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

Abstract

The invention relates to a preparation method of a soybean seed soaking drought-resistant agent. The preparation method of the soybean seed soaking drought-resistant agent of the present invention comprises: gelatinizing straw powder and water in a microwave oven with a reaction power of 450-550w; cooling the gelatinized straw, adding acrylic acid, acrylamide, calcium chloride, and hydrogen Sodium oxide, an initiator and a cross-linking agent are then reacted in a microwave oven under the condition of a reaction power of 550-700w; unreacted reactants are removed, dried and crushed to obtain a soybean seed soaking drought-resistance agent. The soybean seed soaking drought-resistant agent of the invention has a simple synthesis method, short synthesis time, can turn waste into wealth, is degradable, and is harmless to the environment.

Description

Preparation method of soybean seed soaking drought-resistant agent

technical field

The invention relates to a preparation method of a soybean seed-soaking drought-resistance agent, in particular to a preparation method of a soybean seed-soaking drought-resistance agent using straw as one of the raw materials.

Background technique

my country is a large agricultural country, but also a country with relatively short water resources. As industrial and urban water consumption continues to increase, agricultural water consumption is gradually decreasing. In the history of our country, agricultural drought often caused great social disasters. According to many years of statistics, in recent years, the frequency of drought disasters in my country has been increasing, the area of drought disasters has been expanding, and the number of crop drought disasters has also shown an increasing trend. Especially in the context of global climate change, the impact of drought on agricultural production will further increase. Soybean is an important agricultural economic crop. China is the hometown of soybean, and the Northeast, the main producing area, is one of the most suitable regions for growing soybean in the world. In recent years, my country's soybeans mainly rely on imports. Therefore, it is imminent to increase my country's soybean production. Changes in the environment and soil drought will cause great difficulties in the emergence and growth of soybeans. While improving the efficiency of traditional water conservancy projects and improving cultivation techniques, it is a new research direction to use anti-drought agents to increase the drought resistance of crops. Under the same drought water conditions, crops using anti-drought agents can significantly reduce yield loss.

Among the existing anti-drought agents, Handilong is a kind of anti-drought agent with fulvic acid as the main material, and has a good anti-drought effect. There is also the use of inorganic calcium salt alone to soak seeds for drought resistance and seedling protection, but the effect is not ideal.

Contents of the invention

The purpose of the present invention is to provide a preparation method of soybean seed soaking drought resistance agent.

The preparation method of soybean seed soaking anti-drought agent provided by the present invention comprises:

Make straw powder and water gelatinization in microwave oven, the reaction power is 450～550w;

Cool the gelatinized straw, add acrylic acid, acrylamide, calcium chloride, sodium hydroxide, initiator and crosslinking agent, and then react in a microwave oven with a reaction power of 550-700w;

The unreacted reactants are removed with anhydrous methanol, dried and crushed to obtain the soybean seed soaking drought-resistance agent.

In the preparation method of the soybean seed soaking drought resistance agent of the present invention, the straw is one or more selected from corn straw, wheat straw and rice straw.

In the preparation method of the soybean seed soaking drought resistance agent of the present invention, the mass ratio of the straw powder to the water is 1:100˜1:250.

In the preparation method of the soybean seed soaking drought resistance agent of the present invention, the mass ratio of the acrylic acid to the acrylamide is 1:2˜1:4.

In the preparation method of the soybean seed soaking drought resistance agent of the present invention, the amount of the calcium chloride is 10% to 30% of the total mass of acrylic acid and acrylamide.

In the preparation method of the soybean seed soaking drought resistance agent of the present invention, the neutralization degree is 80%.

In the preparation method of the soybean seed soaking drought resistance agent of the present invention, the step of removing unreacted reactants is soaking in anhydrous methanol.

In the preparation method of the soybean seed soaking drought resistance agent of the present invention, the amount of the initiator is 1% of the total mass of acrylic acid and acrylamide, and the amount of the crosslinking agent is 1% of the total mass of acrylic acid and acrylamide.

In the preparation method of the soybean seed soaking drought-resistant agent of the present invention, the straw powder is obtained by drying the straw at 105° C. and then pulverizing it.

The invention uses waste straw as one of the raw materials to prepare the drought-resistant agent for soaking soybean seeds. The soybean seed soaking anti-drought agent can form a layer of water film on the surface of seeds, absorb surrounding water molecules, and use calcium ions to promote the growth of seeds in the early stage of germination to increase the germination rate. The anti-drought agent of the invention has simple synthesis method, short synthesis time, can turn waste into treasure, is degradable, and is harmless to the environment.

Description of drawings

Fig. 1 shows the synthetic process of soybean seed soaking drought resistance agent.

Fig. 2 shows the infrared spectrogram of soybean seed soaking drought resistance agent

Detailed ways

Below in conjunction with specific embodiment, further illustrate the present invention. It should be understood that these examples are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the teachings of the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of the present application.

