CN103374105B - Preparation method of soybean seed soaking drought resistance agent - Google Patents

Preparation method of soybean seed soaking drought resistance agent Download PDF

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Publication number
CN103374105B
CN103374105B CN201210122933.9A CN201210122933A CN103374105B CN 103374105 B CN103374105 B CN 103374105B CN 201210122933 A CN201210122933 A CN 201210122933A CN 103374105 B CN103374105 B CN 103374105B
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China
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drought resistance
preparation
resistance agent
seed soaking
soybean seed
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Expired - Fee Related
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CN201210122933.9A
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CN103374105A (en
Inventor
严登华
宋新山
吴迪
杨贵羽
肖伟华
杨志勇
鲁帆
李传哲
于赢东
张鹏
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China Institute of Water Resources and Hydropower Research
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China Institute of Water Resources and Hydropower Research
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Abstract

The invention relates to a preparation method of a soybean seed soaking drought resistance agent. The preparation method of the soybean seed soaking drought resistance agent comprises the following steps: gelatinizing straw powder and water in a microwave oven, wherein the reaction power is 450-550w; cooling the gelatinized straw and adding acrylic acid and acrylic amide, calcium chloride, sodium hydroxide, an initiator and a cross-linking agent; reacting in the microwave oven under the condition that the reaction power is 550-700w; removing reactants which are not reacted and drying; and crushing to obtain the soybean seed soaking drought resistance agent. The soybean seed soaking drought resistance agent disclosed by the invention is simple in synthetic method, short in synthetic time and harmless to the environment, can change wastes into valuable things, and can be degraded.

