CN101985486B - A preparation method of superabsorbent resin containing compound plant growth regulator - Google Patents

Abstract

The invention provides a method for preparing a super absorbent resin containing a compound plant growth regulator. In the method, sodium fulvate and nitrophenolate are added in a reaction system for polymerization before graft copolymerization of starch or starch derivatives, crylic acid and other monomers, and the absorbent times of the prepared super absorbent resin is 340-700. The method in the invention has the advantages of simple synthesis process, no pollution and low production cost, and the prepared product contains the sodium fulvate and nitrophenolate with the function of plant growth regulation, and can be widely used in the fields of agriculture, forestry, desertification control, gardening and the like.

Description

A preparation method of superabsorbent resin containing compound plant growth regulator

technical field

The invention relates to a method for preparing a superabsorbent resin, in particular to a method for preparing a superabsorbent resin containing a compound plant growth regulator. The product can be widely used in the fields of agriculture, forestry, gardening, and desertification prevention and control.

Background technique

Due to its excellent water absorption and water retention properties, superabsorbent resins have important applications in many fields, especially in the fields of agriculture, forestry, horticulture, and desertification control. Superabsorbent resins are often used in agriculture for soil improvement, desert greening, soilless cultivation, drought resistance and water retention, slow release of pesticides and fertilizers, etc. Adding superabsorbent resin to the soil can improve the soil structure, increase the water absorption and water retention capacity of the soil, improve the soil moisture status, adjust the distribution of solid, liquid and gas in the soil, and improve the soil's ability to regulate temperature. It provides a favorable environment for the reproduction of soil microorganisms, greatly improves their activity, is conducive to the absorption of nutrients by plants, can significantly increase the germination rate of seeds, and promote the growth and development of plants. The production of aquatic plants has created good conditions.

With the continuous expansion of the application range of superabsorbent resins in fields such as agriculture and forestry, ordinary superabsorbent resins can no longer meet the application requirements in terms of performance and function. The development and research of high-performance superabsorbent resins that can meet specific performance requirements has become a hot topic today. . Especially in the application of agriculture, forestry and gardening, there is an urgent need to develop more practical multifunctional superabsorbent resins, such as new superabsorbent resins containing plant growth nutrients and slow-release fertilizers.

Sodium fulvic acid and sodium o/p-nitrophenolate are broad-spectrum plant growth regulators, which are widely used in agriculture and horticulture. They have the functions of promoting cell protoplasm flow, improving cell viability, accelerating plant growth and development, and promoting Strong roots and seedlings, preserved flowers and fruits, increased yield, enhanced stress resistance and other advantages. Sodium fulvic acid and sodium o/p-nitrophenolate are introduced into the superabsorbent resin, so that the superabsorbent resin not only has water absorption and water retention properties, but also has the function of plant growth regulation, which expands the application range of the superabsorbent resin and makes it more Has practical value.

Contents of the invention

The purpose of the present invention is to provide a preparation method of a superabsorbent resin containing a compound plant growth regulator, which is suitable for application in the fields of agriculture, forestry, desertification control and horticulture.

The technical scheme of the present invention is as follows: under cooling and stirring in an ice-water bath, use sodium hydroxide or potassium hydroxide solution to neutralize the acrylic acid that removes the polymerization inhibitor to obtain acrylic acid and its salt solution, and then gelatinize it with starch derivatives or heat Starch, acrylamide, sodium fulvic acid and sodium o/p-nitrophenolate solution, cross-linking agent N, N'-methylenebisacrylamide solution and initiator potassium persulfate are mixed and stirred at room temperature for 0.5-1.0 h, make it mix evenly, wherein the mass ratio of raw materials is 1 part of starch or starch derivatives, 0.168-6.990 parts of sodium hydroxide or 0.47-9.80 parts of potassium hydroxide, 3-14 parts of acrylic acid, 0-20 parts of acrylamide, 0.0004-0.4 parts of sodium fulvic acid, 0.0004-1.0961 parts of o/p-nitrophenolate sodium, 0.00002-0.04000 parts of N, N'-methylenebisacrylamide, 0.005-0.050 parts of potassium persulfate, 20-40 parts of Ionized water, then feed nitrogen and slowly heat in a water bath, make it react at 60-80°C for 1 hour, continue to heat up, then keep warm in a boiling water bath for 1-2 hours, stop nitrogen, cool to room temperature, take out the product, Drying, pulverizing and sieving to obtain a superabsorbent resin containing a compound plant growth regulator, and the water absorption of the product is 340-700 times.

