CN102511480B - Temperature control slow-release cold-resistant seed coating agent and preparing method of cold-resistant agent - Google Patents

Temperature control slow-release cold-resistant seed coating agent and preparing method of cold-resistant agent Download PDF

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CN102511480B
CN102511480B CN201110390123.7A CN201110390123A CN102511480B CN 102511480 B CN102511480 B CN 102511480B CN 201110390123 A CN201110390123 A CN 201110390123A CN 102511480 B CN102511480 B CN 102511480B
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cold
temperature control
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agent
seed
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CN102511480A (en
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胡晋
崔华威
关亚静
祝水金
胡伟民
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Zhejiang University ZJU
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Abstract

The invention provides a temperature control slow-release cold-resistant seed coating agent which is composed of a temperature control slow-release cold-resistant agent and a coating auxiliary material. The temperature control slow-release cold-resistant agent is composed of a temperature control slow-release material and salicylic acid, the temperature control slow-release material is random copolymer of N-isopropyl acrylamide and butyl methacrylate, and mass ratio between the cold-resistant agent and the coating auxiliary material is 0.0015-0.03:1. The invention further provides a preparing method of the temperature control slow-release cold-resistant agent. The temperature control slow-release cold-resistant seed coating agent can give play to temperature control effects of the temperature control slow-release material, controls the cold-resistant agent to be released at a specific temperature so as to guarantee that effective effects of the cold-resistant agent are brought into full play, can saves costs simultaneously, and reduces environmental pollution.

Description

The cold-resistant type seed coat agent of temperature control sustained-release and cold-resistance agent preparation method
Technical field
The present invention relates to agricultural seed and process and packaging technique, be specifically related to a kind of temperature control sustained-release seed coat agent that can improve cold tolerance and preparation method thereof.
Background technology
Early spring, low temperature adverse circumstance all can be brought harm to whole world crop production; tobacco also often can run into low temperature adverse circumstance when sowing early spring; cause seeding ratio reduce, emerge slow, growth of seedling is poor, even makes seed lose germinating capacity completely, causes serious economic loss.The sixties in 20th century, the state such as the U.S., Brazil, Japan started the technical research of tobacco seed pill pelletizing coating, at present, had formed that a whole set of perfect tobacco seed is bred, Pelleting, packing, popularization, marketing system.China promotes tobacco seed-coating pelleted seed since the beginning of the nineties in last century, reached 90% left and right at present in national popularization rate, has got obvious effect in leaf tobacco production.
At present, tobacco seed seed coating medicine effective active composition mainly discharges by flooding mechanism, and pelleted seed is after planting met water and broken, and its active component is with seed and close on soil and contact, and leans on flooding mechanism slowly and freely to discharge.As Chinese patent " tobacco coating seed and preparation method thereof ", number of patent application: 200410022264.3; Patent " coating agent prescription for tobacco seed ", number of patent application: 93103717.4; Patent " a kind of shortening tobacco pelleted seed germinating time and improve cold resistant method ", number of patent application: 200810058970.1; Patent " a kind of production method of biological tobacco type coat pelleted seeds ", number of patent application: 03135484.X.The above-mentioned patent pattern that all adopts active component Spontaneous release without exception, this pattern not only easily causes a large amount of losses of seed coat agent active ingredient, and active component is too short effective acting time.
Because crop has a zero point to the tolerance of cold damage, as worked as temperature lower than 11~13 oduring C, the germination of tobacco seed can be suppressed.Therefore,, if adopt temperature control sustained-release material to control the release of cold-resistance agent, can bring into play to greatest extent the effect of cold-resistance agent in seed coat agent.
Summary of the invention
The object of the invention is to be to overcome existing seed coat agent Spontaneous release active component and active component does not play the shortcoming of due effect completely, provide a kind of temperature control sustained-release cold-resistant type seed coat agent, this seed coat agent can be brought into play the temperature control effect of temperature control sustained-release material to greatest extent, temperature control sustained-release control of material cold-resistance agent is discharged at specific temperature, guarantee that the useful effect of cold-resistance agent is given full play to.Technical scheme provided by the invention is as described below.
The cold-resistant type seed coat agent of a kind of temperature control sustained-release, by temperature control sustained-release cold-resistance agent and dressing auxiliary material, formed, described temperature control sustained-release cold-resistance agent is comprised of temperature control sustained-release material and salicylic acid (SA), described temperature control sustained-release material is the random copolymer (PNIPAm-co-BMA) of NIPA and butyl methacrylate, and the mass ratio of described cold-resistance agent and dressing auxiliary material is 0.0015~0.03:1.