Description

The preparation method of soybean seed soaking drought resistance agent
Technical field
The present invention relates to a kind of soybean seed soaking drought resistance agent preparation method, particularly relate to a kind of with stalk be one of raw material soybean seed soaking drought resistance agent preparation method.
Background technology
Shi Ge large agricultural country of China is also the country of a water resources relative shortage simultaneously.Because process water and urban water consumption constantly increase, agricultural water is less gradually.In China's history, agricultural arid often causes very large social disaster.According to statistics for many years, the occurrence frequency of China's Droughts is improving constantly in recent years, and Droughts area constantly expands, and farm crop Droughts becomes number also in increase trend.Especially, under the overall background of Global climate change, arid can strengthen further for the impact of agriculture production.Soybean is a kind of important rural economy crop, and China is the native place of soybean, and northeast, main product ground is one of area of optimum kind soybean in the world.China soybean mainly relies on import in recent years, and therefore, the output improving China soybean is extremely urgent.The change of environment, soil drought all can cause very large difficulty to soybean growth of emerging.In raising traditional water conservancy engineering efficiency, while improving farming measures, drought resistance agent product is utilized to increase crop drought resistance ability, under equal aridic moisture condition, the research direction using the crop of drought resistance agent significantly can reduce production loss to become new.
In existing drought resistance agent, the drought resistance agent of Handilong to be a kind of with xanthohumic acid be main raw, drought resisting is respond well.Also be used alone inorganic calcium salt to keeping crop seedling from drought of soaking seed, but effect is unsatisfactory.
Summary of the invention
The object of this invention is to provide the preparation method of a kind of soybean seed soaking drought resistance agent.
The preparation method of soybean seed soaking drought resistance agent provided by the present invention, comprising:
In microwave oven, make stalk powder and water gelatinization, reaction power is 450 ~ 550w;
By the stalk cooling after gelatinization, add vinylformic acid and acrylamide, calcium chloride, sodium hydroxide, initiator and linking agent, then react under microwave oven inner reaction power is 550 ~ 700w condition;
Remove unreacted reactant with anhydrous methanol, dry, pulverize and obtain soybean seed soaking drought resistance agent.
In the preparation method of soybean seed soaking drought resistance agent of the present invention, described stalk is be selected from one or more in maize straw, wheat stalk, rice straw.
In the preparation method of soybean seed soaking drought resistance agent of the present invention, the mass ratio of described stalk powder and described water is 1: 100 ~ 1: 250.
In the preparation method of soybean seed soaking drought resistance agent of the present invention, the mass ratio of described vinylformic acid and acrylamide is 1: 2 ~ 1: 4.
In the preparation method of soybean seed soaking drought resistance agent of the present invention, the amount of described calcium chloride is 10% ~ 30% of vinylformic acid and acrylamide total mass.
In the preparation method of soybean seed soaking drought resistance agent of the present invention, described degree of neutralization is 80%.
In the preparation method of soybean seed soaking drought resistance agent of the present invention, the step of the unreacted reactant of described removal for soak in anhydrous methanol.
In the preparation method of soybean seed soaking drought resistance agent of the present invention, the amount of described initiator is 1% of vinylformic acid and acrylamide total mass, and the amount of described linking agent is 1% of vinylformic acid and acrylamide total mass.
In the preparation method of soybean of the present invention seed soaking drought resistance agent, described stalk powder by by stalk 105 DEG C of oven dry, then pulverize acquisition.
The present invention utilizes waste straw as one of raw material obtained soybean seed soaking drought resistance agent.This soybean seed soaking drought resistance agent can form water membrane at seed-coat, absorption surrounding water molecules, and the growth utilizing calcium ion promotion seed germination early stage is to improve bud ratio.Drought resistance agent synthetic method of the present invention is simple, and generated time is short, can turn waste into wealth, degradable, environmental sound.
Accompanying drawing explanation
Fig. 1 represents the building-up process of soybean seed soaking drought resistance agent.
Fig. 2 represents the infrared spectrogram of soybean seed soaking drought resistance agent
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1 prepares soybean seed soaking drought resistance agent
