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Synthesis method of diphenylamine L57 and L67

A synthetic method, the technology of diphenylamine, applied in the field of medicinal chemistry, can solve the problems of unsatisfactory product quality, yield and production cost, low catalytic activity of activated clay, no decolorization of catalyst, etc., and achieve outstanding economy and environmental protection , high economy and environmental protection, easy to separate the effect

Active Publication Date: 2021-06-22
JIANGSU JIYI NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The common deficiencies of these disclosed technologies are that the quality of the product, the yield and / or the production cost are unsatisfactory
For example, when anhydrous AlCl3 is used as a catalyst, chlorine is likely to remain, causing the color to be dark brown, and there is also a risk of corrosion of equipment; the catalytic activity of activated clay is not high, and the product is too average, so it is only suitable for those who do not know the position and number of substituents. The required low-quality alkylated diphenylamine antioxidant; although the amount of heteropoly acid is small, the reaction temperature is high, the catalyst has no decolorization function, and the product color is dark, etc.

Method used

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  • Synthesis method of diphenylamine L57 and L67
  • Synthesis method of diphenylamine L57 and L67

Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0028] Preparation Example 1: AlCl 3 -SnCl 2 Preparation of Two-Component Supported Catalyst

[0029] The sepiolite was calcined at 700°C for 6h in a muffle furnace to activate it. Soak the activated sepiolite in 10% sulfuric acid solution for 24 hours, then centrifuge to separate solid particles, wash thoroughly with water and absolute ethanol in sequence, and dry in vacuum for 4 hours to obtain a catalyst carrier. Take 20 g of the catalyst carrier, add 250 mL of carbon tetrachloride, then add 6.0 g of anhydrous aluminum trichloride and 2.0 g of anhydrous stannous chloride, and stir for 2 h under reflux. Filter, wash with carbon tetrachloride 3 times, and vacuum-dry at 75°C for 10h, then place in a muffle furnace and calcinate at 280°C for 3h to obtain AlCl 3 -SnCl 2 Two-component supported catalyst. The loading was measured by atomic absorption spectroscopy to be 25.6% (calculated based on sepiolite), and the mass ratio of aluminum trichloride to stannous chloride was 1...

preparation example 2

[0030] Preparation Example 2: AlCl 3 -SnCl 2 Preparation of Two-Component Supported Catalyst

[0031] The sepiolite was calcined at 700°C for 6h in a muffle furnace to activate it. Soak the activated sepiolite in 15% sulfuric acid solution for 24 hours, then centrifuge to separate solid particles, wash thoroughly with water and absolute ethanol in sequence, and dry in vacuum for 4 hours to obtain a catalyst carrier. Take 20g of the catalyst carrier, add 250mL of carbon tetrachloride, then add 7.5g of anhydrous aluminum trichloride and 2.5g of anhydrous stannous chloride into it, and stir for 2h under reflux. Filter, wash with carbon tetrachloride 3 times, and vacuum-dry at 75°C for 10h, then place in a muffle furnace and calcinate at 280°C for 3h to obtain AlCl 3 -SnCl 2 Two-component supported catalyst. Using atomic absorption spectrometry, the loading capacity was measured to be 29.4% (calculated based on sepiolite), and the mass ratio of aluminum trichloride to stannou...

Embodiment 1

[0036] Embodiment 1: the synthesis of nonyl diphenylamine (antioxidant L67)

[0037] Add 169.0 grams of diphenylamine, 252.5 grams of nonene in the autoclave, the catalyst 15g of Preparation Example 1, the hydrogenated cardanol-based polymerization inhibitor 5-pentadecyl-2-(((4-(phenylamino )phenyl)amino)methyl)phenol, replace the gas in the system with nitrogen several times, close the reactor, heat to 80°C to melt the diphenylamine and start stirring, then further heat up to 170°C for reaction, the reaction pressure is controlled At 0.4MPa. As the reaction proceeds, the pressure in the reactor decreases gradually. When the reaction pressure drops to 0.2MPa, 126.2g nonene is added to continue the reaction for 2 hours, and then 126.2g nonene is added again to continue the reaction for 4 hours. Stop reaction afterwards, reclaim described AlCl with fiber membrane filtration 3 -SnCl 2 Two-component supported catalyst, liquid phase sampling and analysis of components, and vacuu...

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Abstract

The invention provides a method for synthesizing a liquid alkyl diphenylamine antioxidant, especially a synthesis method of nonyl diphenylamine (antioxidant L67) and octyl / butyl diphenylamine (antioxidant L57). According to the method, an AlCl3-SnCl2 bi-component supported catalyst is used, and the AlCl3-SnCl2 bi-component supported catalyst is high in catalytic efficiency, good in selectivity, easy to separate from a reaction system, capable of being recycled and very outstanding in economical efficiency and environmental protection property; the obtained liquid alkyl diphenylamine antioxidant is high in quality, good in durability and high in oxidation resistance. Therefore, the synthesis method disclosed by the invention is suitable for being applied to industrial production.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, in particular, the invention relates to a preparation method of cimetidine. Background technique [0002] Alkyl dianiline antioxidants have a history of more than half a century, and they have attracted widespread attention due to their excellent oxidation resistance and good compatibility with oil and rubber. Divided by physical form, there are two common types of alkyl dianiline antioxidants, one is solid alkyl dianiline, usually light brown or off-white powder, including octyl dianiline (antioxidant OD) and cumyl diphenylamine Aniline (antioxidant KY-405), mainly used as an antiaging agent for light-colored or bright-colored rubber; the other is liquid alkyl diphenylamine, including octyl / butyl diphenylamine (antioxidant L57), nonyl Diphenylamine (antioxidant L67) and styryl diphenylamine (antioxidant DFC-34), etc., are mainly used as lubricating oil antioxidants, flexible foam polyurethane...

Claims

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Application Information

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IPC IPC(8): C07C209/68C07C209/90C07C211/55B01J27/125B01J27/135
CPCB01J27/125B01J27/135C07C209/68C07C209/90C07C211/55Y02P20/584
Inventor 郭骄阳
Owner JIANGSU JIYI NEW MATERIAL CO LTD
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