Wherein, in described temperature control sustained-release cold-resistance agent, the mass ratio of salicylic acid and temperature control sustained-release material is 1:2.
Wherein, the mass ratio of described temperature control sustained-release cold-resistance agent and dressing auxiliary material is preferably 0.03:1.
Wherein, described dressing auxiliary material comprises talcum powder and bentonite, the talcum powder that its proportioning is 60%-80% and the bentonite of 20%-40%.
Wherein, the preparation method of described temperature control sustained-release cold-resistance agent comprises the steps:
Get random copolymer (PNIPAm-co-BMA) solid particle of NIPA and butyl methacrylate, be immersed in 2g/L aqueous solution of salicylic acid 3~5 d to swelling equilibrium, the random copolymerization composition granule of the NIPA after swelling and butyl methacrylate must have been wrapped up in vacuum desiccator after 40~50 ℃ of vacuum drying 3~5 d to the random copolymer solid particle of salicylic NIPA and butyl methacrylate, the random copolymer solid particle of the salicylic NIPA of parcel and butyl methacrylate is pulverized, cross 100 mesh sieve holes and obtain cold-resistance agent pressed powder.
The temperature control sustained-release of the cold-resistant type tobacco of temperature control sustained-release provided by the invention seed coat agent and traditional diffusion discharge and have the distinct mechanism of action.In traditional diffusion release mode, cold-resistant type seed coat agent, from planting seed, no matter its effective ingredient of temperature height slowly discharges always, until useful effect composition completely loses, generally loses effect at crop seedling in early days.The cold-resistant type tobacco of the temperature control sustained-release seed coat agent of utilizing temperature control sustained-release material to prepare can accomplish seed coat agent effective ingredient only temperature during lower than certain critical value just response type discharge, thereby can bring into play to greatest extent cold-resistant effect.
The present invention is incorporated into temperature control sustained-release material PNIPAm-co-BMA in the cold-resistant dressing of seed, " on-off " effect by this material in uniform temperature critical point, make cold-resistance agent only when the temperature threshold value lower than certain, just discharge and play a role, while not reaching critical value, do not discharge, the response type of accomplishing cold-resistance agent discharges, this will improve the anti-cold effect effect of seed coat agent greatly, extends action time.Meanwhile, cold-resistant type tobacco seed coat agent can reach crop yield effect by seed coat agent active ingredient still less, makes dressing cost, reduces the pollution to environment.In addition, the prices of raw and semifnished materials of preparing temperature control sustained-release cold-resistance agent are moderate, and 10,000 tobacco seed costs of Pelleting are about 0.44 yuan, can significantly not increase pelleted seed cost, have feasibility economically for tobacco seed Pelleting.
Accompanying drawing explanation
Fig. 1 is that temperature control sustained-release cold-resistance agent is 10 ℃ and 20 ℃ of rates of release that replace SA under temperature match curing conditions.
Embodiment
In following embodiment, the seed of tobacco bred " the large gold dollar of safflower " and " MS K326 " is from China Tobacco Seed Yuxi Co., Ltd..Bentonite and talcum powder are from China Tobacco Seed Yuxi Co., Ltd., and carboxymethyl cellulose is purchased from Hangzhou Huadong Medicine Group Co.,Ltd.The model of seed-coating machine is BY300A, purchased from Shanghai Xin Nuo instrument and equipment Co., Ltd.
embodiment 1the preparation of temperature control sustained-release material
Under nitrogen protection, in 100 ml wide-mouth bottles, add successively 45 ml deionized waters, 5 g poly-N-isopropyl acrylamide crystal, 0.81 g butyl methacrylate monomer, 0.136 g crosslinking agent N, N '-methylene-bisacrylamide and 0.125 g initator azodiisobutyronitrile.Wide-mouth bottle is placed in 50 ℃ of thermostat water baths and reacts 12h, takes out product PNIPAm-co-BMA from wide-mouth bottle, and taking-up product by its fragmentation, obtains weight approximately 0.1~0.5 g particle with scissors.Particle after fragmentation is first soaked in to 5 d in deionized water, then takes out and to be soaked in 5 d in methyl alcohol, to remove impurity.Take out the PNIPAm-co-BMA after soaking, in vacuum desiccator, after 40~50 ℃ of vacuum drying 3~5 d, obtain PNIPAm-co-BMA solid particle.
