A kind of preparation method of methylselenoglucose and selenium carbon
A technology of glucose and methyl selenium, applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of affecting the effect, increasing the reaction cost, increasing the labor cost, etc.
Active Publication Date: 2022-07-08
扬州帮杰新材料有限公司
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Problems solved by technology
The biggest problem is that the prepared selenoglucose is not stable, it is easily oxidized and discolored by air in aqueous solution, and decomposes rapidly, thus affecting its effect (see Ind. Eng. Chem. Res. 2020 , 59, 10763 articles figure 1 )
The selenium-enriched foliar fertilizer developed on the basis of this technology needs to be used quickly after the aqueous solution is prepared, and it is difficult to spread it with many pesticides at the same time, and it needs to be fertilized separately, which increases labor costs
Method used
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[0017] 1. Preparation of methylselenoglucose:
[0018] 1. Take 1.42 g (18 mmol) of selenium powder and a magnetic stirrer into a 250 mL three-necked flask, evacuate the nitrogen for 3 to 4 times, and place it in an ice-water bath.
[0019] 2. Under stirring, slowly inject methylmagnesium bromide (1 mol / L, 20 mL, containing 20 mmol of methylmagnesium bromide) into the above three-necked flask with a syringe, stir and react for 1 h, remove the ice-water bath, and continue the reaction at room temperature 1 hour, get methyl selenide magnesium.
[0020] 3. Add 16.2 g (90 mmol) of glucose powder to the above three-necked bottle in three additions, and continue to add the glucose powder after the last addition of glucose powder and stir evenly.
[0021] 4. Seal the three-necked flask, heat the reaction at 50 °C for 4 hours, turn off the heating and continue stirring, then add 30 mL of anhydrous ether or tetrahydrofuran and stir at room temperature for 12 hours, and then use a rotar...
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A preparation method of methylselenoglucose and selenium carbon belongs to the technical field of material production. The glucose and methylselenomagnesium are mixed and reacted in a solvent, and the solvent is evaporated to dryness to obtain methylselenoglucose; after the methylselenoglucose and potassium bromide are mixed and ground, placed in a nitrogen atmosphere for calcination, and after cooling to room temperature After regrinding, washing with deionized water, centrifugation, precipitation, and drying to obtain selenium carbon. In the invention, cheap and easily available glucose is used as the main material, and methylselenoglucose with better stability is prepared by reacting with magnesium methylselenide and then evaporating the solvent to dryness. In methylselenoglucose, the introduction of methyl makes the selenium functional group more stable and difficult to be oxidized and decomposed, which is more practical as a foliar selenium fertilizer. And on this basis, selenium carbon with higher catalytic activity is prepared and obtained, which is used to catalyze the oxidation of β-ionone by molecular oxygen to synthesize useful epoxides.
Description
technical field [0001] The invention belongs to the technical field of material production. Background technique [0002] The development of selenium-containing materials using sugar as a carrier has the advantages of cheap, readily available, and biocompatible materials. The inventor's research group has conducted long-term research on this, and developed selenoglucose, which can be used to prepare selenium-carbon catalyst materials by further calcination ( Catal. Sci. Technol. , 2018, 8 , 5017), the related technology has been protected by authorized invention patents (such as a method for synthesizing nano-selenium materials disclosed in ZL201610899676.8), and selenoglucose has achieved kilogram production ( Ind. Eng. Chem. Res. 2020 , 59, 10763), and is widely used as a selenium-enriched foliar fertilizer. [0003] However, there are some problems with the prior art. The biggest problem is that the prepared selenoglucose is not stable, and is easily oxidized and di...
Claims
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IPC IPC(8): C07H1/00C07H1/06C07H5/08B01J27/057C07D303/32C07D301/04C05D9/02
CPCC07H1/00C07H1/06C07H5/08B01J27/0573C07D303/32C07D301/04C05D9/02Y02E60/10
Inventor 俞磊李培梓李韬王琪远左示敏
Owner 扬州帮杰新材料有限公司