Indolebutyric acid 14-hydroxybrassinosterol-containing soluble powder
By combining modified naphthalene sulfonate formaldehyde condensate and modified vitamin E, the dispersion and stability problems of indolebutyric acid and 14-hydroxybrassinosteroid soluble powder were solved, thus promoting the growth and increasing the yield of Chinese cabbage.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-30
- Publication Date
- 2026-04-10
AI Technical Summary
In the existing technology, the soluble powder of indolebutyric acid and 14-hydroxybrassinosteroid has the following problems: insufficient hydrophilicity of dispersant, single function of stabilizer, and lack of synergistic compatibility between components. This leads to easy aggregation and thermal degradation of active ingredients, which affects the uniformity and stability of drug efficacy.
Modified naphthalene sulfonate formaldehyde condensate is used as a dispersant, modified vitamin E is used as a stabilizer, and a wetting agent and pH buffer are used in combination to form a synergistic effect, ensuring uniform dispersion and thermal stability of the active ingredients.
It achieves uniform dispersion and long-term stability of active ingredients, improves the uniformity of efficacy and storage stability, and promotes the growth of Chinese cabbage, increasing yield and quality.
Smart Images
Figure SMS_1 
Figure SMS_2 
Figure SMS_3
Abstract
Description
Technical Field
[0001] This invention belongs to the field of soluble powder technology, specifically relating to a soluble powder containing indolebutyric acid·14-hydroxybrassinosteroidol. Background Technology
[0002] As people's living standards continue to improve, higher demands are being placed on the quality and yield of vegetables. As a common and popular vegetable, bok choy's cultivation benefits and quality have attracted much attention. However, the cultivation of bok choy faces numerous challenges, such as the threat of pests and diseases, the impact of adverse weather conditions, and limitations in soil fertility. These problems severely restrict the improvement of bok choy's yield and quality.
[0003] Indolebutyric acid (IBA), a highly effective rooting agent, promotes the growth and development of pak choi roots. It increases the number and length of roots by stimulating root cell division and elongation, resulting in a more developed root system and enhancing the pak choi's ability to absorb water and nutrients from the soil. A well-developed root system provides sufficient material support for pak choi growth, improves its resistance to adverse conditions, and reduces the risk of pests and diseases.
[0004] 14-Hydroxybrassinosteroids possess a wide range of physiological activities, regulating the growth and development of pak choi. They promote photosynthesis, increase photosynthetic efficiency, and enhance the accumulation of photosynthetic products, resulting in darker, thicker leaves and stronger plants. Furthermore, 14-Hydroxybrassinosteroids regulate hormonal balance within pak choi, promoting cell division and elongation, thereby boosting stem and leaf growth. They also enhance the plant's stress resistance, improving its adaptability to adverse conditions such as drought, high temperatures, and low temperatures, as well as its resistance to pests and diseases.
[0005] In existing technologies, indolebutyric acid and 14-hydroxybrassinosteroids are combined to form a soluble powder, which can more comprehensively promote the growth and development of pakchoi. To meet the basic usage requirements of soluble powders, conventional auxiliary ingredients are usually used to construct the formulation system: naphthalene sulfonate formaldehyde condensate (NNO) is often used as a dispersant to achieve initial dispersion of the active ingredients; vitamin E (VE) is often used as a stabilizer to alleviate the oxidation problem of the active ingredients; water-soluble carriers such as lactose and anhydrous sodium sulfate are often used as fillers to dilute the active ingredients and improve the flowability of the powder; sodium dodecyl sulfate (K12) is commonly used as a wetting agent to accelerate the wetting process of the powder in water. In terms of preparation process, the industry usually completes the production through conventional steps such as mixing, pulverizing, and sieving.