(1) pulverize: discarded stalk (maize straw) is put to the oven dry of 105 degrees Celsius, baking oven, is pulverized with pulverizer, cross 200 mesh sieves (0.074mm), obtain stalk powder;
(2) gelatinization: the stalk powder 0.2g getting gained in step (1) at normal temperatures, add a small amount of distilled water, stalk powder and the mass ratio added water are about 1: 250, then put high fiery gelatinization to microwave oven (power is 450w) 3 minutes;
(3) Microwave synthesize: the Mierocrystalline cellulose of gelatinization is put in atmosphere to normal temperature, add 3.6ml vinylformic acid (relative density is 1.049 ~ 1.055) successively, 26.7ml acrylamide soln (concentration is 4mol/L), 0.567g calcium chloride powder (calcium chloride quality is 5% of monomer mass), 4.2ml sodium hydroxide solution (massfraction is 40%), 1.0ml ammonium persulfate solution (concentration is 0.5mol/L), 2.9ml N, N-methylene-bisacrylamide solution (concentration is 0.25mol/L), in microwave oven, high fire (power is 550w) reacts 5 minutes,
(4) drought resistance agent is obtained: the anhydrous methanol of the product that step (3) obtains 5 times of volumes soaks removes unreacted impurity 4 hours, constant temperature (105 DEG C) is dried, pulverized 80 mesh sieves (0.25mm), obtain soybean seed soaking drought resistance agent, the Infrared Characterization result of this soybean seed soaking drought resistance agent as shown in Figure 2.
Embodiment 2 prepares soybean seed soaking drought resistance agent
(1) pulverize: with (1) of embodiment 1;
(2) gelatinization:
Get the stalk powder 0.2g of gained in step (1) at normal temperatures, add a small amount of distilled water, stalk powder and the mass ratio added water are about 1: 100, then put high fiery gelatinization to microwave oven (power is 550w) 3 minutes;
(3) Microwave synthesize: the Mierocrystalline cellulose of gelatinization is put in atmosphere to normal temperature, add 3.6ml vinylformic acid (relative density is 1.049 ~ 1.055) successively, 26.7ml acrylamide soln (concentration is 4mol/L), 1.134g calcium chloride (calcium chloride quality is 10% of monomer), 4.2ml sodium hydroxide solution (massfraction is 40%), 1.0ml ammonium persulfate solution (concentration is 0.5mol/L), 2.9ml N, N-methylene-bisacrylamide solution (concentration is 0.25mol/L), in microwave oven, high fire (power is 700w) heats 5 minutes,
(4) drought resistance agent is obtained: the anhydrous methanol of the product that step (3) obtains 5 times of volumes soaks removes unreacted impurity 4 hours, constant temperature (105 DEG C) is dried, pulverize 80 mesh sieves (0.25mm), obtain soybean seed soaking drought resistance agent.
Embodiment 3 prepares soybean seed soaking drought resistance agent
(1) pulverize: with (1) of embodiment 1;
(2) gelatinization: with (2) of embodiment 1;
(3) Microwave synthesize: the Mierocrystalline cellulose of gelatinization is put in atmosphere to normal temperature, add 3.6ml vinylformic acid (relative density is 1.049 ~ 1.055) successively, 26.7ml acrylamide soln (concentration is 4mol/L), 2.268g calcium chloride powder (calcium chloride quality is monomer 20%), 4.2ml sodium hydroxide solution (massfraction is 40%), 1ml ammonium persulfate solution (concentration is 1mol/L), 2.9ml N, N-methylene-bisacrylamide solution (concentration is 0.25mol/L), in microwave oven, high fire (power range is 550w) heats 5 minutes,
(4) drought resistance agent is obtained: the anhydrous methanol of the product that step (3) obtains 5 times of volumes soaks removes unreacted impurity 4 hours, constant temperature (50 DEG C) is dried, pulverize 80 mesh sieves (0.25mm), obtain soybean seed soaking drought resistance agent.
Embodiment 4:
1. water-absorbent test: the powder getting 1g embodiment 1-3 respectively, be placed in distilled water, 0.3% sodium chloride solution, 0.6% sodium chloride solution, 0.9% sodium chloride solution respectively, leave standstill 4 hours, filter with 100 order nylon filtering cloths, gel leaves standstill 5 minutes and drips to anhydrous on filter cloth, takes off and weighs.
Calculate water-intake rate formula: Q = W 1 - W 0 W 0 × 100 %
Wherein, W 1gel net weight after water suction, g; W 0resin net weight before water suction, g.Result is as shown in table 1.
Table 1
2. percentage of germination test
Test group 1: adopt distilled water to soak seed 24 hours to black agriculture No. 44 soybean; The soybean 30 of soaking seed is put into the culture dish of diameter 15cm, growth cabinet is set and cultivates 30 degree, humidity 30%, observe soybean bud ratio.
Test group 2: the soybean seed soaking drought resistance agent of embodiment 1 is made into 0.005g/100ml, 0.015g/100ml, 0.025g/100ml, 0.05g/100ml, 0.10g/100ml concentration, black agriculture No. 44 soybean are soaked seed respectively 5 kinds of different concns soybean seed soaking drought resistance agent in 24 hours; The soybean of being soaked seed by different concns 30 places the culture dish of diameter 15cm, arranges growth cabinet and cultivates 30 degree, humidity 30%, observe soybean bud ratio.