Embodiment 1 prepares soybean soaking anti-drought agent

(1) Pulverization: Put the discarded stalks (corn stalks) in an oven to dry at 105 degrees Celsius, pulverize them with a pulverizer, and pass through a 200-mesh sieve (0.074mm) to obtain straw powder;

(2) Gelatinization: Take 0.2 g of the straw powder obtained in step (1) at normal temperature, add a small amount of distilled water, the mass ratio of the straw powder to the added water is about 1:250, and then put it into a microwave oven for gelatinization on high heat (power 450w) for 3 minutes;

(3) Microwave synthesis: After the gelatinized cellulose is placed in the air at room temperature, 3.6ml of acrylic acid (relative density is 1.049-1.055), 26.7ml of acrylamide solution (concentration of 4mol/L), 0.567g of chlorinated Calcium powder (calcium chloride mass is 5% of monomer mass), 4.2ml sodium hydroxide solution (mass fraction is 40%), 1.0ml ammonium persulfate solution (concentration is 0.5mol/L), 2.9ml N, N - Methylenebisacrylamide solution (concentration: 0.25mol/L), react in a microwave oven on high heat (power: 550w) for 5 minutes;

(4) Obtaining drought-resistant agent: the product obtained in step (3) was soaked with 5 times the volume of anhydrous methanol to remove unreacted impurities for 4 hours, dried at a constant temperature (105° C.), pulverized and passed through an 80-mesh sieve (0.25 mm), to obtain Soybean seed soaking drought resistance agent, the infrared characterization results of the soybean seed soaking drought resistance agent are shown in Figure 2.

Embodiment 2 prepares soybean soaking anti-drought agent

(1) pulverizing: with (1) of embodiment 1;

(2) Gelatinization:

Take 0.2 g of the straw powder obtained in step (1) at room temperature, add a small amount of distilled water, the mass ratio of the straw powder to the added water is about 1:100, and then put it in a microwave oven for gelatinization on high heat (550w power) for 3 minutes;

(3) Microwave synthesis: After the gelatinized cellulose is placed in the air at room temperature, 3.6ml of acrylic acid (relative density is 1.049-1.055), 26.7ml of acrylamide solution (concentration of 4mol/L), 1.134g of chlorinated Calcium (the quality of calcium chloride is 10% of the monomer), 4.2ml sodium hydroxide solution (mass fraction is 40%), 1.0ml ammonium persulfate solution (concentration is 0.5mol/L), 2.9ml N, N- Methyl bisacrylamide solution (concentration is 0.25mol/L), heated in microwave oven on high fire (power is 700w) for 5 minutes;

(4) Obtaining drought-resistant agent: the product obtained in step (3) was soaked with 5 times the volume of anhydrous methanol to remove unreacted impurities for 4 hours, dried at a constant temperature (105° C.), pulverized and passed through an 80-mesh sieve (0.25 mm), to obtain Soybean Seed Soaking Drought Resistant Agent.

Embodiment 3 prepares soybean soaking anti-drought agent

(1) pulverizing: with (1) of embodiment 1;

(2) Gelatinization: (2) with embodiment 1;

(3) Microwave synthesis: After the gelatinized cellulose is placed in the air at room temperature, 3.6ml of acrylic acid (relative density is 1.049-1.055), 26.7ml of acrylamide solution (concentration of 4mol/L), 2.268g of chloride Calcium powder (mass of calcium chloride is 20% of monomer), 4.2ml sodium hydroxide solution (mass fraction is 40%), 1ml ammonium persulfate solution (concentration is 1mol/L), 2.9ml N, N-methylene Bisacrylamide solution (concentration: 0.25mol/L), heated in a microwave oven (power range: 550w) for 5 minutes;

(4) Obtaining drought-resistant agent: the product obtained in step (3) was soaked with 5 times the volume of anhydrous methanol to remove unreacted impurities for 4 hours, dried at a constant temperature (50° C.), and pulverized through an 80-mesh sieve (0.25 mm) to obtain Soybean Seed Soaking Drought Resistant Agent.

Example 4:

1. Water absorption test: Take 1g of the powders of Examples 1-3 respectively, place them in distilled water, 0.3% sodium chloride solution, 0.6% sodium chloride solution, and 0.9% sodium chloride solution, let stand for 4 hours, use Filter with 100-mesh nylon filter cloth, let the gel stand on the filter cloth for 5 minutes until no water drips, take it off and weigh it.

Calculate water absorption formula: $Q=\frac{W_1-W_0}{W_0}\×100\%$

Among them, W ₁ is the net weight of the gel after water absorption, g; W ₀ is the net weight of the resin before water absorption, g. The results are shown in Table 1.

Table 1

2. Germination rate test

Test group 1: Soak Heinong No. 44 soybean seeds in distilled water for 24 hours; put 30 soaked soybeans into a petri dish with a diameter of 15 cm, set up an artificial climate chamber for cultivation at 30 degrees, humidity 30%, and observe the germination rate of soybeans.

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, soaks Heinong No. 44 soybeans in 5 Soak soybean seeds of different concentrations in drought-resistant agents for 24 hours; place 30 soybeans soaked in different concentrations on a petri dish with a diameter of 15 cm, set up an artificial climate chamber to cultivate at 30 degrees, humidity 30%, and observe the soybean germination rate.

