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Sulfonated vinegar grains, its preparation method and application

A technology for sulfonating vinegar grains and vinegar grains, which is applied to the sulfonation method and the product field prepared by the method, can solve the problems such as the inability of rational application of vinegar grain waste residue, environmental pollution and the like, and achieves the realization of recycling and reusing technology. The process is simple and easy, and the synthesis rate is fast.

Active Publication Date: 2018-07-24
LULIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] To sum up, in order to solve the problem that vinegar residues cannot be used rationally and cause environmental pollution due to long-term stacking, the present invention has developed a method for sulfonating vinegar residues to expand its utilization channels and improve utilization rates. And utilize the product that this method makes to be used for the synthesis of catalysis hydantoin

Method used

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  • Sulfonated vinegar grains, its preparation method and application
  • Sulfonated vinegar grains, its preparation method and application
  • Sulfonated vinegar grains, its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Example 1 Preparation of sulfonated vinegar grains with sulfuric acid as sulfonating agent, the steps are:

[0042] (1) The natural vinegar lees left after the fermentation of aspergillus, yeast, and acetobacter in the solid state are made into vinegar in a solid state, air-dried naturally, and then crushed with a stone mill to a particle size range of 160-180 mesh, and the particles are collected by sieving Graded components, fully rinsed with water to remove free acetic acid, dried, kept the material quality to constant weight, terminated drying, and sampled and analyzed after cooling to calculate the accurate acid value of the solid vinegar grains;

[0043] (2) Accurately weigh 500 g of graded vinegar grains (acid value 0.082 mmol / g) and a certain amount of sulfonating agent. Then add 1 % accelerator (anhydrous aluminum chloride, w / w), spray water (water content 40%, w / w), mix well, put the mixed material into a volatilization porcelain crucible, Close the lid, wrap...

Embodiment 2

[0044] Example 2 Using sodium sulfite as a sulfonating agent to prepare sulfonated vinegar grains, the steps are:

[0045] (1) Same as embodiment 1;

[0046] (2) Accurately weigh 500 g of graded vinegar grains (acid value 0.082 mmol / g) and a certain amount of sulfonating agent. Then add 1 % accelerator (anhydrous ferric chloride, w / w), spray water (water content 40%, w / w), mix well, put the mixed material into a volatilization porcelain crucible, Close the lid, wrap the crucible with red mud, bake in an oven at 150 ºC for 5 hours, stop heating and cool down; wash the sample with distilled water until the pH of the filtrate reaches 7, collect the filtrate, dry the solid sulfonated vinegar grains, and obtain the final product.

Embodiment 3

[0047] Example 3 Prepare sulfonated vinegar grains with sodium sulfamate as sulfonating agent, the steps are:

[0048] (1) Same as embodiment 1;

[0049] (2) Accurately weigh 500 g of graded vinegar grains (acid value 0.082 mmol / g) and a certain amount of sulfonating agent. Then add 1 % accelerator (anhydrous aluminum chloride, w / w), spray water (water content 40%, w / w), mix well, put the mixed material into a volatilization porcelain crucible, Close the lid, wrap the crucible with red mud, put it in an oven at 150 ºC for 5 h, stop heating and cool down; wash the sample with distilled water, and dry it at 60 ºC for 30 min.

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Abstract

The invention discloses sulfonated vinegar residue, its preparation method and application, and belongs to the fields of chemical industry and pharmaceutical production. A kind of sulfonated vinegar residue is made by mixing vinegar residue and sulfonating agent and baking it by wet method. The particle size is about 170-190 mesh. The amount of sulfonic acid group in every gram of vinegar residue is 41.382-53.298 mg. The specific surface area It is 2.3864-2.5417 m2 / g, and the pore diameter is 0.3±0.04μm. The invention adopts wet baking technology to achieve efficient sulfonation of vinegar residue, with less pollutant discharge, low cost, high sulfonation efficiency, high activity of the sulfonated vinegar residue catalyst and long service life.

Description

technical field [0001] The invention belongs to the fields of chemical and pharmaceutical production, and relates to a method for sulfonating vinegar grains, a product prepared by the method, and an application of the product. Background technique [0002] Vinegar is made from starchy raw materials through three processes of starch saccharification, alcohol fermentation and acetic acid fermentation under the fermentation of microorganisms Aspergillus, yeast and Acetobacter. Since 2005, my country's annual output of vinegar has reached 2-2.5 million tons (calculated at 3.5% HAc), and it has grown at a rate of 7% year by year. Vinegar grains are the solid waste residues left in the process of solid-state fermentation and brewing vinegar with grain as the main raw material. For every ton of standard solid-state fermented secondary vinegar produced, 600-700 kg of vinegar grains are produced, which is the annual output of vinegar grains It can reach 1.20-1.75 million tons (calcu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02B01J35/10C07D233/74C07D233/78
CPCC07D233/74C07D233/78B01J31/0225B01J35/40B01J35/612B01J35/651
Inventor 乔元彪苏彬林李文姣李艳芳秦文浩王元宋尧
Owner LULIANG UNIV
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