Test group 3: the soybean seed soaking drought resistance agent of embodiment 2 is made into 0.005g/100ml, 0.015g/100ml, 0.025g/100ml, 0.05g/100ml, 0.10g/100ml concentration, black agriculture No. 44 soybean are soaked seed respectively 5 kinds of different concns soybean seed soaking drought resistance agent in 24 hours; The soybean of being soaked seed by different concns 30 places the culture dish of diameter 15cm, arranges growth cabinet and cultivates 30 degree, humidity 30%, observe soybean bud ratio.
Test group 4: the soybean seed soaking drought resistance agent of embodiment 3 is made into 0.005g/100ml, 0.015g/100ml, 0.025g/100ml, 0.05g/100ml, 0.10g/100ml concentration, black agriculture No. 44 soybean are soaked seed respectively 5 kinds of different concns soybean seed soaking drought resistance agent in 24 hours; The soybean of being soaked seed by different concns 30 places the culture dish of diameter 15cm, arranges growth cabinet and cultivates 30 degree, humidity 30%, observe soybean bud ratio.
Result is as shown in table 2.
Table 2
Percentage of germination (the 3rd day) Percentage of germination (the 7th day) Percentage of germination increment
Test group 1 60% 65% 5%
Test group 2 (0.005g/100ml) 62% 72% 10%
Test group 2 (0.015g/100ml) 65% 70% 5%
Test group 2 (0.025g/100ml) 60% 68% 8%
Test group 2 (0.05g/100ml) 58% 68% 10%
Test group 2 (0.10g/100ml) 50% 58% 8%
Test group 3 (0.005g/100ml) 50% 65% 15%
Test group 3 (0.015g/100ml) 55% 70% 15%
Test group 3 (0.025g/100ml) 50% 67% 17%
Test group 3 (0.05g/100ml) 57% 77% 20%
Test group 3 (0.10g/100ml) 56% 73% 17%
Test group 4 (0.005g/100ml) 60% 70% 10%
Test group 4 (0.015g/100ml) 70% 82% 12%
Test group 4 (0.025g/100ml) 67% 77% 10%
Test group 4 (0.05g/100ml) 62% 80% 12%
Test group 4 (0.10g/100ml) 67% 81% 14%
Shown by above-mentioned experimental data, about first three day of germination, the impact of soybean seed soaking drought resistance agent on bud ratio is little, illustrate that soybean desired nutritional in early stage is mainly soybean self and provides, but in germination after seven days, with the soybean after the seed soaking of soybean seed soaking drought resistance agent, percentage of germination obviously increases, when test group 3 soybean seed soaking drought resistance agent be made into concentration be 0.05g/100ml seed soaking time, percentage of germination is the highest, illustrate that the concentration optimum soybean of now soybean seed soaking drought resistance agent sprouts growth, excessive concentration, soybean is suppressed to sprout on the contrary, soybean seed soaking drought resistance agent institute calcium ions promotes soya cells division and promotes soybean germination.
3. pot experiment
Test group: take 900g soil and put into flowerpot, be numbered 1, take respectively in addition 650g soil and 250g embodiment 1, embodiment 2, embodiment 3 drought resistance agent mix, numbering is respectively 2,3,4.In four flowerpots, put into the strain of growing way the same soybean plant strain 5 respectively, pour into 200ml water, do not rewater later, observe two groups of potted plant plant changes, 5 groups of parallel tests are set, put into 30 degree of growth cabinets cultivations.Result: the 4th day, in No. 1 basin, soybean leaf starts here to wither, and all the other do not occur here withering; 7th day, in No. 1 basin, here 3 strains withered, and here did not wither in 2, No. 3 basins, and in No. 4 basins, here 1 strain withers; 15th day, in No. 1 basin, 1 strain was dead, and here 4 strains wither, and in No. 2 basins, here 1 strain withers, and all the other are normal, and in No. 3 basins, here 2 strains wither, and all the other are normal, and in No. 4 basins, here 2 strains wither, and all the other are normal; 30th day, in No. 1 basin, 5 strains were all dead, and in No. 2 basins, 2 strains are dead, and here 2 strains wither, and 1 strain is normal, and in No. 3 basins, 2 strains are dead, and here 3 strains wither, and in No. 4 basins, 3 strains are dead, and here 2 strains wither.
This shows, soybean seed soaking drought resistance agent synthesized by embodiment 1-3 in soil water retention property by by force to weak, this is consistent with the water-intake rate intensity of its mensuration, and calcium ion concn contained by embodiment 1-3 is different, has the function promoting seed germination when the amount showing calcium chloride is 5% ~ 20% of monomer mass.
Soybean seed soaking drought resistance agent is as a kind of high molecular polymer with super-strong moisture absorbing water conservation, slowly-releasing outlet capacity of synthetic, the evaporation of energy soil moisture control, after mixing with soil, form reticulated structure absorption soil moisture and nutritive substance, when soil is in exsiccosis, soybean seed soaking drought resistance agent just can slow releasing moisture and nutritive substance, needed for supply plant-growth, improve Soil structure simultaneously, strengthen soil activation, it is had broad application prospects in soil application.

