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Method for preparing 4,4'-butylidene bis(6-tert-butyl m-cresol) through one-pot process

A technology of cresol and methanol, which is applied in the field of one-pot preparation 4, can solve problems such as neutralization product pollution, achieve great economic benefits, green and environmental protection industrial application, and reduce the cost of pollution control

Active Publication Date: 2018-09-28
淄博万科化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] The object of the present invention is to provide a kind of method for preparing 4,4'-butylene bis(6-tert-butyl m-cresol) in one pot method, which is used to solve the problem that a large amount of acid water needs to be neutralized in the production process. The method avoids the use of a large amount of lye, and at the same time avoids the pollution of neutralized products caused by the use of lye

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] In the 1000 milliliter four-neck flask with reflux device, stirrer, add 111 grams of 6-tert-butyl m-cresol, 100 milliliters of methyl alcohol and 30 grams of concentrated hydrochloric acid (massfraction 36%), under stirring, heat material temperature to At 40°C, add 10ml of methanol and 24g of n-butyraldehyde mixture slowly with a normal pressure burette for 60 minutes, then keep the material under 75±3°C under methanol reflux for 4 hours, add 200# petroleum aromatic Hydrocarbon solvent oil 500 ml, heat preservation and stirring to make the material completely dissolve at 73±2°C, stop stirring, and use the method of changing bottles to separate 73 ml of acid water after standing for stratification, and use ammonia water reagent 1.5 The milliliter was neutralized to neutral, and no aqueous phase was found after standing. Stir the organic phase and heat up to evaporate methanol and other volatiles. When the temperature of the material rises to 100 ° C, stop, distill 41 ml...

Embodiment 2

[0033]The present embodiment is the same as Example 1, except that, in a 1000 milliliter four-necked flask with a reflux device and a stirrer, add 111 grams of 6-tert-butyl m-cresol and the sour water separated in Example 1 73 ml, and then add 5 g of concentrated hydrochloric acid (mass fraction 36%) and 40 ml of methanol. After separating acid water in addition, add 700 milliliters of aromatic hydrocarbon solvent naphtha mother liquors produced in embodiment 1. Results: The product weighed 95 grams, the yield was 73.6%, the dissolution range: 209.8-210.8°C, and the light transmittance (425, 500): 95.8, 97.0.

Embodiment 3

[0035] With reflux device, in the 1000 milliliters of four-neck flasks of stirrer, add 111 gram 6-tert-butyl m-cresols, 70 milliliters of sour waters that separate in example 2, add 5 grams of concentrated hydrochloric acid (massfraction 36% again) ) and 30 milliliters after phase separation of the methanol liquid steamed out in Example 2. Other operations are the same as in Example 2, the result: the product weighs 87.5 grams, the yield is 67.8%, the dissolution range: 208.1-209.1° C., and the light transmittance (425, 500): 94.7, 97.1.

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Abstract

The invention relates to a method for preparing 4,4'-butylidene bis(6-tert-butyl m-cresol) through a one-pot process. In the method for preparing the 4,4'-butylidene bis(6-tert-butyl m-cresol) by using 6-tert-butyl m-cresol and n-butyraldehyde as raw materials, methanol as a solvent and hydrochloric acid as a catalyst, an aromatic hydrocarbon solvent is added after a condensation reaction is completed, and a reaction mixture is completely dissolved and layered at a reflux temperature of the methanol through a mixed solvent composed of a methanol solvent and the aromatic hydrocarbon solvent, wherein an acid water layer is separated; an organic layer is heated to evaporate remaining methanol; and a crystallized product is obtained through after-treatment. The method provided by the inventionsolves the problem that a large amount of acid water needs to be neutralized in the production process, avoids the use of a large amount of an alkali liquid, and avoids the problem of pollution to aneutralized product due to the use of the alkali liquid. The process of acid-water separation facilitates improving the melting point and light transmittance indexes of a product, and separated acid water can be partially or completely reused, so the cost of pollution treatment is reduced.

Description

technical field [0001] The invention relates to a method for preparing 4,4'-butylene bis(6-tert-butyl m-cresol) in one pot, and belongs to the technical field of antioxidant production for polyolefins and rubbers. Background technique [0002] 4,4'-butylene bis(6-tert-butyl m-cresol) is used as an antioxidant for polyolefin and rubber, and its preparation method is to use 6-tert-butyl m-cresol and n-butyraldehyde under the condition of acid catalyst Prepared by following reaction. The acid used is an inorganic acid or an organic acid, such as hydrochloric acid, and the amount of the acid used is particularly large. [0003] In US 2970151, hydrochloric acid is used as a catalyst to generate 4,4'-butylene bis(6-tert-butyl m-cresol). After the reaction is completed, the volatile matter is evaporated to remove the acid, then benzene is added, and the excess is washed with water. acid. In Example 2, heptane is added after the reaction is completed, and then the product is filt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/20C07C37/68C07C37/72C07C39/16
CPCC07C37/20C07C37/685C07C37/72C07C39/16
Inventor 王文举朱永国张青郝仲华崔华松张胜传
Owner 淄博万科化工有限公司
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