[0006] However, existing technologies still have certain problems when targeting the specific compound active ingredient IBA and 14-hydroxybrassinosteroids: the conventional dispersant NNO has limited hydrophilicity and is insufficient in dispersing the extremely low concentration of 14-hydroxybrassinosteroids, easily leading to aggregation of the active ingredient after powder dissolution, directly affecting the uniformity of efficacy; in addition, the conventional stabilizer VE only has a single antioxidant function and cannot regulate the pH value of the system, while IBA is sensitive to acid and alkaline environments and is prone to degradation when the system pH deviates from the stable range of 5.0-7.0. At the same time, 14-hydroxybrassinosteroids has poor thermal stability, and VE alone is difficult to effectively inhibit its thermal degradation during storage or use. Moreover, existing auxiliary ingredients are mostly designed with independent functions, and there is a lack of synergistic compatibility between the ingredients for this compound active ingredient, which restricts the application effect and market promotion potential of the product. Summary of the Invention
[0007] The purpose of this invention is to provide a soluble powder containing indolebutyric acid·14-hydroxybrassinosteroidol to solve the problems existing in the prior art.
[0008] To achieve the above objectives, the present invention provides the following technical solution: A soluble powder, by weight percentage, is prepared from the following components: indolebutyric acid 0.04-0.06%, 14-hydroxybrassinosteroidol 0.00008-0.00012%, dispersant 1.5-5.0%, stabilizer 0.5-2.0%, wetting agent 1.0-3.0%, pH buffer pair 0.8-1.2%, and water-soluble filler to 100%; wherein the dispersant is a modified naphthalene sulfonate formaldehyde condensate; and the stabilizer is modified vitamin E.
[0009] Furthermore, the preparation method of the modified naphthalene sulfonate formaldehyde condensate includes the following steps: S1. Add 75.0 g of naphthalene sulfonate formaldehyde condensate and 500 mL of toluene to a 5 L container, and purge with nitrogen gas at a flow rate of 50 mL / min to remove air; heat the container in a water bath to 80 °C and stir at 200 r / min for 30 min to dissolve the naphthalene sulfonate formaldehyde condensate toluene solution; slowly add 22.5 g of ethylene glycol diglycidyl ether dropwise along the inner wall of the container to the naphthalene sulfonate formaldehyde condensate toluene solution at a drop rate of 1.5 mL / min, while maintaining stirring at 200 r / min during the dropwise addition; after the dropwise addition is complete, react at 80 °C, 200 r / min, and under a nitrogen atmosphere for 2 h to obtain a hydroxylated naphthalene sulfonate formaldehyde condensate solution; S2. Add 25g of polyethylene glycol monomethyl ether MPEG-450 to the hydroxylated naphthalene sulfonate formaldehyde condensate solution, stir at 200r / min for 15min, then heat to 90℃, add 0.5g of stannous octoate, and react at 90℃, 200r / min, under a nitrogen atmosphere for 4h. S3. Continue stirring and allow to cool naturally to room temperature. Distill at 60℃ and -0.095MPa for 2 hours to remove toluene. Add 100mL of deionized water to the distillation residue, stir and wash at 100r / min for 30min, allow to stand and separate into layers, then discard the upper aqueous phase. Repeat washing 3 times. S4. Transfer the washed product to a vacuum drying oven and dry it at 60℃ and -0.090MPa for 4 hours. Then pulverize it through a 200-mesh sieve to obtain the modified naphthalene sulfonate formaldehyde condensate.
[0010] Furthermore, the preparation method of the modified vitamin E includes the following steps: S1. Add 68.3g of vitamin E and 400mL of anhydrous ethanol to a 5L container, heat to 50℃ in a constant temperature water bath, and stir at 150r / min for 20min to dissolve vitamin E; after naturally cooling to 30℃, add 31.7g of acrylic acid, and continue stirring for 10min to obtain a transparent reaction solution. S2. Add 0.3g of initiator benzoyl peroxide to the reaction solution and stir at 150r / min for 8min; heat to 75℃ in a constant temperature water bath, wrap the outer wall of the container with black light-blocking cloth, and react at a constant temperature for 3h with stirring at 150r / min. S3. Continue stirring and allow to cool naturally to room temperature. Distill at 60℃ and -0.090MPa for 1.5h to remove anhydrous ethanol and obtain a concentrate. Add 150mL of deionized water to the concentrate, stir and wash at 100r / min for 40min, let stand for 11h and discard the aqueous phase. Repeat the washing twice. S4. Transfer the washed product to a vacuum drying oven and dry it at 60℃ and -0.095MPa for 8 hours. Then pulverize it through a 200-mesh sieve to obtain modified vitamin E.
