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Preparation process of capryloyl hydroxamic acid

A technology of octanoyl hydroxamic acid and preparation process, which is applied in the field of preparation technology of octanoyl hydroxamic acid, can solve the problems of equipment corrosion, environmental pollution of waste liquid, difficult separation of catalyst and reaction system, etc. good effect

Active Publication Date: 2021-01-29
烟台东方化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In related industrial production, homogeneous catalysts are generally used for the esterification reaction of n-octanoic acid and ethanol. Homogeneous catalysts have the advantages of low cost, strong acidity, and high catalytic efficiency, but it is easy to cause equipment corrosion, and it is difficult to separate the catalyst from the reaction system. , Disadvantages such as environmental pollution caused by a large amount of waste liquid discharge

Method used

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Examples

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preparation example Construction

[0036] Examples of Preparation of Raw Materials and / or Intermediates

[0037] Styrene pretreatment: adding styrene to 2mol / L sodium hydroxide solution, stirring for 30min, standing still, taking the supernatant, then washing the supernatant with distilled water until the distilled water after washing is neutral; then Add anhydrous magnesium sulfate, dry for 12 hours, and filter to obtain pretreated styrene.

preparation example 1

[0039] TiO of Preparation Example 1 2 / ZrO 2 Each raw material and each raw material consumption of solid super acid are shown in table 1, and its preparation steps are as follows:

[0040] 1) Under the protection of nitrogen, add 0.9kg of pretreated styrene and 0.4kg of polyvinylpyrrolidone to 9kg of distilled water, stir and heat to 75°C, then add 0.014kg of potassium persulfate, stir for 8 hours, and then react at 4500r / Centrifuge at a speed of 5 min to obtain solid A, and then dry solid A at 70°C for 6 h to obtain polystyrene spheres;

[0041] 2) Put polystyrene balls in 13kg of distilled water, ultrasonically disperse for 10min, then add 1.2kg of zirconium oxychloride and 0.10kg of titanium sulfate, stir for 0.5h, and then add ammonia water dropwise during stirring to make the pH reach After 10 hours, stop the dropwise addition, then age for 22 hours, filter to obtain solid B, wash solid B with water three times, and then dry at 100°C for 7 hours to obtain solid C;

...

preparation example 2

[0044] TiO of Preparation Example 2 2 / ZrO 2 Each raw material and each raw material consumption of solid super acid are shown in table 1, and its preparation steps are as follows:

[0045] 1) Under the protection of nitrogen, add 1 kg of pretreated styrene and 0.5 kg of polyvinylpyrrolidone into 10 kg of distilled water, stir and heat to 78 ° C, then add 0.017 kg of potassium persulfate, stir for 7 hours, and then react at 5000 r / Centrifuge at a speed of 4 min to obtain solid A, and then dry solid A at 75°C for 5 h to obtain polystyrene spheres;

[0046]2) Put polystyrene balls in 15kg of distilled water, ultrasonically disperse for 15 minutes, then add 1.38kg of zirconium oxychloride and 0.12kg of titanium sulfate, stir for 0.5h, and then add ammonia water dropwise during stirring to make the pH reach 10 After that, stop the dropwise addition, then age for 24 hours, filter to obtain solid B, wash solid B with water for 3 times, and then dry at 105°C for 6 hours to obtain ...

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Abstract

The invention relates to the field of chemical synthesis, and particularly discloses a preparation process of capryloyl hydroxamic acid, which comprises the following steps: preparing ethyl n-caprylate, and preparing the capryloyl hydroxamic acid, wherein the ethyl n-caprylate is prepared by the following steps: mixing 1-1.5 kg of n-caprylic acid with 0.35-0.7 kg of ethanol, adding solid superacid, performing heating reflux for 5-7 hours, filtering to obtain precipitate and filtrate, and performing reduced pressure distillation on the filtrate to obtain the ethyl n-caprylate, and the obtainedprecipitate is washed and roasted to obtain the solid superacid, and the solid superacid is recycled to the preparation step of the ethyl n-caprylate for use. By using the solid superacid catalyst, the environmental friendliness of the esterification reaction in the n-capryloyl hydroxamic acid preparation process is improved.

Description

technical field [0001] The application relates to the field of chemical synthesis, more specifically, it relates to a preparation process of caprylyl hydroxamic acid. Background technique [0002] Caprylyl hydroxamic acid, also known as caprylyl hydroxamic acid, is an organic acid that can maintain a non-ionized state from acidic to neutral. It has high-efficiency chelation, can inhibit the active elements required by mold, and limit microorganisms. The environment required for growth is an ideal antibacterial agent and is widely used in the fields of cosmetics, medicine and fine chemicals. [0003] In the preparation process of octanoyl hydroxamic acid, it is usually first to generate n-octanoic acid ethyl ester through n-octanoic acid and ethanol under the catalysis of sulfuric acid; Obtain n-octanoyl hydroxamic acid. [0004] In related industrial production, homogeneous catalysts are generally used for the esterification reaction of n-octanoic acid and ethanol. Homogen...

Claims

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Application Information

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IPC IPC(8): C07C259/06C07C67/08B01J37/00B01J35/10B01J35/08B01J27/02B01J21/06C07C69/24
CPCC07C259/06C07C67/08B01J21/066B01J27/02B01J37/0018B01J35/51B01J35/61C07C69/24
Inventor 蔡建陈晓辉薛天辉秦莉锦
Owner 烟台东方化学有限公司
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