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High polysaccharide derivatives derived from vinegar grains and their preparation methods and applications

A technology of high polysaccharides and new structure, applied in chemical instruments and methods, chemical/physical processes, physical/chemical process catalysts, etc., can solve the problems of difficult catalyst recycling, increased phenytoin production cost, complicated product separation process, etc. , to achieve the effect of superior catalyst performance, easy long-term reuse, and simple recovery process

Active Publication Date: 2021-06-01
LULIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of the allantoin reaction method is that it uses a strong acid catalyst, which easily causes serious corrosion effects on the reaction equipment, and produces a large amount of waste water in the later stage of phenytoin concentration and crystallization process, making it difficult to recycle the catalyst.
In addition, strong alkali solution of sodium hydroxide with a concentration of about 30% can also catalyze the reaction of urea with 1,2-diphenylethanedione to produce phenytoin. There are many product components, the product separation process is complex, and acidification and desalination steps are required
It is estimated that the strong base catalyzed process increases the production cost of phenytoin by more than 30%. Due to the use of ethanol system, it is easy to remain in phenytoin products and stimulate the central nervous system

Method used

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  • High polysaccharide derivatives derived from vinegar grains and their preparation methods and applications
  • High polysaccharide derivatives derived from vinegar grains and their preparation methods and applications
  • High polysaccharide derivatives derived from vinegar grains and their preparation methods and applications

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Example 1 Preparation of new structural derivatives of high polysaccharides derived from vinegar grains by step-by-step reaction method

[0045] A method for preparing high polysaccharide derivatives with new structures derived from acetic acid grains, the specific steps of which are as follows:

[0046] (1) Mix 50 grams of vinegar grains powder and 50 grams of sodium periodate, use 40 ml of deionized water to wet the mixture by spraying method, stir evenly and put it into a volatile porcelain crucible, and wrap the crucible with red mud after sealing , bake at 50±3°C for 8±0.5 hours, then stop heating, take out the reaction material, cool for 30 minutes, transfer to a 250ml Buchner funnel, rinse with deionized water repeatedly, and suction filter until there is no As far as the oxidant is concerned, the filtrate is collected. The collected filtrate contains the reaction product sodium iodate and the remaining sodium periodate after the reaction, which is used as a samp...

Embodiment 2

[0049] Example 2 Preparation of new structural derivatives of high polysaccharides derived from vinegar grains by step-by-step reaction method

[0050] A method for preparing high polysaccharide derivatives with new structures derived from acetic acid grains, the specific steps of which are as follows:

[0051](1) Mix 50 grams of vinegar grain powder and 100 grams of sodium periodate, use 60 milliliters of deionized water, use the spray method to wet the mixed material, stir evenly, put it into a volatile porcelain crucible, and wrap the crucible with red mud after sealing , bake at 50±3°C for 8±0.5 hours, then stop heating, take out the reaction material, cool for 30 minutes, transfer to a 250ml Buchner funnel, rinse with deionized water repeatedly, and suction filter until there is no As far as the oxidizing agent is concerned, the filtrate is collected. The collected filtrate contains the reaction product sodium iodate and the remaining sodium periodate after the reaction. ...

Embodiment 3

[0054] Example 3 Preparation of new structural derivatives of high polysaccharides derived from vinegar grains by step-by-step reaction method

[0055] A method for preparing high polysaccharide derivatives with new structures derived from acetic acid grains, the specific steps of which are as follows:

[0056] (1) Mix 50 grams of vinegar grains powder and 75 grams of sodium periodate, use 50 milliliters of deionized water to wet the mixture by spraying method, stir evenly and put it into a volatile porcelain crucible, and wrap the crucible with red mud after sealing , baked at 50±3°C for 5±0.5 hours, then stopped heating, took out the reaction material, cooled for 30 minutes, transferred to a 250ml Buchner funnel, repeatedly rinsed with deionized water, and suction filtered until the filtrate was free of As far as the oxidizing agent is concerned, the filtrate is collected. The collected filtrate contains the reaction product sodium iodate and the remaining sodium periodate a...

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Abstract

The invention discloses a new structure derivative of high polysaccharide derived from vinegar grains and its preparation method and application. Fresh vinegar grains, sodium periodate, benzenesulfonic acid or p-toluenesulfonic acid produced after aged vinegar brewing are used as initial materials , the oxidizing agent at the specific site of the phenolic or D-pyran ring structural unit in the polysaccharide, and the raw material of the sulfonating agent, the oxidation-sulfonation reaction is carried out by a step-by-step reaction method or a "chemical cascade coupling" method, and the The new structure derivatives of high polysaccharides derived from vinegar grains are obtained by reaction under slight heat and wet roasting; then the new structure derivatives of high polysaccharides derived from vinegar grains are used as catalysts to catalyze the condensation reaction of diphenylglycolic acid and urea to prepare Phenytoin. The new structure derivative of high polysaccharides derived from vinegar grains of the present invention has simple preparation and high reaction efficiency, the degree of sulfonation (calculated based on the sulfonic acid groups in vinegar grains) is 101.1-156.6 mg / g, and the specific activity of the catalyst reaches 2607.76-3096.89 Micromol / g·hour, the catalyst life is 96 hours (residual activity ≥ 70%), and the catalyst can be regenerated and reused.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and pharmacy, and relates to a new structural derivative of high polysaccharides derived from vinegar grains, in particular to a new structural derivative of oxidation-sulfonation of high polysaccharide components derived from vinegar grains, a preparation method and an application. Background technique [0002] Mature vinegar ranks first among the four famous vinegars in China and is a product of China's National Geographical Indication. The brewing technique of mature vinegar was awarded the first batch of national intangible cultural heritage. It adopts the secondary fermentation process of all-solid-state, lactic acid bacteria and acetic acid bacteria. It uses sorghum, bran, rice bran and water as the main raw materials, and is made from barley and peas. Hongxin Daqu is a high-quality saccharification starter, which is made into vinegar after starch saccharification, alcohol fermenta...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/10C07D233/74
CPCB01J31/10C07D233/74Y02P20/584
Inventor 乔元彪霍宇平李越徐寅生王晓伟胡雪梅
Owner LULIANG UNIV