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Process for recovering tert butyl hydroquinone during production of butyl hydroxy anisol

A technology of tert-butyl hydroxyanisole and tert-butyl hydroquinone, which is applied in the field of recovery of tert-butyl hydroquinone, can solve the problems of high toxicity of dimethyl sulfate, generation of by-products, and high cost, and achieve technological The effect of simple and feasible operation, short processing time and low equipment loss

Active Publication Date: 2013-03-06
WENGYUAN GUANGYE QINGYI FOOD TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In the first method, due to the higher activity of p-hydroxyanisole, a large amount of by-products are produced in the process of synthesizing BHA, the utilization rate of raw materials is not high, and separation is difficult, the cost is higher, and it is rarely used; the second In a kind of method, dimethyl sulfate is highly poisonous, and environmental pollution is bigger, and cost is higher, is unfavorable for industrial production
In the third method, using TBHQ as a raw material to produce BHA, its conversion rate and selectivity are all satisfactory, but the utilization rate of TBHQ is not 100%, and there will always be some raw materials (TBHQ) that do not participate in the reaction in the synthetic production process or by-products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Take 1000ml of the mother liquor produced after synthesizing BHA with TBHQ as raw material, distill off the solvent under reduced pressure, add 200ml of petroleum ether to dissolve the obtained oil, add 20ml of water and stir at room temperature for 15 minutes, let stand to separate and remove the water phase, and collect the organic layer; Transfer the petroleum ether solution to a 250ml three-neck flask, add 0.2g of hydrosulfite, heat and reflux for 120 minutes, concentrate and recover the solvent, add 300ml of water, heat to a slight boil and stir to dissolve, filter to remove some oily impurities, cool and crystallize to collect 11.8g of white solid, GC 98.4% of the TBHQ content was detected.

Embodiment 2

[0021] Take 1000ml of the mother liquor produced after synthesizing BHA with TBHQ as raw material, distill off the solvent under reduced pressure, add 200ml of petroleum ether to dissolve the resulting mixture, add 20ml of water and stir at room temperature for 15 minutes, let stand to separate and remove the water phase, and transfer the petroleum ether solution to In a 250ml three-neck flask, add 0.5g of zinc powder and heat to reflux for 90 minutes, concentrate and recover the solvent. Then add 300ml of water and heat to a slight boil and stir to dissolve, filter to remove some impurities, cool and crystallize the water phase to collect 11.2g of a light yellow solid, and the TBHQ content is 97.9% as detected by GC.

Embodiment 3

[0023] Take 1000ml of the mother liquor produced after synthesizing BHA with TBHQ as raw material, distill off the solvent under reduced pressure, add 200ml of petroleum ether to dissolve the resulting mixture, add 20ml of water and stir at room temperature for 15 minutes, let stand to separate and remove the water phase, and transfer the petroleum ether solution to In a 250ml three-neck flask, add 0.4 g of sodium hydrosulfite and heat to reflux for 90 minutes, then concentrate and recover the solvent. Then add 300ml of water and heat to a slight boil and stir to dissolve, filter to remove some impurities, cool and crystallize the water phase to collect 12.0g of white solid, GC detection TBHQ content 98.5%.

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PUM

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Abstract

The invention discloses a process for recovering tert butyl hydroquinone (TBHQ) during production of butyl hydroxy anisol (BHA). The process comprises the steps: concentrating mother liquid remained after producing the BHA, adding an organic solvent for dissolution, washing to remove the residual metal salt and catalyst acid, then standing to layer and remove aqueous phase, collecting an organic layer, adding a reducing agent in the organic layer to heat and stir and reflux for a period, and concentrating to remove the organic solvent to obtain the TBHQ mixer, adding a solvent in the TBHQ mixer, heating, stirring, dissolving, filtering and cooling for crystallization to obtain the TBHQ. The process has the advantages of convenient and feasible technical operation, short processing time, little loss to the device and no pollution to the environment; and the recovered TBHQ has high purity and good colour, can be directly used as the material to produce the BHA after being dried and also can be used as a food additive.

Description

technical field [0001] The invention relates to a process for recovering tert-butylhydroquinone (TBHQ) from the production process of tert-butylhydroxyanisole (BHA). Background technique [0002] tert-butylhydroquinone Chemical name: 2-tert-butylhydroquinone [0003] English name: 2-t-butyl-1, 4-dihydroxybenzene [0004] tert-butyl hydroxyanisole Chemical name 3(2)-tert-butyl-4-hydroxyanisole [0005] English name 3(2)-t-butyl-4-dihydroxyanisole [0006] Tert-butylhydroxyanisole (BHA) is a commonly used food antioxidant, it generally refers to 3-tert-butyl-4-hydroxyanisole (3-BHA) and 2-tert-butyl-4-hydroxyanisole The mixture of (2-BHA) is mainly composed of 3-tert-butyl-4-hydroxyanisole, and the content of 3-BHA is more than 98%. BHA has a wide range of applications, mainly in baked food, animal fats and feed, and has been used by most industrial countries in the world such as the United States. [0007] At present, the methods for t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/08C07C37/68
Inventor 李家林杜晨光李骅
Owner WENGYUAN GUANGYE QINGYI FOOD TECH
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