[0011] Furthermore, the wetting agent is sodium dodecyl sulfate.
[0012] Furthermore, the pH buffer is composed of citric acid and sodium citrate in a 1:2 molar ratio.
[0013] Furthermore, the water-soluble filler is composed of lactose and anhydrous sodium sulfate in equal mass ratios.
[0014] The present invention also provides a method for preparing the soluble powder, specifically: adding dispersant, stabilizer and 5% of the total mass of the finished product of deionized water to a 5L container, stirring to dissolve, and then uniformly spraying it into the water-soluble filler, stirring and mixing at 150r / min for 20min; then adding the remaining other components, stirring and mixing at 150r / min for 20min, and then air-jetting and sieving to obtain the soluble powder.
[0015] The present invention also provides the application of the soluble powder in promoting the growth of Chinese cabbage and improving its yield and quality.
[0016] Compared with the prior art, the present invention has the following beneficial effects: (1) This invention uses graft-modified naphthalene sulfonate formaldehyde condensate and the strong adsorption properties of hydrophilic long-chain polymers to solve the problem of easy aggregation of 14-hydroxybrassinosteroid due to its extremely low content, thus ensuring uniform efficacy. In addition, graft-modified vitamin E has both pH regulation and synergistic antioxidant functions, which can not only accurately stabilize the pH of the system in the suitable stable range of IBA, but also effectively inhibit the thermal degradation of the dual active ingredients, thus taking into account both active ingredients.
[0017] (2) The wetting agent of this invention accelerates the wetting of the powder, laying the foundation for the modified dispersant to play its role; the water-soluble composite filler is adapted to the dispersion requirements of the modified components; the pH buffer helps the auxiliary modified stabilizer stabilize the pH of the system and avoid interference from the external environment. The combined effect of the auxiliary components achieves rapid wetting of the finished product, long-term stability of the active ingredients, and good dispersion uniformity, which is of great significance for the development of soluble powders containing indolebutyric acid and 14-hydroxybrassinosteroidol.
[0018] (3) The soluble powder of the present invention has excellent effects on promoting the growth of Chinese cabbage, increasing the yield and quality of Chinese cabbage. Detailed Implementation
[0019] The technical solution of this invention patent will be clearly and completely described below. Obviously, the described embodiments are some embodiments of this invention, but not all embodiments.
[0020] 1. The effect of different additives on the performance of soluble powders 1.1 Soluble Powder Formulation See Table 1.
[0021] Table 1. Formulation of soluble powder (unit: g) formula Q1 Q2 Q3 Q4 Indolebutyric acid 0.0499 0.0499 0.0499 0.0499 14-Hydroxybrassinosteroid 0.0001 0.0001 0.0001 0.0001 naphthalenesulfonate formaldehyde condensate 3.0 -- 3.0 -- Modified naphthalene sulfonate formaldehyde condensate -- 3.0 -- 3.0 Vitamin E 1.0 1.0 -- -- Modified Vitamin E -- -- 1.0 1.0 Sodium dodecylbenzenesulfonate 1.4 1.4 1.4 1.4 Citric acid 0.033 0.033 0.033 0.033 Sodium citrate 0.067 0.067 0.067 0.067 lactose 47.225 47.225 47.225 47.225 Anhydrous sodium sulfate 47.225 47.225 47.225 47.225 1.2 Modified naphthalene sulfonate formaldehyde condensate The preparation method of the modified naphthalene sulfonate formaldehyde condensate in Table 1 includes the following steps: S1. Add 75.0 g of naphthalene sulfonate formaldehyde condensate and 500 mL of toluene to a 5 L container, and purge with nitrogen gas at a flow rate of 50 mL / min to remove air; heat the container in a water bath to 80 °C and stir at 200 r / min for 30 min to dissolve the naphthalene sulfonate formaldehyde condensate toluene solution; slowly add 22.5 g of ethylene glycol diglycidyl ether dropwise