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A technology of isovanillin and ethyl vanillin, applied in the chemical field, can solve the problem of low reaction activity, and achieve the effects of optimizing reaction conditions, reducing costs, and being easy to recycle.
Inactive Publication Date: 2021-07-30
浙江优创材料科技股份有限公司
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Problems solved by technology
Therefore need to provide a kind of new method for preparing isovanillin, the present invention adopts dimethyl sulfoxide as methylation reagent, because it has the advantages such as little toxicity and few side reactions concurrently, is superior to traditional methylation reagent; As a methylation reagent, dimethyl sulfoxide still has the defect of low reactivity. This project solved this problem by optimizing the catalyst and process conditions.
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Embodiment 1
[0041] (1) Add 549g ethyl vanillin, 128g dimethyl sulfoxide, 5g Pd(OAc) in the reactor 2 , 264g sodium hydroxide solution (50%), oxygen replacement 3 times, the oxygen pressure is controlled at 0.2MPa, at 100°C, react for 6h, and finish the reaction. The reaction solution was filtered and separated to obtain an oil phase intermediate: 572.05 g of the crude product of ethoxy-4-methoxybenzaldehyde, based on the amount of ethyl vanillin, the yield of the intermediate was 97%, and the purity was 99.5%.
[0042] (2) Add 728g intermediate, 150g SO in the reactor 4 2- / ZrO 2 -TiO 2 Catalyst and 1500g of water were reacted at 65°C for 3h to end the reaction. Suction filter the reaction solution, dissolve the filter cake with 2000g ethanol, heat and stir at 60°C for 2h, and suction filter; cool the filtrate to 0°C, heat and stir for 2h, and suction filter to obtain 631.23g of wet product; the obtained solid is vacuum-dried to constant weight to obtain 3- Hydroxy-4-methoxybenzalde...
Embodiment 2
[0043] Embodiment 2 (amplification experiment)
[0044] Major equipment
[0045]
[0046] (1) Add 549kg ethyl vanillin, 128kg dimethyl sulfoxide, 5kg Pd(OAc) in No. 1 reactor 2 , 264kg sodium hydroxide solution (50%), oxygen replacement 3 times, oxygen pressure is controlled at 0.2MPa, at 100 ℃, react 6h, finish reaction; Reaction liquid obtains the intermediate in oil phase through press filtration, liquid separation The crude product of ethoxy-4-methoxybenzaldehyde is 572.05g, based on the amount of ethyl vanillin.
[0047] (2) Add 728kg intermediate, 150kg SO in the reactor 4 2- / ZrO 2 -TiO 2 Catalyst, 1500kg water, react at 65°C for 3h, and finish the reaction. Pressure filter the reaction solution, dissolve the filter cake with 2000kg of ethanol, keep stirring at 60°C for 4 hours; press filter, transfer the filtrate to the crystallization kettle, cool down to 0°C, keep stirring for 4 hours; press filter to obtain 631.23kg of wet product, and transfer the filtrate...
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Abstract
The invention provides a method for synthesizing isovanillin, and belongs to the technical field of chemical engineering. The method for synthesizing isovanillin comprises the steps of (1) conducting a methylation reaction, specifically, adding ethyl vanillin, dimethyl sulfoxide, Pd (OAc) 2 and a sodium hydroxide solution into a reaction kettle, carrying out oxygen replacement, controlling the oxygen pressure at 0.2 MPa, reacting at the temperature of 100 DEG C for 6 hours, ending the reaction, and filtering and separating the reaction liquid to obtain an oil-phase intermediate; (2) conducting a hydrolysis reaction, specifically, adding the oil-phase intermediate, a SO4<2-> / ZrO<2->TiO2 catalyst and water into the reaction kettle, reacting at the temperature of 65 DEG C, and ending the reaction; carrying out suction filtration on the reaction liquid, dissolving a filter cake with 2000g of ethanol, carrying out heat preservation stirring at the temperature of 60 DEG C for 2-6 hours, and carrying out suction filtration; cooling the filtrate to 0 DEG C, preserving heat and stirring for 2-6 hours, and performing suction filtration to obtain a wet product; and drying the obtained solid in vacuum until the weight is constant to obtain the isovanillin.
Description
technical field [0001] The invention provides a method for synthesizing isovanillin, which belongs to the technical field of chemical industry. Background technique [0002] Isovanillin is used as a flavor enhancer and sweetener, as a deodorizing and flavoring agent for soap, toothpaste, rubber, plastic and other products, as an additive to cosmetics and skin care products, especially for special flavors and flavors industries. [0003] There are industrialized production reports of this product both at home and abroad, but the process routes are different: there is a process for extracting isovanillin from plants, and the process cost is too high; The raw material is the process of hydrolyzing and synthesizing isovanillin under the action of strong acid. The high cost of the raw material limits the development; some use hydroxybenzaldehyde as the raw material and synthesize it through bromination, methylation and hydrolysis or bromination, hydrolysis and oxidation reaction ...
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