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, soaks Heinong No. 44 soybean in 5 Soak soybean seeds of different concentrations in drought-resistant agents for 24 hours; place 30 soybeans soaked in different concentrations on a petri dish with a diameter of 15 cm, set up an artificial climate chamber to cultivate at 30 degrees, humidity 30%, and observe the soybean germination rate.

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, soaks Heinong No. 44 soybeans in 5 Soak soybean seeds of different concentrations in drought-resistant agents for 24 hours; place 30 soybeans soaked in different concentrations on a petri dish with a diameter of 15 cm, set up an artificial climate chamber to cultivate at 30 degrees, humidity 30%, and observe the soybean germination rate.

The results are shown in Table 2.

Table 2

Germination rate (third day) Germination rate (7th day) Incremental germination rate 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%

According to the above experimental data, about three days before germination, the soybean seed soaking drought-resistant agent has little effect on the germination rate, indicating that the nutrients required by soybeans in the early stage are mainly provided by soybean itself, but after seven days of germination, soaking soybean seeds with drought-resistant agent Soybean germination rate increased significantly. When the soybean seed soaking drought-resistance agent of test group 3 was mixed with a concentration of 0.05g/100ml for soaking seeds, the germination rate was the highest. , On the contrary, it inhibits soybean germination, and the calcium ion contained in the soybean soaking drought resistance agent promotes soybean cell division and soybean germination.

3. Pot experiment

Test group: Weigh 900g of soil and put it into a flower pot, numbered 1. In addition, weigh 650g of soil and 250g of the drought-resisting agent of Example 1, Example 2, and Example 3 and mix evenly, and the numbers are 2, 3, and 4 respectively. Put 5 soybean plants with the same growth in four flower pots, pour 200ml of water, and then no longer water, observe the changes of the plants in the two groups of pots, set up 5 groups of parallel experiments, and put them in a 30-degree artificial climate box nourish. Results: On the 4th day, the soybean leaves in the No. 1 pot began to wilt, but the rest did not appear to be wilted; on the 7th day, 3 plants in the No. On the 15th day, 1 plant died in No. 1 pot, 4 plants withered, 1 plant in No. 2 pot, and the rest were normal, 2 plants in No. The plants wilted, and the rest were normal; on the 30th day, all 5 plants in pot No. 1 died, 2 plants in No. 2 pot died, 2 plants wilted, and 1 plant was normal. In pot No. 4, 3 plants died and 2 plants withered.

This shows that the soybean seed soaking drought-resistant agent synthesized in embodiment 1-3 has water retention performance in soil from strong to weak, which is consistent with the water absorption strength measured by it. The calcium ion concentration contained in embodiment 1-3 is different, indicating that chlorination When the amount of calcium is 5% to 20% of the mass of the monomer, it has the function of promoting seed germination.

Soybean seed soaking anti-drought agent is a synthetic polymer with super water absorption and water retention and slow release water capacity. It can control the evaporation of soil water. After mixing with soil, it forms a network structure to absorb water and nutrients in the soil. When the soil is in a state of water shortage, the soybean soaking drought-resistant agent will slowly release water and nutrients to supply the needs of plant growth, while improving the soil structure and enhancing soil activity, making it have broad application prospects in soil fertilization.

Claims (9)

1. A preparation method of soybean seed soaking drought-resistant agent, comprising: Make the straw powder and water gelatinization in the microwave oven, react with medium-high heat, and the reaction power is 450-550w; Cool the gelatinized straw, add acrylic acid, acrylamide, calcium chloride, sodium hydroxide, initiator and cross-linking agent, and then react in a microwave oven at high heat with a reaction power of 550-700w; the calcium chloride The amount is 5% to 20% of the total mass of acrylic acid and acrylamide; The unreacted reactants are removed with anhydrous methanol, dried and crushed to obtain the soybean seed soaking drought-resistance agent. 2. The preparation method according to claim 1, characterized in that: the straw is one or more selected from corn straw, wheat straw and rice straw. 3. The preparation method according to claim 1, characterized in that: the mass ratio of the straw powder to the water is 1:100-1:250. 4. The preparation method according to any one of claims 1-3, characterized in that: the mass ratio of acrylic acid to acrylamide is 1:2-1:4. 5. The preparation method according to claim 4, characterized in that: the degree of neutralization is 80%. 6. The preparation method according to claim 5, characterized in that: the step of removing unreacted reactants with anhydrous methanol is soaking in anhydrous methanol. 7. The preparation method according to claim 6, characterized in that: the amount of the initiator is 1% of the total mass of acrylic acid and acrylamide, and the amount of the crosslinking agent is 1% of the total mass of acrylic acid and acrylamide . 8 . The preparation method according to claim 7 , wherein the straw powder is obtained by drying the straw at 105° C. and then pulverizing it. 9. the soybean seed soaking drought-resisting agent prepared by the method described in any one of claims 1-8.