along the inner wall of the container to the naphthalene sulfonate formaldehyde condensate toluene solution at a drop rate of 1.5 mL / min, while maintaining stirring at 200 r / min during the dropwise addition; after the dropwise addition is complete, react at 80 °C, 200 r / min, and under a nitrogen atmosphere for 2 h to obtain a hydroxylated naphthalene sulfonate formaldehyde condensate solution; S2. Add 25g of polyethylene glycol monomethyl ether MPEG-450 to the hydroxylated naphthalene sulfonate formaldehyde condensate solution, stir at 200r / min for 15min, then heat to 90℃, add 0.5g of stannous octoate, and react at 90℃, 200r / min, under a nitrogen atmosphere for 4h. S3. Continue stirring and allow to cool naturally to room temperature. Distill at 60℃ and -0.095MPa for 2 hours to remove toluene. Add 100mL of deionized water to the distillation residue, stir and wash at 100r / min for 30min, allow to stand and separate into layers, then discard the upper aqueous phase. Repeat washing 3 times. S4. Transfer the washed product to a vacuum drying oven and dry it at 60℃ and -0.090MPa for 4 hours. Then pulverize it through a 200-mesh sieve to obtain the modified naphthalene sulfonate formaldehyde condensate.
[0022] 1.3 Modified Vitamin E The preparation method of modified vitamin E in Table 1 includes the following steps: S1. Add 68.3g of vitamin E and 400mL of anhydrous ethanol to a 5L container, heat to 50℃ in a constant temperature water bath, and stir at 150r / min for 20min to dissolve vitamin E; after naturally cooling to 30℃, add 31.7g of acrylic acid, and continue stirring for 10min to obtain a transparent reaction solution. S2. Add 0.3g of initiator benzoyl peroxide to the reaction solution and stir at 150r / min for 8min; heat to 75℃ in a constant temperature water bath, wrap the outer wall of the container with black light-blocking cloth, and react at a constant temperature for 3h with stirring at 150r / min. S3. Continue stirring and allow to cool naturally to room temperature. Distill at 60℃ and -0.090MPa for 1.5h to remove anhydrous ethanol and obtain a concentrate. Add 150mL of deionized water to the concentrate, stir and wash at 100r / min for 40min, let stand for 11h and discard the aqueous phase. Repeat the washing twice. S4. Transfer the washed product to a vacuum drying oven and dry it at 60℃ and -0.095MPa for 8 hours. Then pulverize it through a 200-mesh sieve to obtain modified vitamin E.
[0023] 1.4 Soluble Powder The specific preparation method of the soluble powder in Table 1 is as follows: add dispersant, stabilizer and 5% of the total mass of deionized water to a 5L container, stir to dissolve and then spray evenly onto the water-soluble filler, stir and mix at 150 r / min for 20 min; then add the remaining other components, stir and mix at 150 r / min for 20 min, and then air-jet pulverize through a 75 μm sieve (particle size ≥ 98% of the material passes through the 75 μm sieve) to obtain the soluble powder.
[0024] 1.5 Performance Testing The test indicators are shown in Table 2, and the test results are shown in Tables 3 and 4.
[0025] Table 2. Test Items and Test Methods
[0026] Table 3. Effects of different additives on the properties of soluble powders
[0027] As shown in Table 3, the residue of soluble powder Q4, which uses modified naphthalene sulfonate formaldehyde condensate and modified vitamin E, is only 0.1% after 5 minutes and only 0.3% after 18 hours, which is significantly better than that of Q1-Q3. This indicates that the modified naphthalene sulfonate formaldehyde condensate combined with modified vitamin E can synergistically prevent the aggregation of low-content active ingredients and improve the dispersion effect. Moreover, the wetting time of Q4 is 23 seconds, which is significantly lower than that of Q1-Q3, indicating that the modified naphthalene sulfonate formaldehyde condensate and sodium dodecylbenzene sulfonate can synergistically improve the wetting effect, which helps to achieve rapid dissolution and uniform dispersion of soluble powder.
