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Method for synthesizing butyl hydroxy anisd

A technology for butyl hydroxyanisole and a synthetic method, which is applied in chemical instruments and methods, preparation of ether, preparation of ether by ester reaction, etc., can solve problems such as high production cost, high activity, and difficult separation, and achieve less reaction by-products, The effect of stable catalytic activity and simple recycling

Active Publication Date: 2018-07-24
BROTHER ENTERPRISES HLDG CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the first method, p-hydroxyanisole has high activity and is prone to electrophilic substitution reaction. During the reaction, a large number of by-products are generated and separation is difficult.
In the second method, dimethyl sulfate is a high-risk, highly toxic, and highly corrosive reagent, which requires a large investment in equipment and high production costs, which is not conducive to industrial production
In the third method, the conversion rate and selectivity of the product are better, and the purification is simple, but the steps are cumbersome, requiring multiple extractions and recrystallization

Method used

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  • Method for synthesizing butyl hydroxy anisd

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Experimental program
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Effect test

Embodiment 1-4

[0023] The preparation of bimetallic basic catalyst: configure the magnesium sulfate solution of 10% mass concentration, then add the nitrate solution of the second basic metal M (M=Ca, Ba, Sr or La) of 5% mass concentration, make element Mg The molar ratio to M is 1:2, and the selection of the second basic metal M is shown in Table 1. After stirring evenly, slowly add 10 times the volume of the precipitant potassium carbonate solution with a mass concentration of 2%, and keep stirring. After the precipitation is complete, filter, wash the precipitate repeatedly with double distilled water, dry at 120° C., and then calcinate at 750° C. in a muffle furnace for 15 hours. The MgO-MO obtained after calcination was pulverized and soaked overnight in 1% K and Na nitrate solution, so that the alkali metal components of K and Na in the catalyst accounted for the total content of the double alkali metal oxide MgO-MO 10mol%, the molar ratio of K and Na is 1:1. Stir and evaporate to pas...

Embodiment 5-8

[0028] Preparation of bimetallic basic catalyst: configure magnesium sulfate solution with 10% mass concentration, and then add calcium nitrate solution with 5% mass concentration, so that the molar ratio of elements Mg and Ca is within the range of 1:0.5-9, Mg / Ca The ratio is as shown in Table 2, and slowly adding 10 times the mass concentration of the volume after stirring is the precipitating agent potassium carbonate solution of 2%, and constantly stirring. After the precipitation is complete, filter, wash the precipitate repeatedly with double distilled water, dry at 120° C., and then calcinate at 750° C. in a muffle furnace for 15 hours. The MgO-MO obtained after calcination was pulverized and soaked overnight in 1% K and Na nitrate solution, so that the alkali metal components of K and Na in the catalyst accounted for the total content of the double alkali metal oxide MgO-MO 10mol%, the molar ratio of K and Na is 1:1. Stir and evaporate to paste at 100°C, dry, extrude,...

Embodiment 9-12

[0033] Preparation of bimetallic basic catalyst: configure 10% mass concentration of magnesium sulfate solution, then add 5% mass concentration of calcium nitrate solution, so that the molar ratio of elements Mg and Ca is 1:1, stir well and slowly add 10 times the volume The mass concentration is 2% precipitant potassium carbonate solution, and keep stirring. After the precipitation is complete, filter, wash the precipitate repeatedly with double distilled water, dry at 120° C., and then calcinate at 750° C. in a muffle furnace for 15 hours. The MgO-MO obtained after calcination was pulverized, and soaked in 1% K and Na sulfate, nitrate, chloride, hydroxide solution (as shown in Table 3) overnight, so that K and Na in the catalyst The alkali metal component accounts for 10 mol% of the total content of the double alkali metal oxide MgO-MO, and the molar ratio of K and Na is 1:1. Stir and evaporate to paste at 100°C, dry, extrude, calcined at 700°C for 12 hours, crush to 60 mes...

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Abstract

The invention discloses a method for synthesizing butyl hydroxy anisd (BHA). The BHA is synthesized by taking tert-Butylhydroquinone (TBHQ) and dimethyl carbonate (DMC) as raw materials and taking self-made double alkali metals as catalysts. The conversion ratio of the TBHQ is 28-40%, the selectivity of the produced target product 3-tert-butyl-4-hydroxy anisole (3-BHA) is 84-100%, and when the catalyst is repeatedly used in five batches, the catalytic activity is not reduced. The method disclosed by the invention has the advantages that the BHA prepared by catalysis of the self-made double alkali metal catalyst is high in selectivity, the catalyst can be simply filtered and repeatedly used, and the used raw material dimethyl carbonate is a green reagent without any environmental pollution.Moreover, the unreacted TBHQ and dimethyl carbonate can be directly recycled for the next reaction, the amount of reaction by-products is small, the reaction conditions are relatively mild, the synthesizing cost is low, and the 3-BHA with relatively high purity (purity of being greater than or equal to 98%) can be obtained. Therefore, the method has wide industrialized application prospects.

Description

technical field [0001] The invention relates to the technical field of synthesis of fat-soluble antioxidants in the fields of edible oils and oils, fried foods, dried fish products, etc., and in particular to a method for synthesizing butyl hydroxyanisole (BHA). Background technique [0002] Butylated hydroxyanisole (BHA) is a good antioxidant, widely used in edible oils, dried fish products, biscuits, cured meat products and other fields, can delay the oxidative deterioration of meat products, improve the quality of cheese, milk powder, baked food shelf life. As a fat-soluble antioxidant, it has better thermal stability, and it has better synergistic effect when mixed with other fat-soluble antioxidants. [0003] Butylated hydroxyanisole has two isomers, namely 3-tert-butyl-4-hydroxyanisole (3-BHA) and 2-tert-butyl-4-hydroxyanisole (2-BHA), in which 3- The antioxidant effect of BHA is 1.5 to 2 times that of 2-BHA. Commercially available BHA is generally a mixture of the ...

Claims

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Application Information

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IPC IPC(8): C07C41/16C07C43/23B01J23/04B01J23/10
CPCB01J23/04B01J23/10C07C41/16C07C43/23
Inventor 周中平张秋华吴小乐朱宇翔
Owner BROTHER ENTERPRISES HLDG CO LTD
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