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A kind of synthetic method of butyl hydroxyanisole

A technology of butylated hydroxyanisole and a synthesis method, which are applied in chemical instruments and methods, ether preparation, ether preparation by ester reaction, etc., can solve the problems of difficult separation, high activity and high production cost, and achieve simple recovery and application, catalytic activity Stable and less reaction by-products

Active Publication Date: 2021-04-13
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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  • A kind of synthetic method of butyl hydroxyanisole
  • A kind of synthetic method of butyl hydroxyanisole
  • A kind of synthetic method of butyl hydroxyanisole

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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 butylhydroxyanisole (BHA), which uses tert-butyl hydroquinone (TBHQ) and dimethyl carbonate (DMC) as raw materials and self-made double alkali metal as a catalyst to synthesize BHA . The conversion rate of TBHQ was 28-40%, and the selectivity of the target product 3-tert-butyl-4-hydroxyanisole (3-BHA) was 84-100%. The catalyst was reused for 5 batches without any decrease in catalytic activity. The present invention has the advantages of: the self-made double alkali metal catalyst is used to catalyze the preparation of BHA with high selectivity, the catalyst can be simply filtered and reused, and the raw material dimethyl carbonate used is a green reagent that does not pollute the environment, and unreacted TBHQ and dimethyl carbonate can be directly recovered for the next reaction, with few reaction by-products, relatively mild reaction conditions, low synthesis cost, and relatively high purity 3-BHA (purity greater than or equal to 98%) can be obtained, so this method It has broad industrial 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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Patent Type & Authority Patents(China)
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