[0028] Secondly, the Q4 powder is uniform and free of lumps, with a 75μm sieve pass rate of 99.2%, which is slightly higher than that of Q1-Q3. This indicates that the modified naphthalene sulfonate formaldehyde condensate and modified vitamin E do not affect the formability of the soluble powder, but rather improve the physical properties of the powder.
[0029] In addition, the moisture absorption rate of Q4 was only 1.3%, which was significantly lower than that of Q1 and significantly lower than that of Q2 and Q3. This may be because the modified naphthalene sulfonate formaldehyde condensate and modified vitamin E were dispersed on the surface of the water-soluble filler, which blocked the moisture absorption channels of the soluble powder and helped to improve storage stability.
[0030] Table 4. Effects of thermal storage on the properties of different soluble powders
[0031] As shown in Tables 3 and 4, modified vitamin E possesses both pH-regulating and antioxidant functions, stabilizing the system pH within the suitable range of 5.0-7.0 for indolebutyric acid. After heat storage, the pH fluctuations in Q3 and Q4 were minimal, indicating that it helps inhibit the pyrolysis of indolebutyric acid. Furthermore, Q4 exhibited the least pyrolysis of the active ingredient after heat storage, demonstrating that the modified naphthalenesulfonate formaldehyde condensate can continuously prevent the aggregation of 14-hydroxybrassinosteroidol, reducing the heat storage degradation rate, and synergistically enhancing the dispersion and stability of the active ingredient in conjunction with modified vitamin E.
[0032] 2. Field experiments 2.1 The tested bok choy Shanghai Qing 2.2 Test Methods Multiple plots were divided, each 1m × 1m, with a plot spacing of 0.5m. A randomized block design was used, with multiple treatment groups. Bok choy was sown uniformly after germination until it showed white sprouts, with a row spacing of 20cm and a plant spacing of 15cm. Spraying was performed once at the 2-leaf-1-heart stage and again at the 4-leaf-1-heart stage, with a spraying volume of 500mL per plot. Water and fertilizer management and other treatments were identical across all treatment groups. Details of each treatment group are as follows: Treatment 1: Spray with an 800-fold dilution of Q1 powder; Treatment 2: Spray with an 800-fold dilution of Q2 powder; Treatment 3: Spray with an 800-fold dilution of Q3 powder; Treatment 4: Spray with an 800-fold dilution of Q4 powder; Treatment 5: Spray with an equal amount of clean water.
[0033] 2.3 Measurement Indicators The bok choy was harvested 15 days after the second spraying. The plant height, fresh weight of the above-ground parts, vitamin C content and soluble sugar content of the bok choy were measured. The results are shown in Table 5.
[0034] Table 5. Effects of thermal storage on the properties of different soluble powders
[0035] As shown in Table 5, the use of Q4 soluble powder can significantly increase the plant height, fresh weight of the above-ground parts, vitamin C content and soluble sugar content of Chinese cabbage, indicating that the soluble powder of the present invention has excellent effects on promoting the growth of Chinese cabbage and improving its yield and quality.
[0036] In summary, the soluble powder of this invention works synergistically with its auxiliary components to achieve rapid wetting of the finished product, long-term stability of the active ingredients, and good dispersion uniformity. It also has excellent effects on promoting the growth of Chinese cabbage, increasing its yield and quality. This invention is of great significance for developing soluble powders containing indolebutyric acid and 14-hydroxybrassinosteroidol and achieving high-quality and high-yield Chinese cabbage production.
Claims
1. A soluble powder, characterized in that, It is prepared by weight percentage from the following components: indolebutyric acid 0.04-0.06%, 14-hydroxybrassinosteroidol 0.00008-0.00012%, dispersant 1.5-5.0%, stabilizer 0.5-2.0%, wetting agent 1.0-3.0%, pH buffer 0.8-1.2%, and water-soluble filler to 100%; wherein the dispersant is a modified naphthalene sulfonate formaldehyde condensate; and the stabilizer is modified vitamin E.
