizer, hormone isoreactivity composition, be kind of the active ingredient that the clothing agent directly plays a role, the 2nd, non-active ingredients such as film forming agent, stabilizing agent, bleeding agent are the important component that can solidify to form film when keeping kind of the physics of clothing agent and chemical property, dressing at the surface of the seed.Wherein film forming agent is the component of most critical, and its principal security kind clothing agent has certain viscosity, good film forming and the suitable clothing film fastness and the uniformity, also is the key component that guarantees active component slowly-releasing in the clothing film.
Traditional kind clothing film forming agent mainly comprises synthetic macromolecular compound and natural polymer.The former comprises polyvinyl acetate, polyethylene/acetate ethylene copolymer, polyvinyl alcohol or copolymer, polyacrylate, polyacrylate, polyacrylamide etc., its film forming, water penetration and swelling are all better, but belong to non-renewable resources, biological degradability is poor, and the production cost height.The latter comprises cellulose and derivative (as cellulose acetate, HPMC, L-HPC, ethyl cellulose, methylcellulose, microcrystalline cellulose etc.) thereof, macromolecule polysaccharide compound (as chitin, starch, modified starch etc.).Modified starch has characteristics such as low, the bonding fastness of cost is strong, biodegradability good, genus renewable resources, but film forming and the resistance to water used separately are relatively poor, can not use as kind of clothing agent film forming agent separately.
Summary of the invention
The purpose of this invention is to provide a kind of kind clothing agent film forming agent that contains polyvinyl alcohol and oxidized starch-acrylamide copolymer,, reduce kind of the production cost of clothing agent film forming agent simultaneously with resistance to water and the film forming that improves oxidized starch.
The above-mentioned preparation method who contains the kind clothing agent film forming agent of polyvinyl alcohol and oxidized starch-acrylamide copolymer is provided, and is another goal of the invention of the present invention.
For achieving the above object, the present invention makes film forming agent with polyvinyl alcohol blending again with oxidized starch and acrylamide copolymerization, has reached the requirement of suspension seed-coating agent production standard fully through evidence.
The kind clothing agent film forming agent that contains polyvinyl alcohol and oxidized starch-acrylamide copolymer of the present invention composed as follows:
A. polyvinyl alcohol, consumption is 0.2～1.2%;
B. oxidized starch-acrylamide copolymer is the mixture copolymer that polymerization obtains in the presence of 0.1% ammonium persulfate by 5.0% oxidized starch and 3.8～4.8% acrylamides;
C. water supplies 100%;
All percentages are percetage by weight.
Wherein, described polyvinyl alcohol selects that alcoholysis degree is 90～98% for use, the degree of polymerization is 1700～1800 product.
The preparation method that the present invention contains the kind clothing agent film forming agent of polyvinyl alcohol and oxidized starch-acrylamide copolymer steeps 60～90min with polyvinyl alcohol with the part water logging earlier, under agitation add oxidized starch, acrylamide and ammonium persulfate, mix, be heated to 80～90 ℃ of reaction 30～60min, add the residue water gaging, stir, be cooled to room temperature, obtain kind of a clothing agent film forming agent.
Wherein, in order to make oxidized starch and acrylamide polymerization can take place better, be polyvinyl alcohol to be added to account in half the water of Total Water earlier to soak among the preparation method of the present invention.
Advantage of the present invention is that the kind clothing agent film forming agent for preparing is compared with existing commercial polyvinyl alcohol film forming agent, under the film forming prerequisite close with film formation time, bonding firmly and the uniformity all be significantly improved, the production cost of film forming agent especially of the present invention is low, after planting easily degraded is little to environmental hazard.
Film forming agent of the present invention is tested according to national standard " GB/T17768-1999 " (the suspension seed-coating agent product standard is write standard) through plant protection research institute of the Chinese Academy of Agricultural Sciences; use according to conventional amount used 1.5～2.5%; the preparation expulsion rate is on average below 1.88%; coating uniformity is on average more than 76.25%; film formation time 2.4～3.0min; percentage of seedgermination meets the index request of national standard more than 99.00% fully.
Embodiment
Embodiment 1
Getting the 0.2g polyvinyl alcohol joins in the 50g water, soak 60min, under constantly stirring, add 5.0g oxidized starch, 4.8g acrylamide and 0.1g ammonium persulfate, mix, be heated to 85 ℃, sustained response 45min, after thing to be mixed was uniform liquid, supplying water again was 100g to gross mass, stirs, be cooled to room temperature, make solid content and be 10% kind clothing agent film forming agent.
Embodiment 2
Getting the 0.6g polyvinyl alcohol joins in the 50g water, soak 80min, under constantly stirring, add 5.0g oxidized starch, 4.4g acrylamide and 0.1g ammonium persulfate, mix, be heated to 82 ℃, sustained response 55min, after thing to be mixed was uniform liquid, supplying water again was 100g to gross mass, stirs, be cooled to room temperature, make solid content and be 10% kind clothing agent film forming agent.