When prepared by temperature control sustained-release material, according to the difference of butyl methacrylate amount of monomer, its responsive to temperature point is different, and when temperature reaches or during lower than its sensitive temperature, macromolecular material deformation can occur and expands, internal voids strengthens, and internal package logistics goes out.The temperature control sustained-release material of preparing with embodiment 1 method will reach or play a role during lower than 15 ℃ in temperature.
embodiment 2the preparation of temperature control sustained-release cold-resistance agent
Get the PNIPAm-co-BMA solid particle of 4 grams of embodiment, 1 preparation, be immersed in 2g/L aqueous solution of salicylic acid 1.0L 4 d to swelling equilibrium, PNIPAm-co-BMA random copolymerization composition granule after swelling must have been wrapped up in vacuum desiccator after 40~50 ℃ of vacuum drying 4 d to salicylic PNIPAm-co-BMA random copolymer solid particle, 100 mesh sieve holes are pulverized, crossed to the salicylic PNIPAm-co-BMA random copolymer of parcel solid particle and obtain cold-resistance agent pressed powder.Wherein the mass ratio of salicylic acid and slow-release material PNIPAm-co-BMA random copolymer is 1:2.
Shown in Fig. 1, the temperature control sustained-release drought resistance agent of embodiment 2 preparation is in the time of 10 ℃, due to lower than its sensitive temperature point, therefore its inner salicylic rate of release obviously increases, and when temperature is 20 ℃, salicylic acid rate of release obviously reduces, and all maintain a lower level.Along with the prolongation of time, SA rate of release reduces at 10 ℃, but all the time higher than 20 ℃.
embodiment 3the preparation of tobacco pelleted seed
The PNIPAm-of SA will be loaded co-BMA powder is with dressing auxiliary material in mass ratio for 0.0015:1 mixes, and dressing auxiliary material is comprised of 70g talcum powder and 30g bentonite, obtains the cold-resistant type tobacco of temperature control sustained-release seed coat agent.
Get large gold dollar seed 2 g of tobacco bred safflower, be poured into seed-coating machine, the moistening the surface of the seed of spraying clear water, adds the cold-resistant type tobacco of 0.1g temperature control sustained-release seed coat agent, constantly stirs and makes it to be wrapped in the surface of the seed, repeats above-mentioned steps 3~5 times, forms small pill shape.Then add the cold-resistant type tobacco of 0.4g-1g temperature control sustained-release seed coat agent, spray adhesive, constantly stirs, and makes pill shape seed particle size be increased to gradually 1.60 mm~1.80 mm at every turn.Then screening, polishing, colouring, the dry complete seed of dressing that obtains.
Separately get MS K326 seed 2 g, the dressing operation through same, obtains MS K326 pelleted seed finished product.
All pelleted seeds are dry, and to be placed on 4 ℃ of Refrigerator stores standby.
embodiment 4the preparation of tobacco pelleted seed
The flow process that repeats embodiment 3, unique different, in embodiment 3, will load the PNIPAm-of SA co-BMA powder and dressing auxiliary material mass ratio are made as 0.0075:1.
embodiment 5the preparation of tobacco pelleted seed
The flow process that repeats embodiment 3, unique different, in embodiment 3, will load the PNIPAm-of SA co-BMA powder and dressing auxiliary material mass ratio are made as 0.03:1.
embodiment 6tobacco pelleted seed germinates
Get embodiment 3-5 gained tobacco pelleted seed and carry out seed sprouting and growth of seedling test, for the ease of representing, embodiment 3 gained tobacco pelleted seeds are referred to as T 1, embodiment 4 gained tobacco pelleted seeds are referred to as T 2, embodiment 5 gained tobacco pelleted seeds are referred to as T 3.Meanwhile, in order to study the PNIPAm-that loads SA co-BMA is with respect to independent use SA or PNIPAm- cothe advantage of-BMA, has prepared again 7 kinds of pelleted seeds in contrast, respectively with CK1, and CK2 ... CK7 represents, the Pelleting method of control group seed is with embodiment 3, and the concrete formula of all processing is in Table 1.Dressing auxiliary material is wherein comprised of 70% talcum powder and 30% bentonite.
Table 1 test treatment formulations
Process Dressing auxiliary material (g) SA(g) PNIPAm- co-BMA(g)
CK1 100 0 0
CK2 100 0 0.10
CK3 100 0 0.50
CK4 100 0 2
CK5 100 0.05 0
CK6 100 0.25 0
CK7 100 1 0
T 1 100 0.05 0.10
T 2 100 0.25 0.50
T 3 100 1 2
The germination condition of 3 processing and 7 contrast seeds is: adopt on paper and germinate, 100 seeds of every processing, repeat for 4 times.20~30 ℃ of alternating temperature germination 7d, then proceed to 11 ℃ of low temperature stress 5d, and last 20~30 ℃ of recoveries grow into 16d, illumination every day 12 hours.The 16th d calculates germination rate, germination index (GI) and average germinating time (MGT).Computing formula: GI=∑ ( gt/ dt), MGT=∑ gtDt/ ∑ gt, in formula: gtbe tit chitting piece number, dtfor germination number of days.