The starch described in the above-mentioned technical scheme is potato starch, cornstarch, tapioca starch, and starch derivative is carboxymethyl starch, phosphate ester starch, cross-linked starch, acetate starch, sulfonate starch, pregelatinized starch, Preference is given to potato starch or potato starch derivatives.

The degree of neutralization of the acrylic acid described in the scheme is 20%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 70%, 80%, preferably 30%-60%.

The deionized water in the raw material ratio described in the scheme is the total amount of deionized water used for dissolving sodium hydroxide or potassium hydroxide, acrylamide, sodium fulvic acid, o/p-nitrophenol sodium and thermal gelatinization of starch.

The advantages of the present invention are as follows:

(1) In addition to the water-absorbing and water-retaining properties of the superabsorbent resin, the product prepared by the present invention also contains sodium fulvic acid and sodium o/p-nitrophenolate with nutritional functions.

(2) The present invention uses starch or starch derivatives as a matrix, which can greatly reduce production costs, and the product has the advantages of easy degradation and no pollution.

(3) The present invention adopts a one-step synthesis method, the production process is simple, and no three wastes are produced, which is beneficial to industrial production.

Description of drawings

Fig. 1 is the preparation process flowchart of product

Fig. 2 is the infrared spectrogram of embodiment 4 products

Detailed ways

Embodiment 1: Dissolve 5.0g sodium hydroxide with 15ml deionized water, under ice-water bath cooling and stirring, neutralize 30g (28.6ml) acrylic acid; Dissolve 0.01g sodium o-nitrophenolate, 0.01g para Sodium nitrophenolate and 0.1g sodium fulvic acid; Weigh 5.0g potato starch and dissolve in 25ml deionized water, heat and gelatinize at 60-70°C for 1-2 minutes, cool to room temperature and mix with neutralized acrylic acid and Its salt solution, sodium fulvic acid, o/p-nitrophenolate sodium solution, 80mg potassium persulfate, 4ml of N,N'-methylenebisacrylamide solution with a concentration of 5mg/ml were mixed, and stirred at room temperature for 0.5h , then pass nitrogen and slowly heat in a water bath, make it react at 60-75 ° C for 1 hour, continue to heat up, and then keep warm in a boiling water bath for 1.5 hours, stop nitrogen, cool to room temperature, take out the product, dry, Crushed and sieved, the superabsorbent resin containing the compound plant growth regulator was obtained, and the water absorption ratio of the product obtained in this example was 475 times.

Embodiment 2: Dissolve 8.33g sodium hydroxide with 27ml deionized water, under ice-water bath cooling and stirring, neutralize 30g (28.6ml) acrylic acid; Dissolve 0.1g o-nitrophenol, 0.2g p-nitrophenol with 35ml deionized water phenol and 0.3g sodium fulvic acid, then add neutralized acrylic acid and its salt solution, 2.5g carboxymethyl potato starch, 8ml concentration of 5mg/ml N, N'-methylenebisacrylamide solution and 65mg of potassium persulfate, stirred at room temperature for 0.5h, then fed nitrogen and started to heat slowly, made it react at 60-80°C for 1h, continued to heat up, and then kept it in a boiling water bath for 1-2h, stopped nitrogen, cooled After reaching room temperature, the product was taken out, dried, pulverized, and sieved to obtain a superabsorbent resin containing a compound plant growth regulator. The water absorption ratio of the product obtained in this example was 660 times.

Embodiment 3: The experimental conditions are the same as in Example 2, except that 0.01g of o-nitrophenol, 0.01g of p-nitrophenol and 0.3g of sodium fulvic acid are dissolved in 35ml of deionized water. The water absorption rate of the product obtained in this embodiment is 610 times.

Embodiment 4: Experimental condition is the same as embodiment 2, and difference is to dissolve 0.05g o-nitrophenol, 0.05g p-nitrophenol and 0.3g sodium fulvic acid with 35ml deionized water, and the water absorption multiple of the product obtained in this embodiment is 675 times.

Embodiment 5: experimental condition is the same as embodiment 2, and difference is to dissolve 0.1g o-nitrophenol, 0.1g p-nitrophenol and 0.3g sodium fulvic acid with 35ml deionized water, and the water absorption multiple of the product obtained in this embodiment is 655 times.

Embodiment 6: experimental condition is the same as embodiment 2, and difference is to dissolve 0.2g o-nitrophenol, 0.2g p-nitrophenol and 0.3g sodium fulvic acid with 35ml deionized water, and the water absorption multiple of the product obtained in this embodiment is 390 times.