Embodiment 3
Getting the 1.2g polyvinyl alcohol joins in the 50g water, soak 90min, under constantly stirring, add 5.0g oxidized starch, 3.8g acrylamide and 0.1g ammonium persulfate, mix, be heated to 90 ℃, sustained response 30min, after thing to be mixed was uniform liquid, supplying water again was 100g to gross mass, stirs, be cooled to room temperature, make solid content and be 10% kind clothing agent film forming agent.
Embodiment 4
The film forming agent of selecting embodiment 1, embodiment 3 to make respectively is an experimental group, with the polyvinyl alcohol film forming agent is control group, and according to conventional method, choosing carbendazim commonly used in the current kind of clothing agent is active component, being added into other must component, and sand milling is pulverized and made kind of a clothing agent.
According to national standard " GB/T17768-1999 " (the suspension seed-coating agent product standard is write standard), the film forming of above-mentioned 3 all clothing agent is measured.
Take by weighing corn seed 50g (being accurate to 0.01g) in conical flask, draw sample 1g, be injected into shake 5min in the conical flask, open and flat the opening of capsuled seed made its film forming, stir seed, observe the surface of the seed with glass bar with liquid-transfering gun.If the kind clothing agent of all thes surface of the seed is film-forming, then film forming is qualified.
When being film forming agent with embodiment 1, embodiment 3 and polyvinyl alcohol, the film formation time behind the preparation dressing sees Table 1.
The film formation time measurement result of table 1 suspension seed-coating agent
As can be seen from Table 1, with embodiment 1, embodiment 3 and polyvinyl alcohol be film formation time behind the kind clothing agent dressing corn seed of film forming agent between 2.4～3min, the film formation time between different disposal is all very fast, the film formation time amplitude of variation is little.Compare with the film formation time of conventional film forming agent polyvinyl alcohol, embodiment 1 film formation time behind the dressing and contrast in 1.5～3.6% amount ranges do not have significant difference; The consumption of embodiment 3 is 3.6% o'clock, preparation dressing film formation time is significant difference compared with the control, but the film formation time of also only comparing photograph increases 0.5min, is under 1.5～2.5% consumptions at embodiment 3, and the film formation time of preparation does not then have significant difference (α=0.05) with contrast.
Embodiment 5
According to national standard " GB/T17768-1999 " (the suspension seed-coating agent product standard is write standard), the dressing expulsion rate of above-mentioned 3 all clothing agent is measured.
Take by weighing 3g (being accurate to 0.001g) and measure 2 parts of capsuled seeds behind the film forming, place centrifuge tube respectively, the a 30mL chloroform that accurately adds is jumped a queue, and places the ultrasonic cleaner 10min that vibrates, the kind clothing agent of seed appearance is fully dissolved, take out static 10min, get supernatant 2.0mL in the 10mL volumetric flask, be settled to scale with chloroform, shake up, be solution A.
Another part is placed on the oscillator, behind the vibration 10min, carefully seed is taken out in another centrifuge tube, obtain solution B by the disposal methods of solution A.
Make reference with chloroform, measure solution A and the absorbance of solution B under the 511nm wavelength respectively with ultraviolet specrophotometer.
More than measure and repeat 3 times, average.
Expulsion rate behind the dressing (X1) is calculated as follows:
In the formula: m0---the quality of seed behind the obtain solution dressing that A takes by weighing;
M1---the quality of seed behind the obtain solution dressing that B takes by weighing;
The absorbance of A0---solution A;
The absorbance of A1---solution B.
The dressing expulsion rate measurement result of 3 all clothing agent sees Table 2.
The dressing expulsion rate measurement result of table 2 suspension seed-coating agent
As can be seen from Table 2, the dressing expulsion rate of testing sample is all below 2.6%, and show through variance analysis, difference between the dressing expulsion rate measurement result of embodiment 1, embodiment 3 is handled under different amounts is not remarkable, with the expulsion rate difference of contrast polyvinyl alcohol also not significantly (α=0.05).Therefore, as film forming agent, the dressing fastness is very good, difficult drop-off behind the medicament dressing with embodiment 1 and embodiment 3.
Embodiment 6
According to national standard " GB/T17768-1999 " (the suspension seed-coating agent product standard is write standard), the coating uniformity of above-mentioned 3 all clothing agent is measured.
Get 20 in the seed measured behind the film forming at random, place 20 10mL centrifuge tubes with cover respectively, accurately add the 5mL chloroform with pipette in each centrifuge tube, add a cover, behind the shaking out 15min, leave standstill and the centrifugal red liquid that obtains clarifying, make reference, measure its absorbance under the 511nm wavelength with ultraviolet specrophotometer with chloroform.
20 absorbance datas that record are arranged from small to large, and to calculate its mean light absorbency value be Aa.Sample coating uniformity (X2) is calculated as follows:
In the formula: n---record the pelleted seed subnumber of absorbance A in 0.7～1.3Aa scope;
20---test dressing seed number.