The growth conditions of 3 processing and 7 contrast seedling is: adopt on long-term paper and germinate, 100 seeds of every processing, repeat for 4 times.20~30 ℃ of alternating temperature growth 16d, then proceed to 11 ℃ of low temperature stress 16d, and last 20~30 ℃ of alternating temperatures recover growth 8d, illumination every day 12 hours.40d measures root length, full stand length, full stand fresh weight and full stand dry weight.Get the seedling of growth 40d, after rinsing with running water, with filter paper, blot excessive moisture, with ruler, measure the length of its root and full stand; With one thousandth sensibility reciprocal balance, weigh full stand fresh weight, seedling is dried at 80 ℃ to 24 h, measure seedling gross dry weight.
Due to when temperature is during lower than 11~13 ℃, the germination of tobacco seed can be suppressed, and what therefore experiment adopted is 11 ℃ of low temperature, and this temperature both can make seed sprouting suppressed, can not stop again the growth of seed completely, made seedling in a kind of low temperature stress state.And the temperature control sustained-release cold-resistance agent that we adopt, it reaches or just can play a role during lower than 15 ℃, and therefore, it is rational in experiment, adopting 11 ℃ of low temperature.
Result shows, pelleted seed prepared by the present invention is compared with conventional pelleted seed, can significantly improve the large gold dollar of safflower and MS K326 germination rate and the germination index under low temperature stress, shortens average germinating time (table 2, table 5).T wherein 3effect is best, and germination rate and germination index are significantly higher than 7 contrasts, and average germinating time is lower than 7 contrasts.CK2, CK3, CK4 compare with CK1, and germination rate, germination index and average germinating time are without significant difference.CK7 compares germination rate with CK1 and germination index significantly reduces, and average germinating time is elongated.From seedling root length, height of seedling and seedling dry weight and fresh weight of plant seedlings, T 1, T 2and T 3effect integral body be better than 7 contrasts (table 3, table 4, table 6, table 7).Wherein, the large gold dollar T of safflower 3long, the fresh and dried weight average of seedling of root be significantly higher than all the other 9 processing (table 3, table 4).And MS K326 T 3long, the seedling dry weight and fresh weight of plant seedlings of root be also significantly higher than all the other 9 processing, height of seedling is significantly higher than except CK6 and T 2outer 7 processing (table 6, table 7), show T 3for preferably processing.
The different Pelletings of table 2 are processed the large gold dollar seed sprouting impact of tobacco bred safflower under low temperature adverse circumstance
Process GP(%) GI MGT(d)
CK1 72.0 d * 11.93 de 7.12 ab
CK2 73.2 cd 12.15 d 6.61 bc
CK3 74.0 cd 11.49 e 7.56 a
CK4 74.8 cd 11.43 e 6.89 bc
CK5 75.5 cd 12.34 cd 6.70 bc
CK6 88.4 b 14.45 b 6.73 bc
CK7 46.5 e 7.66 f 7.69 a
T 1 77.4 c 12.83 c 6.78 bc
T 2 89.2 ab 15.08 a 6.55 bc
T 3 93.4 a 14.90 ab 6.45 c
* the lowercase after data represents the significance of difference (α=0.05, Lsd test) between same breed different disposal, lower same.
