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Clean production method for preparing bisphenol antioxidant

A clean production and antioxidant technology, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of increased labor consumption and power consumption, limited number of repetitions, unfavorable environmental protection, etc., and achieve economical reaction Time, easy procurement, and the effect of protecting water resources and the environment

Active Publication Date: 2012-07-25
SHANDONG LINYI SUNNY WEALTH CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method disclosed in this patent uses surfactant sodium dodecylbenzene sulfonate and sulfuric acid as catalyst, and needs to use water not less than 1.3 times of the quality of the product obtained as the reaction solvent, and filter after the reaction, although the reaction process ends in The water-based solvent system can be reused, but the number of repetitions is limited, so the production process still produces a certain amount of wastewater containing organic matter and acidic impurities, which is not conducive to environmental protection, and the filtered cake needs to be crystallized with alcohol, which increases labor consumption. and power consumption

Method used

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  • Clean production method for preparing bisphenol antioxidant
  • Clean production method for preparing bisphenol antioxidant
  • Clean production method for preparing bisphenol antioxidant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] In a 500 ml four-neck flask equipped with electric stirring, a thermometer, a reflux condenser, and a nitrogen replacement device, add 100 grams (0.485 moles) of 2,6-di-tert-butylphenol, 150 milliliters of industrial ethanol (concentration 97%), Add 0.4 g of catalyst sodium hydroxide, replace with nitrogen, start stirring, raise the temperature to 65°C, start to slowly add 20.0 g of formaldehyde solution (37% formaldehyde concentration, 0.246 moles of formaldehyde) dropwise, and finish the dropwise addition in about 30 minutes. The temperature of the material is 75-85°C, keep the reflux reaction, after observing a large number of crystals, cool down to 50-60°C, replace with nitrogen, add 50 ml of ethanol, replace with nitrogen again, raise the temperature to 75-85°C, and continue the reaction After 20 minutes, after the reaction was replaced by nitrogen, 0.64 g of citric acid was added for neutralization. The neutralization temperature was 80-85°C, and the neutralization...

Embodiment 2

[0032] In a 500 ml four-necked flask equipped with electric stirring, a thermometer, a reflux condenser, and a nitrogen replacement device, add 100 grams (0.485 moles) of 2,6-di-tert-butylphenol, and 150 milliliters of industrial ethanol (recovered from Example 1) Ethanol, concentration 95%), add 0.5 g of catalyst potassium hydroxide, replace with nitrogen, start stirring, heat up to 80 ° C, start to slowly add 20.5 g of formaldehyde aqueous solution (formaldehyde concentration 37%, containing 0.253 moles of formaldehyde), about 40 minutes After the dropwise addition, control the temperature of the material in the flask to 80-85°C, and keep the reflux reaction. After observing a large amount of crystallization, cool down to 50-60°C, replace with nitrogen, add 50 ml of ethanol, replace with nitrogen again, and heat up to 80-85°C, continue to react for 20 minutes, add 0.535 g of glacial acetic acid for neutralization after the reaction is completed, and replace with nitrogen. The...

Embodiment 3

[0035]In a 500 ml four-neck flask equipped with electric stirring, a thermometer, a reflux condenser, and a nitrogen replacement device, add 100 grams (0.485 moles) of 2,6-di-tert-butylphenol, 150 ml of industrial isopropanol (concentration 95%) ), add 0.4 g of catalyst sodium hydroxide, replace with nitrogen, start stirring, heat up to 80°C, slowly add 19.0 g of formaldehyde solution (formaldehyde concentration 40%, containing 0.253 moles of formaldehyde) dropwise, and the dropwise addition ends in about 30 minutes. The temperature of the internal material is 80-90°C, keep the reflux reaction, after observing a large amount of crystallization, cool down to 50-60°C, replace with nitrogen, add 50 ml of isopropanol, replace with nitrogen again, and heat up to 80-90°C , continue to react for 20 minutes, add 0.64 g of citric acid for neutralization after the reaction is replaced by nitrogen, the neutralization temperature is 80-85°C, and the neutralization time is 10 minutes. ; an...

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Abstract

The invention provides a clean production method for preparing a bisphenol antioxidant. Alkyl phenol and aldehydes react under the action of a catalyst to prepare the bisphenol antioxidant. The method comprises the following steps: sequentially adding certain amounts of alkyl substituted phenol and lower alcohol solvents and the catalyst into a reaction kettle; replacing by introducing nitrogen gas, starting mixing, heating, slowly and dropwisely adding formalin, and keeping the reflux reaction to generate massive crystals; replacing by introducing nitrogen gas, supplementing a right amount of alcohol solvent, and continuing the reaction for some time; and neutralizing with organic acid, cooling, filtering to obtain the white or light yellow solid powdery product, and distilling the filtrate to recycle the solvent for cyclic utilization. The production process does not need water to participate into the reaction, can not generate wastewater, has the advantages of short production cycle, high product purity and high yield, is easy to control, and can overcome the defects in the prior art.

Description

technical field [0001] The invention relates to a preparation method of a bisphenol antioxidant, in particular to a clean production method of a bisphenol solid antioxidant. [0002] More specifically, the present invention relates to a clean production method without waste water and waste gas emission for preparing bisphenol antioxidants by reacting alkylphenols and aldehydes under the action of a catalyst. [0003] Bisphenol antioxidants involved in the present invention refer specifically to the compound of the following structure: [0004] [0005] where R 1 , R 2 is C 1 -C 5 Straight chain or branched alkyl substituent, R 1 , R 2 Can be the same or different. Background technique [0006] Antioxidants are indispensable additives in the production and processing of high molecular polymers. Without antioxidants, polymers will be oxidatively degraded during processing and will age quickly during use. Antioxidants can not only help polymers overcome the above pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C39/16C07C37/20
Inventor 付建英
Owner SHANDONG LINYI SUNNY WEALTH CHEM CO LTD
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