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Method for synthesizing modified-antioxidant 300

A synthesis method and antioxidant technology are applied in the improved synthesis field of antioxidant 300, which can solve the problems of difficulty in mastering the degree of reaction equilibrium, low yield of reaction crude products, and unsatisfactory effects, and achieves a thorough organic reaction and synthesis. The method is ingenious, reasonable and easy to implement

Inactive Publication Date: 2007-05-30
淄博市新材料研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] As we all know, almost all organic reactions are quite complicated processes, which contain many side reactions, and the balance of the reactions is also difficult to grasp.
The synthesis process of Antioxidant 300 is no exception. We found in the experiment that due to the large dissolution of hydrogen chloride gas generated during the reaction process in the solution, the further progress of the forward reaction was prevented, and the thiolation reaction could not be carried out as we hoped. So thorough, resulting in low reaction crude yield
At present, the more traditional method is to pass N to the reaction system at the end of the thiolation reaction. 2 , drive away a certain amount of hydrogen chloride gas, and prolong the reaction time at the same time, but the effect is not very ideal
As can be seen from relevant reports, the yield of antioxidant 300 crude product prepared by this method is about 85%, which is still low and needs further improvement

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 100g of 5-methyl-2-tert-butylphenol and 300ml of petroleum ether into a 500ml four-necked flask equipped with a stirrer, a thermometer and a constant pressure funnel, and cool the solution to 12°C under stirring, and dissolve the dissolved Put the petroleum ether (100ml) solution of sulfur dichloride (31.4g) into the constant pressure funnel, and slowly add it dropwise in the reaction flask within 2.5 hours, while keeping the temperature in the four-necked flask not exceeding 12°C, drop After the addition, continue to stir and keep warm, and pass NH at a flow rate of 30ml / min. 3 Gas 50min, detect solution pH value 7.3, stop aeration reaction solution and slowly rise to room temperature, wash to remove by-product and ammonium chloride, reaction solution pressure filtration, filter cake obtains crude product 101g after petroleum ether solvent washing low-temperature drying, yield is 92.6%. The melting point of the product was determined to be 157-159°C by capillary m...

Embodiment 2

[0018] Add 200g of 5-methyl-2-tert-butylphenol and 550ml of petroleum ether into a 1000ml four-necked reaction flask equipped with a stirrer, a thermometer and a constant pressure funnel, and cool the solution to 12°C under stirring. Pour the good sulfur dichloride (63g)+petroleum ether (200ml) solution into the constant pressure funnel, slowly drop the solution in the constant pressure funnel into the reaction flask within 3 hours, while keeping the temperature in the reaction flask not exceeding 12°C, After the dropwise addition, continue to stir and keep warm, and pass NH at a flow rate of 50ml / min. 3 Gas for 40 minutes, check the pH value of the solution to be 7.5, stop the aeration and the reaction solution slowly rises to room temperature, remove some by-products and ammonium chloride by washing with water, filter the solution under pressure, wash the filter cake with petroleum ether solvent and dry at low temperature to obtain antioxidant 300 The crude product is 102g, ...

Embodiment 3

[0020] Add 200g of 5-methyl-2-tert-butylphenol and 550ml of sherwood oil in a 1000ml four-necked reaction flask equipped with a stirrer, a thermometer and a constant pressure funnel, and make the solution drop to 10°C under stirring. The petroleum ether (200ml) solution that has been dissolved with sulfur dichloride (63g) is moved into a constant pressure funnel, and slowly added dropwise to the reaction flask within 3 hours, keeping the temperature of the solution not exceeding 10°C. Pass NH into the reaction bottle at a speed of 50ml / min 3 Gas for 30min, detect the pH value of the solution at 7.8, stop ventilation and slowly rise to room temperature, wash to remove by-products and ammonium chloride, pressurize and filter the reaction solution, wash the filter cake with petroleum ether solvent and dry at low temperature to obtain 98g of antioxidant 300 crude product, yield 90%. The melting point of the product was determined to be 157-159°C by capillary measurement.

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Abstract

An improved process for preparing the antioxidizing agent 300 includes such steps as the thio-reaction between SCl2 and 5-methyl-2-tert-butyl phenol existence of petroleum ether while filling N2 at final reaction phase for regulating pH value and promoting reaction, water washing the coarse product for removing by-product and impurities, filtering and drying. Its advantages are high purity and quality of product and no environmental pollution.

Description

technical field [0001] The invention relates to an improved synthetic method of antioxidant 300, which belongs to the synthetic technology of organic matter. Background technique [0002] Antioxidant 300 refers to 4,4'-thiobis(5-methyl-2-tert-butylphenol) antioxidant, which is a very good thiobisphenol antioxidant in polyolefin Adding a small amount can achieve the effect of preventing olefin degradation and delaying discoloration. Its synthetic route is prepared by thiolation of sulfur dichloride and 5-methyl-2-tert-butylphenol at a relatively low temperature under the condition of a non-polar solvent (such as petroleum ether). Crude product, but the yield is often not very high. There have been reports about using carbon tetrachloride as a reaction solvent. Although it can increase the reaction yield, carbon tetrachloride is poisonous and extremely harmful to the human body, and it has also been found in experiments that its solubility to 300 products is higher than that...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/14C07C321/30
Inventor 朱永国王文举黄东华
Owner 淄博市新材料研究所
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