Example 7: Dissolve 6.5g potassium hydroxide with 24ml deionized water, and neutralize 28g (26.7ml) acrylic acid under ice-water bath cooling and stirring; Dissolve 0.05g o-nitrophenol, 0.05g p- Nitrophenol and 0.5g sodium fulvic acid, then with neutralized acrylic acid and its salt solution, 2.5g phosphate potato starch, 7g acrylamide, 6ml concentration of 5mg/ml N, N'-methylene Mix bisacrylamide solution and 100mg potassium persulfate, stir at room temperature for 0.5h, then pass nitrogen gas and start to heat slowly, make it react at 70-80°C for 1h, continue to heat up, and keep warm in boiling water bath for 1-2h , stop the nitrogen flow, cool to room temperature, take out the product, dry, pulverize, and sieve to obtain a superabsorbent resin containing a composite plant growth regulator. The water absorption ratio of the product obtained in this embodiment is 605 times.

Embodiment 8: The experimental conditions are the same as in Example 7, except that 0.05g of o-nitrophenol, 0.05g of p-nitrophenol and 0.01g of sodium fulvic acid are dissolved in 40ml of deionized water. The water absorption of the product obtained in this embodiment is 340 times.

Embodiment 9: The experimental conditions are the same as in Example 7, except that 0.05g of o-nitrophenol, 0.05g of p-nitrophenol and 0.05g of sodium fulvic acid are dissolved in 40ml of deionized water. The water absorption rate of the product obtained in this embodiment is 400 times.

Example 10: The experimental conditions are the same as in Example 7, except that 0.05g of o-nitrophenol, 0.05g of p-nitrophenol and 0.1g of sodium fulvic acid are dissolved in 40ml of deionized water. The water absorption rate of the product obtained in this example is 385 times.

Example 11: The experimental conditions are the same as in Example 7, except that 0.05g of o-nitrophenol, 0.05g of p-nitrophenol and 0.7g of sodium fulvic acid are dissolved in 40ml of deionized water. The water absorption of the product obtained in this example is 700 times.

The infrared spectrum of the product of Example 7 is measured by a NEXUS _TM 670FT-IR ESP infrared spectrometer. As determined by the German Elementar Vario ELIII type elemental analysis instrument, the element content of the product of Example 7 is: C%=40.09, H%=5.867, N%=3.110.

Claims (5)

1. preparation method who contains the composite plant growth regulator High hydrophilous resin, it is characterized in that: under the ice-water bath cooling and stirring, remove the vinylformic acid of stopper with sodium hydroxide or potassium hydroxide solution neutralization, obtain vinylformic acid and salts solution thereof, afterwards with starch derivative or hot gelatinization after starch, acrylamide, SODLUM FULVATE and sodium onitrophenol or p-NP sodium solution, linking agent N, N ＇-methylene-bisacrylamide solution and initiator potassium persulfate are mixed, at room temperature stir 0.5-1.0h, it is mixed, wherein raw material mass mixture ratio is 1 part of starch or starch derivative, 0.168-6.990 part sodium hydroxide or 0.47-9.80 part potassium hydroxide, 3-14 part vinylformic acid, 0-20 part acrylamide, 0.0004-0.4 part SODLUM FULVATE, 0.0004-1.0961 part sodium onitrophenol or Sodium p-nitrophenoxide, 0.00002-0.04000 part N, N ＇-methylene-bisacrylamide, 0.005-0.050 part Potassium Persulphate, 20-40 part deionized water, feed nitrogen then and slowly heating in water-bath, make it react 1h down, continue to heat up, in boiling water bath, be incubated 1-2h again at 60-80 ℃, stop logical nitrogen, be cooled to room temperature, product is taken out, oven dry, pulverize, sieve, promptly get the High hydrophilous resin that contains composite plant growth regulator, the suction multiple of product is 340-700 times.

2. a kind of preparation method who contains the composite plant growth regulator High hydrophilous resin according to claim 1 is characterized in that: used starch is yam starch, W-Gum, tapioca (flour).

3. a kind of preparation method who contains the composite plant growth regulator High hydrophilous resin according to claim 1 is characterized in that: used starch derivative is carboxymethyl starch, phosphate ester starch, cross-linking starch, acetate starch, sulphur ortho ester starch.

4. a kind of preparation method who contains the composite plant growth regulator High hydrophilous resin according to claim 1 is characterized in that: used starch or starch derivative are yam starch or yam starch derivative.

5. a kind of preparation method who contains the composite plant growth regulator High hydrophilous resin according to claim 1 is characterized in that: acrylic acid degree of neutralization is 30%-60%.

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