The impact of and height of seedling long on the large gold dollar seedling of tobacco safflower root under low temperature adverse circumstance is processed in the different Pelletings of table 3
Process Root long (mm) Height of seedling (mm)
CK1 9.75 c 22.22 d
CK2 9.68 c 22.61 cd
CK3 9.51 c 22.72 cd
CK4 9.74 c 22.38 d
CK5 9.89 bc 23.36 bc
CK6 10.38 b 24.26 ab
CK7 8.70 d 20.52 e
T 1 10.01 bc 22.71 cd
T 2 10.44 b 24.44 a
T 3 11.04 a 24.82 a
The impact on tobacco safflower large gold dollar seedling fresh weight and dry weight under low temperature adverse circumstance is processed in the different Pelletings of table 4
Process Fresh weight (g/50plant) Dry weight (g/50plant)
CK1 0.815 c 0.087 d
CK2 0.818 c 0.086 d
CK3 0.819 c 0.087 d
CK4 0.836 c 0.089 d
CK5 0.831 c 0.090 cd
CK6 0.906 b 0.096 b
CK7 0.589 d 0.064 e
T 1 0.899 b 0.096 b
T 2 0.903 b 0.095 bc
T 3 0.980 a 0.103 a
The different Pelletings of table 5 are processed tobacco MS K326 seed sprouting impact under low temperature adverse circumstance
Process GP(%) GI MGT(d)
CK1 72.5 ef 10.94 de 7.57 b
CK2 73.2 ef 10.85 e 7.51 b
CK3 71.1 f 11.65 cd 7.46 b
CK4 72.0 ef 10.92 de 7.74 b
CK5 79.2 cd 12.02 bc 7.77 b
CK6 82.2 bc 12.27 bc 7.96 b
CK7 36.8 g 4.72 f 9.21 a
T 1 75.5 de 11.81 c 7.90 b
T 2 83.6 b 12.7 b 7.39 bc
T 3 91.9 a 14.12 a 6.80 c
The impact of and height of seedling long on tobacco MS K326 seedling root under low temperature adverse circumstance is processed in the different Pelletings of table 6
Process Root long (mm) Height of seedling (mm)
CK1 7.21 e 16.82 c
CK2 7.27 e 16.67 c
CK3 6.95 e 17.11 bc
CK4 7.58 de 17.23 bc
CK5 7.93 cd 17.61 bc
CK6 8.55 bc 20.48 a
CK7 6.02 f 15.29 d
T 1 7.97 cd 18.06 b
T 2 9.04 b 21.05 a
T 3 9.98 a 21.52 a
The impact on tobacco MS K326 seedling fresh weight and dry weight under low temperature adverse circumstance is processed in the different Pelletings of table 7
Process Fresh weight (g/50plant) Dry weight (g/50plant)
CK1 0.755 c 0.095 c
CK2 0.752 c 0.094 c
CK3 0.754 c 0.095 c
CK4 0.789 bc 0.099 bc
CK5 0.765 c 0.099 bc
CK6 0.833 b 0.104 b
CK7 0.542 d 0.071 d
T 1 0.809 bc 0.104 b
T 2 0.831 b 0.103 b
T 3 0.895 a 0.111 a
By test data analyzer, learnt, PNIPAm-co-BMA has no adverse effects to seed germination, belongs to comparatively green macromolecular material.And in dressing pulvis, directly add salicylic acid, seed germination under low temperature stress and growth of seedling be there is no to obvious facilitation, and when Determination of Salicylic Acid is higher, seed sprouting is had to harmful effect.And when salicylic acid is loaded into PNIPAm- coafter-BMA, to seed pelleting, it produces obvious facilitation to the seed germination under low temperature stress and growth of seedling, and PNIPAm-is described when temperature reaches 11 ℃ co-BMA just can discharge salicylic acid wherein, makes salicylic acid just when low temperature, bring into play its function.If there is no PNIPAm- cothe temperature-sensitive of-BMA is controlled, and salicylic acid just discharges in advance at ambient temperature, if seed cold hardiness be there is no to remarkable facilitation during its low concentration, if not only can not bring into play its cold-resistant function when its concentration is high, unfavorable to seed sprouting on the contrary.

Claims (4)

1. the cold-resistant type seed coat agent of temperature control sustained-release, it is characterized in that, by temperature control sustained-release cold-resistance agent and dressing auxiliary material, formed, described temperature control sustained-release cold-resistance agent is comprised of temperature control sustained-release material and salicylic acid, described temperature control sustained-release material is the random copolymer of NIPA and butyl methacrylate, and their mass ratio is 500:81, described temperature control sustained-release cold-resistance agent and the mass ratio of dressing auxiliary material are 0.0015~0.03:1.
2. the cold-resistant type seed coat agent of temperature control sustained-release as claimed in claim 1, is characterized in that, in described temperature control sustained-release cold-resistance agent, the mass ratio of salicylic acid and slow-release material is 1:2.
3. the cold-resistant type seed coat agent of temperature control sustained-release as claimed in claim 1, is characterized in that, described dressing auxiliary material comprises talcum powder and bentonite, the talcum powder that its proportioning is 60%~80% and 20%~40% bentonite.
4. the cold-resistant type seed coat agent of temperature control sustained-release as described in claim 1-3 any one, is characterized in that, described temperature control sustained-release cold-resistance agent and the mass ratio of dressing auxiliary material are preferably 0.03:1.
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