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Preparation method of plant growth regulation compound sodium nitrophenolate

A technology for plant growth regulation and complex sodium nitrophenolate, which is applied in the direction of plant growth regulators, plant growth regulators, botany equipment and methods, etc., can solve the problem of increasing the cost of 5-nitroguaiacol sodium, 5-nitroguaiacol The low yield of sodium guaiacol and the difficult separation of by-products have achieved the effects of promoting healthy development, improving market competitiveness, and reducing the difficulty of obtaining

Inactive Publication Date: 2021-08-03
何志松
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] 5-Nitroguaiacol Sodium is the most active monomer in Compound Sodium Nitrophenolate. At present, the method of synthesizing 5-Nitroguaiacolate Sodium is mainly chemical synthesis. The current route commonly used in industrial production is Guaiac Wood phenol is prepared through acetylation, nitration, and hydrolysis reactions; although this process is simple and easy to control, each step of the reaction is easy to realize, but because of many by-products, the yield of 5-nitroguaiacol sodium is low (about 42% ), and the by-products are not easy to separate
Not only that, the process requires a large amount of acetic anhydride, but acetic anhydride is a precursor drug, and its application is increasingly restricted
Moreover, the price of acetic anhydride is also constantly rising, which will inevitably cause the cost of 5-nitroguaiacol sodium to increase

Method used

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  • Preparation method of plant growth regulation compound sodium nitrophenolate
  • Preparation method of plant growth regulation compound sodium nitrophenolate
  • Preparation method of plant growth regulation compound sodium nitrophenolate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A kind of preparation method of plant growth regulating compound sodium nitrophenolate, its specific scheme is as follows:

[0027] Add 12.4g of guaiacol and 80g of organic solvent into the reaction kettle, stir and mix evenly, then control the temperature to 5°C, slowly add 8g of acetyl chloride into the reaction kettle under stirring conditions, and control the addition within 60min. After the completion, the temperature was controlled to 35°C, and the stirring reaction was continued for 2 hours. After the completion, the vacuum distillation was performed under a vacuum of 0.08MPa, and the distillate was collected to obtain acetylguaiacol; then 16.6g of acetylguaiacol and 8g of acetic acid were mixed evenly Finally, add 10g of fuming nitric acid, slowly control the temperature to 50°C, react for 2h, finally precipitate in ice water, filter, wash with water, add to 30g of sodium hydroxide solution, mix well, add 0.1g of phase transfer catalyst, and then heat up to 80 ℃...

Embodiment 2

[0036] A kind of preparation method of plant growth regulating compound sodium nitrophenolate, its specific scheme is as follows:

[0037] Add 14.8g of guaiacol and 110g of organic solvent into the reaction kettle, stir and mix evenly, then control the temperature to 10°C, slowly add 10.8g of acetyl chloride into the reaction kettle while stirring, and control the addition within 90min After the completion, the temperature was controlled to 40°C, and the stirring reaction was continued for 3.5 hours. After the completion, the vacuum distillation was carried out under a vacuum of 0.085MPa, and the distillate was collected to obtain acetylguaiacol; then 18.2g of acetylguaiacol and 10g of acetic acid After mixing evenly, add 10-15g of fuming nitric acid, slowly control the temperature to 65°C, react for 4h, then precipitate in ice water, filter, wash with water, add to 38g of sodium hydroxide solution, mix evenly, add 0.24g of phase transfer catalyst, Then heat up to 90°C, stir a...

Embodiment 3

[0046] A kind of preparation method of plant growth regulating compound sodium nitrophenolate, its specific scheme is as follows:

[0047] Add 16.8g of guaiacol and 140g of organic solvent into the reaction kettle, stir and mix evenly, then control the temperature to 15°C, slowly add 12.8g of acetyl chloride into the reaction kettle while stirring, and control the addition within 120min After the completion, the temperature was controlled to 45°C, and the stirring reaction was continued for 5 hours. After the completion, the vacuum distillation was performed under a vacuum of 0.095MPa, and the fraction was collected to obtain acetylguaiacol; then 20.4g of acetylguaiacol was mixed with 12g of acetic acid After uniformity, add 15g of fuming nitric acid, slowly control the temperature to 75°C, react for 6h, then precipitate in ice water, filter, wash with water, add to 48g of sodium hydroxide solution, mix well, add 0.38g of phase transfer catalyst, and then heat up to Stir and r...

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Abstract

The invention relates to the field of preparation of agricultural auxiliaries, in particular to a preparation method of plant growth regulation compound sodium nitrophenolate. According to the invention, acetyl chloride is adopted to replace acetic anhydride which is a precursor to serve as a protecting group for hydroxyl acetylation, so that the acquisition difficulty of process raw materials is reduced, and the production cost of 5-nitroguaiacol sodium salt is controlled; and besides, a phase transfer catalyst is applied to the hydrolysis reaction of 5-nitroacetyl guaiacol, so that the hydrolysis of the product can be effectively promoted, the yield of the hydrolysis reaction is greatly improved, and the overall yield of the 5-nitroguaiacol sodium salt is further improved. The prepared 5-nitroguaiacol sodium salt has the advantage of low cost, and as a main effective component of the compound sodium nitrophenolate, the 5-nitroguaiacol sodium salt can improve the market competitiveness of the compound sodium nitrophenolate product, avoid the behavior that the drug effect of the compound sodium nitrophenolate product is reduced due to the fact that the cost of the 5-nitroguaiacol sodium salt is high and the ratio is reduced by bad manufacturers, and make contribution for promoting the benign development of the market.

Description

technical field [0001] The invention relates to the field of preparation of agricultural adjuvants, in particular to a method for preparing plant growth regulating sodium compound nitrophenolate. Background technique [0002] Sodium nitrophenolate is a high-efficiency plant growth regulator first discovered in Japan in the 1960s. The Japanese product name is Aiduoshou. The product dosage form is 1.8% sodium nitrophenolate aqueous solution, which can be diluted 2000-6000 times for use. The actual commonly used concentration is 3-10ppm, which is equivalent to the dosage of 0.2-0.4 grams per mu, which has obvious effect of increasing production, and its preparation method has attracted people's attention. [0003] CN103027035A discloses a nano-preparation of sodium nitrophenolate and its preparation method. The preparation method follows the steps in turn: mix sodium nitrophenolate powder with distilled water, and the dosage ratio of sodium nitrophenolate powder to distilled wa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A01N33/22A01P21/00C07C201/12C07C205/22C07C201/08C07C205/43C07C67/14C07C69/157B01J31/06C08G65/331C08G65/333C08G65/336
CPCA01N33/22B01J31/06C07C67/14C07C69/157C07C201/08C07C201/12C07C205/22C07C205/43C08G65/3317C08G65/33306C08G65/336C08G2650/04Y02P20/55
Inventor 何志松
Owner 何志松
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