2. The soluble powder according to claim 1, characterized in that, The preparation method of the modified naphthalene sulfonate formaldehyde condensate includes the following steps: S1. Add 75.0 g of naphthalene sulfonate formaldehyde condensate and 500 mL of toluene to a 5 L container, and purge with nitrogen gas at a flow rate of 50 mL / min to remove air; heat the container in a water bath to 80 °C and stir at 200 r / min for 30 min to dissolve the naphthalene sulfonate formaldehyde condensate toluene solution; slowly add 22.5 g of ethylene glycol diglycidyl ether dropwise along the inner wall of the container to the naphthalene sulfonate formaldehyde condensate toluene solution at a drop rate of 1.5 mL / min, while maintaining stirring at 200 r / min during the dropwise addition; after the dropwise addition is complete, react at 80 °C, 200 r / min, and under a nitrogen atmosphere for 2 h to obtain a hydroxylated naphthalene sulfonate formaldehyde condensate solution; S2. Add 25g of polyethylene glycol monomethyl ether MPEG-450 to the hydroxylated naphthalene sulfonate formaldehyde condensate solution, stir at 200r / min for 15min, then heat to 90℃, add 0.5g of stannous octoate, and react at 90℃, 200r / min, under a nitrogen atmosphere for 4h. S3. Continue stirring and allow to cool naturally to room temperature. Distill at 60℃ and -0.095MPa for 2 hours to remove toluene. Add 100mL of deionized water to the distillation residue, stir and wash at 100r / min for 30min, allow to stand and separate into layers, then discard the upper aqueous phase. Repeat washing 3 times. S4. Transfer the washed product to a vacuum drying oven and dry it at 60℃ and -0.090MPa for 4 hours. Then pulverize it through a 200-mesh sieve to obtain the modified naphthalene sulfonate formaldehyde condensate.
3. The soluble powder according to claim 1, characterized in that, The method for preparing the modified vitamin E includes the following steps: S1. Add 68.3g of vitamin E and 400mL of anhydrous ethanol to a 5L container, heat to 50℃ in a constant temperature water bath, and stir at 150r / min for 20min to dissolve vitamin E; after naturally cooling to 30℃, add 31.7g of acrylic acid, and continue stirring for 10min to obtain a transparent reaction solution. S2. Add 0.3g of initiator benzoyl peroxide to the reaction solution and stir at 150r / min for 8min; heat to 75℃ in a constant temperature water bath, wrap the outer wall of the container with black light-blocking cloth, and react at a constant temperature for 3h with stirring at 150r / min. S3. Continue stirring and allow to cool naturally to room temperature. Distill at 60℃ and -0.090MPa for 1.5h to remove anhydrous ethanol and obtain a concentrate. Add 150mL of deionized water to the concentrate, stir and wash at 100r / min for 40min, let stand for 11h and discard the aqueous phase. Repeat the washing twice. S4. Transfer the washed product to a vacuum drying oven and dry it at 60℃ and -0.095MPa for 8 hours. Then pulverize it through a 200-mesh sieve to obtain modified vitamin E.
4. The soluble powder according to claim 1, characterized in that, The wetting agent is sodium dodecyl sulfate.
5. The soluble powder according to claim 1, characterized in that, The pH buffer is composed of citric acid and sodium citrate in a 1:2 molar ratio.
6. The soluble powder according to claim 1, characterized in that, The water-soluble filler is composed of lactose and anhydrous sodium sulfate in equal mass ratios.
7. A method for preparing the soluble powder according to any one of claims 1-6, characterized in that, Specifically, the dispersant, stabilizer, and 5% of the total mass of the finished product in deionized water are added to a 5L container. After stirring and dissolving, the mixture is evenly sprayed into the water-soluble filler and stirred at 150 r / min for 20 min. Then, the remaining ingredients are added and stirred at 150 r / min for 20 min. The mixture is then pulverized by air jet milling and sieved to obtain the soluble powder.
8. The application of the soluble powder according to any one of claims 1-6 in promoting the growth of Chinese cabbage and improving its yield and quality.