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Preparation method for 2,4-bis(n-octylthiomethyl)-6-methylphenol serving as antioxidant

A technology of o-cresol and antioxidant, which is applied in the field of antioxidant preparation, can solve the problems of many contact opportunities between materials and air, many personnel requirements, and low production capacity, and achieves easy industrial production, simple process, and high production efficiency. powerful effect

Inactive Publication Date: 2018-01-12
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The purpose of the invention is to overcome the existing batch method preparation method, there are many personnel requirements, low production capacity, environmental pollution of the incoming and outgoing materials, and the crude product 2,4-bis(n-octyl Sulfuryl methylene)-6-methylphenol often has deficiencies such as color, which provides a continuous reaction, strong production capacity, and less environmental pollution antioxidant 2,4-bis(n-octyl sulfide The preparation method of methylene)-6-methylphenol

Method used

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  • Preparation method for 2,4-bis(n-octylthiomethyl)-6-methylphenol serving as antioxidant
  • Preparation method for 2,4-bis(n-octylthiomethyl)-6-methylphenol serving as antioxidant

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Experimental program
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Effect test

Embodiment 1

[0031] Get raw material paraformaldehyde (36.24g, 1.21mol), o-cresol (34.69g, 0.32mol), n-octyl mercaptan (98.3g, 0.67mol), piperidine (2.72g, 0.032mol), solvent DMF ( 60.0mL) into a 250mL three-necked flask, stirred, and heated to about 60°C. Then use a metering pump to pump it into a glass tube reactor with a diameter of 16 mm and a length of 1 m for reaction. The reactor is spring-shaped and heated to about 180°C with an oil bath. The flow rate is 10mL / min, and the residence time is about 20min. The effluent was collected, and the low-boiling substances were removed under reduced pressure to obtain 125.52 g of crude product. After cooling, it was recrystallized from anhydrous methanol to obtain 120.05 g of a colorless product.

Embodiment 2

[0033] Get raw material paraformaldehyde (62.40g, 2.08mol), o-cresol (70.28g, 0.65mol), n-octyl mercaptan (209.18g, 1.43mol), piperidine (9.37g, 0.11mol), solvent DMF ( 100.0mL) into a 500mL three-necked flask, stirred, and heated to about 60°C. Then use a metering pump to pump it into a glass tube reactor with a diameter of 16 mm and a length of 1 m for reaction. The reactor is spring-shaped and heated to about 180°C with an oil bath. The flow rate is 10mL / min, and the residence time is about 20min. The material flowing out was collected with a three-necked flask, and the low boiling point substances were removed under reduced pressure to obtain 249.46 g of crude product. After cooling, it was recrystallized from anhydrous methanol to obtain 202.15 g of a colorless product.

Embodiment 3

[0035] Get raw material paraformaldehyde (50.70g, 1.69mol), o-cresol (50.82g, 0.47mol), n-octyl mercaptan (150.67g, 1.03mol), piperidine (8.52g, 0.10mol), solvent DMF ( 97.8mL) into a 500mL three-necked flask, stirred, and heated to about 60°C. Then use a metering pump to pump it into a glass tube reactor with a diameter of 16 mm and a length of 1 min for reaction. The reactor is spring-shaped and heated to about 180°C with an oil bath. The flow rate is 10mL / min, and the residence time is about 20min. Collect the flow-out material with a three-necked flask, and remove low-boiling substances under reduced pressure to obtain 249.47 g of crude product. After cooling, it was recrystallized from anhydrous methanol to obtain 202.11 g of a colorless product.

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Abstract

The invention relates to a preparation method for 2,4-bis(n-octylthiomethyl)-6-methylphenol serving as an antioxidant. The preparation method is characterized by comprising the following steps: in theexistence of a secondary amine catalyst, enabling raw materials, namely, o-methylphenol, paraformaldehyde and n-octyl mercaptan to react in a continuous pipeline reactor to generate the 4-bis(n-octylthiomethyl)-6-methylphenol serving as the antioxidant; removing a solvent, water, the catalyst and excessive unreacted raw materials to obtain a product after the reaction, wherein the product can befurther purified. The invention provides a continuous preparation method for the 2,4-bis(n-octylthiomethyl)-6-methylphenol, which is high in production capacity and less in environmental pollution.

Description

technical field [0001] The invention relates to a preparation method of an antioxidant, specifically a preparation process of a phenolic antioxidant 1520, which is a preparation process of o-cresol, n-octyl mercaptan, and paraformaldehyde under the catalysis of a secondary amine. After the reaction in a pipelined reactor, the method is purified to obtain a colorless product with a light odor. Background technique [0002] The antioxidant 2,4-bis(n-octylthiomethylene)-6-methylphenol, also known as antioxidant 1520, has the molecular formula C 25 h 44 OS 2 , the structural formula is as follows: [0003] [0004] 2,4-bis(n-octylthiomethylene)-6-methylphenol is a hindered phenolic antioxidant containing a thiol alkyl group, which has two functional groups of thioether and hindered phenol in its structure. Two types of groups with synergistic effect together provide antioxidant effect. 2,4-bis(n-octylthiomethylene)-6-methylphenol has the advantages of low toxicity, littl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/14C07C323/16
Inventor 林富荣仲艳艳
Owner CHANGZHOU UNIV