Claims (9)

1. a preparation method for soybean seed soaking drought resistance agent, comprising:
In microwave oven, make stalk powder and water gelatinization, middle high fire reaction, reaction power is 450 ~ 550w;
By the stalk cooling after gelatinization, add vinylformic acid and acrylamide, calcium chloride, sodium hydroxide, initiator and linking agent, then high fire reaction in microwave oven, reaction power is 550 ~ 700w; The amount of described calcium chloride is 5% ~ 20% of vinylformic acid and acrylamide total mass;
Remove unreacted reactant with anhydrous methanol, dry, pulverize and obtain soybean seed soaking drought resistance agent.
2. preparation method according to claim 1, is characterized in that: described stalk is be selected from one or more in maize straw, wheat stalk, rice straw.
3. preparation method according to claim 1, is characterized in that: the mass ratio of described stalk powder and described water is 1:100 ~ 1:250.
4., according to described preparation method arbitrary in claim 1-3, it is characterized in that: the mass ratio of described vinylformic acid and acrylamide is 1:2 ~ 1:4.
5. preparation method according to claim 4, is characterized in that: degree of neutralization is 80%.
6. preparation method according to claim 5, is characterized in that: described anhydrous methanol removes the step of unreacted reactant for soak in anhydrous methanol.
7. preparation method according to claim 6, is characterized in that: the amount of described initiator is 1% of vinylformic acid and acrylamide total mass, and the amount of described linking agent is 1% of vinylformic acid and acrylamide total mass.
8. preparation method according to claim 7, is characterized in that: described stalk powder by by stalk 105 DEG C of oven dry, then pulverize acquisition.
9. the soybean seed soaking drought resistance agent that in claim 1-8 prepared by arbitrary described method.
CN201210122933.9A 2012-04-24 2012-04-24 Preparation method of soybean seed soaking drought resistance agent Expired - Fee Related CN103374105B (en)

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CN104448160A (en) * 2014-11-25 2015-03-25 皖西学院 Preparation method of farm-oriented water retaining agent using waste paper craps as raw materials
CN104448164A (en) * 2014-11-25 2015-03-25 皖西学院 Preparation method of composite farm-oriented water retaining agent using hemp stalks as raw materials

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CN101117371A (en) * 2006-07-31 2008-02-06 孙明 Process for producing plant drought-resisting water-loss reducer by using farm crop by-products
CN101519476A (en) * 2009-03-30 2009-09-02 中国科学技术大学 Method for preparing high-hydroscopicity resin in homogeneous aqueous medium by using straw as raw material
CN102119596A (en) * 2011-01-29 2011-07-13 浙江大学 Seed soaking processing method for simultaneously improving cold and drought resistance of tobacco seed
CN102181011A (en) * 2011-04-08 2011-09-14 甘肃圣大方舟马铃薯变性淀粉有限公司 Method for preparing water-retaining agent by utilizing straws

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Publication number Priority date Publication date Assignee Title
US6800712B2 (en) * 2002-10-07 2004-10-05 Steven William Doane Starch graft copolymers and method of making and using starch graft copolymers for agriculture

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101117371A (en) * 2006-07-31 2008-02-06 孙明 Process for producing plant drought-resisting water-loss reducer by using farm crop by-products
CN101519476A (en) * 2009-03-30 2009-09-02 中国科学技术大学 Method for preparing high-hydroscopicity resin in homogeneous aqueous medium by using straw as raw material
CN102119596A (en) * 2011-01-29 2011-07-13 浙江大学 Seed soaking processing method for simultaneously improving cold and drought resistance of tobacco seed
CN102181011A (en) * 2011-04-08 2011-09-14 甘肃圣大方舟马铃薯变性淀粉有限公司 Method for preparing water-retaining agent by utilizing straws

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