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Synthesis method for hindered phenolic compound antioxidant 330

A synthesis method and technology for hindered phenols, which are applied in the field of organic chemical synthesis, can solve the problems that the catalyst types need to be developed, the reaction process needs to be simplified, the reaction yield needs to be improved, etc., and the effect of good application potential and prospects can be achieved.

Active Publication Date: 2015-07-22
黑龙江佳宜宏大化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] Li Chunhua et al. ("Research on the Synthesis of Antioxidant 330", Plastic Additives, 2006, 6, 29-31, 47) disclosed a method for preparing antioxidant 330 by catalyzing dimethylamine, but the reaction temperature It is relatively low and has the problem of harsh process conditions, and the product yield is only 75%, so it cannot be applied to large-scale production
[0011] As mentioned above, although many researchers have developed a variety of synthetic methods for hindered phenol antioxidant 330, there are still many defects in these methods, such as the reaction yield needs to be improved, the reaction process needs to be simplified, and the types of catalysts need to be developed. question

Method used

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  • Synthesis method for hindered phenolic compound antioxidant 330
  • Synthesis method for hindered phenolic compound antioxidant 330
  • Synthesis method for hindered phenolic compound antioxidant 330

Examples

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preparation example 1

[0044] Preparation Example 1: Preparation of Carbon Nanotube-supported Acid Catalyst

[0045] S1: adding carbon nanotubes to a sufficient amount of concentrated nitric acid with a concentration of 90% by mass, heating to reflux for 35 minutes, filtering, fully washing with deionized water, and drying in a vacuum oven to obtain acidified carbon nanotubes;

[0046] S2: adding the acidified carbon nanotubes obtained in step S1 into absolute ethanol, and fully stirring until a suspension is formed; wherein the mass volume ratio of the acidified carbon nanotubes to absolute ethanol is 1:4g / ml ;

[0047] S3: Add tetraisopropyl titanate Ti(OC) dropwise to the suspension obtained in step S2 3 h 7 ) 4 , continue to stir while adding dropwise until it becomes a sol, then fully dry and pulverize to obtain powder; wherein the mass of the acidified carbon nanotubes (ie, the acidified carbon nanotubes obtained in step S1) and tetraisopropyl titanate The ratio is 1:0.2;

[0048] S4: Add...

preparation example 2

[0049] Preparation Example 2: Preparation of Carbon Nanotube-supported Acid Catalyst

[0050] Except that the acidification treatment of step S1 was not carried out, preparation example 2 was carried out in the same manner as preparation example 1, that is, the carbon nanotubes were not subjected to acidification treatment with concentrated nitric acid, but the treatment of step S2 was directly carried out, and the obtained carbon nanotubes were The supported acid catalyst was named T2.

preparation example 3-8

[0051] Preparation Example 3-8: Preparation of Carbon Nanotube-supported Acid Catalyst

[0052] Except changing the temperature rise rate in step S4, other all remain unchanged, carry out preparation example 3-8 with the same embodiment as preparation example 1, the gained carbon nanotube supported acid catalyst is named as T3-T8 in sequence; Wherein temperature rise rate, resulting catalyst see Table 1 below Shown:

[0053] Table 1 .Carbon nanotube-supported acid catalysts obtained at different heating rates

[0054]

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Abstract

The invention provides a synthesis method for a hindered phenolic compound antioxidant 330; the method comprises the following steps: in the presence of a ternary composite catalyst and a diluted hydrochloric acid aqueous solution with specific concentration and amount, a compound represented by the following formula (I) and a compound represented by the following formula (II) are subjected to a reaction in a solvent, and thus the antioxidant 330 is obtained. In the synthesis method, through suitable selection and combination of a catalyst system and a solvent system, the target product is obtained with high yield; and the synthesis method is quite suitable for industrialization large-scale production and application and has a quite broad market prospect.

Description

technical field [0001] The present invention relates to a method for synthesizing an antioxidant, more particularly to a method for synthesizing a hindered phenolic antioxidant, i.e. Antioxidant 330, which belongs to the technical field of organic chemical synthesis. Background technique [0002] Antioxidants are one of the reagents used to prevent material aging. Due to the poor oxidation resistance of polymer materials during production, storage and use, product performance is often unstable or significantly decreased. Therefore, the use of antioxidants is increasingly popular General attention. [0003] So far, people have developed a variety of antioxidants, among which hindered phenolic compounds such as antioxidant 330 is a very widely used antioxidant, its chemical name is 1,3,5-trimethyl-2 , 4,6-tri(3,5-di-tert-butyl-4-hydroxybenzyl)benzene (where t-Bu is tert-butyl, the same below), its structural formula is as follows: [0004] [0005] The antioxidant was dev...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/18C07C39/15B01J31/26B01J27/02
CPCC07C17/263C07C37/18B01J27/02B01J31/0227B01J31/0244B01J31/26B01J2231/4205B01J35/19C07C39/15C07C22/04
Inventor 李翠勤王俊施伟光李杰张志秋刘继伟
Owner 黑龙江佳宜宏大化工有限公司
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