The coating uniformity measurement result of 3 all clothing agent sees Table 3.
The coating uniformity measurement result of table 3 suspension seed-coating agent
Annotate: 1.Aa is the absorbance mean value of 20 samples;
2. (0.7～1.3) Aa is 0.7～1.3 times of 20 sample absorbance mean values;
Measure in the sample sample number of absorbance in (0.7～1.3) Aa 3.n be 20.
As can be seen from Table 3, embodiment 1 and embodiment 3 are during as film forming agent, and the coating uniformity of planting the clothing agent formulation reduces gradually with the increase of consumption.The dressing homogeneous phase ratio of preparation when being film forming agent with the contrast polyvinyl alcohol, the consumption of embodiment 3 is 1.5～3.6% o'clock, coating uniformity is significantly better than contrast; The consumption of embodiment 1 is 1.5～2.5% o'clock, and coating uniformity is significantly better than contrast, and is identical with the coating uniformity of contrast when consumption 3.6%, even 50%.Therefore, from the coating uniformity index analysis, when embodiment 1 and embodiment 3 used as kind clothing agent film forming agent, the coating uniformity of preparation was better than contrasting polyvinyl alcohol.
Claims (4)
1. kind clothing agent film forming agent that contains polyvinyl alcohol and oxidized starch-acrylamide copolymer, it is composed as follows:
A. polyvinyl alcohol, consumption is 0.2～1.2%;
B. oxidized starch-acrylamide copolymer is the mixture copolymer that polymerization obtains in the presence of 0.1% ammonium persulfate by 5.0% oxidized starch and 3.8～4.8% acrylamides;
C. water supplies 100%;
All percentages are percetage by weight.
2. the kind clothing agent film forming agent that contains polyvinyl alcohol and oxidized starch-acrylamide copolymer according to claim 1 is characterized in that described polyvinyl alcohol selects that alcoholysis degree is 90～98% for use, the degree of polymerization is 1700～1800 product.
3. the described preparation method who contains the kind clothing agent film forming agent of polyvinyl alcohol and oxidized starch-acrylamide copolymer of claim 1, be earlier polyvinyl alcohol to be steeped 60～90min with the part water logging, under agitation add oxidized starch, acrylamide and Ammonium Persulfate 98.5, mix, be heated to 80～90 ℃ of reaction 30～60min, add the residue water gaging, stir, be cooled to room temperature, obtain kind of a clothing agent film forming agent.
4. the preparation method who contains the kind clothing agent film forming agent of polyvinyl alcohol and oxidized starch-acrylamide copolymer according to claim 3 is characterized in that elder generation's half immersion polyvinyl alcohol with Total Water.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2008100801095A CN101438701B (en) | 2008-12-12 | 2008-12-12 | Film-forming agent for seed-coating containing polyvinyl alcohol and oxidized starch-acrylamide copolymer |
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| CN2008100801095A CN101438701B (en) | 2008-12-12 | 2008-12-12 | Film-forming agent for seed-coating containing polyvinyl alcohol and oxidized starch-acrylamide copolymer |
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| CN101438701A CN101438701A (en) | 2009-05-27 |
| CN101438701B true CN101438701B (en) | 2011-08-17 |
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| US9174871B2 (en) | 2012-11-02 | 2015-11-03 | Empire Technology Development Llc | Cement slurries having pyranose polymers |
| US9238774B2 (en) | 2012-11-02 | 2016-01-19 | Empire Technology Development Llc | Soil fixation, dust suppression and water retention |
| US9212245B2 (en) | 2012-12-04 | 2015-12-15 | Empire Technology Development Llc | High performance acrylamide adhesives |
| CN103329890B (en) * | 2013-07-04 | 2014-08-20 | 黑龙江省新兴农药有限责任公司 | Film-forming agent of flowable seed coating formulation and preparation method thereof |
| CN104839198B (en) * | 2015-03-20 | 2017-05-10 | 山西省农业科学院植物保护研究所 | Thermosensitive pesticide slow release agent for preventing and treating carposina niponensis walshingham |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4983390A (en) * | 1987-04-01 | 1991-01-08 | Lee County Mosquito Control District | Terrestrial delivery compositions and methods for controlling insect and habitat-associated pest populations in terrestrial environments |
| CN101182267A (en) * | 2007-11-16 | 2008-05-21 | 沈阳农业大学 | Organic-inorganic compound fertilizer integument liquid and method for manufacturing the same |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4983390A (en) * | 1987-04-01 | 1991-01-08 | Lee County Mosquito Control District | Terrestrial delivery compositions and methods for controlling insect and habitat-associated pest populations in terrestrial environments |
| CN101182267A (en) * | 2007-11-16 | 2008-05-21 | 沈阳农业大学 | Organic-inorganic compound fertilizer integument liquid and method for manufacturing the same |
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