Process for producing isovitamine C by membrane-resin method

An isovitamin and resin technology, applied in the field of chemical technology, can solve the problems of interfering with crystal formation, interfering with esterification, conversion, heavy environmental protection burden of manufacturers, etc., to reduce the production of melanin-like melanin, reduce Maillard reaction, reduce The effect of depigmentation burden

Inactive Publication Date: 2007-09-05
凯能高科技工程(上海)有限公司
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Problems solved by technology

[0007] 1. Low filtration yield: due to the addition of sulfuric acid, a large amount of calcium sulfate (calcium sulfate content is about 8%) is produced, the bacteria and calcium sulfate flocs are relatively small, and the plate and frame filter cloth and filter aid will be blocked when the plate and frame are used for filtration Therefore, it is difficult to filter, and it is difficult to wash out the products entrained in the bacteria and calcium sulfate during the top washing process, so the filtration yield is low, less than 94%.
[0008] 2. The cost of using acid is high: due to the high solubility of calcium sulfate, if sulfuric acid is to be used to completely precipitate calcium ions, the sulfuric acid must be excessively large. High; on the other hand, a large amount of excess sulfate interferes with subsequent processes such as esterification and conversion
Because the pH is too low when using oxalic acid to decalcify, the oxalate in the solution is easy to form hydrogen oxalate, which reduces the removal effect of calcium ions. The amount of oxalic acid is large, and can only remove calcium ions to about 400ppm.
Due to the high price of oxalic acid, and under the current market situation, the price of oxalic acid will continue to rise, so the cost of decalcification is very high
[0009] 3. Poor quality of diketone-based gluconate solution: Diketo-based calcium gluconate fermentation broth only uses sulfuric acid and oxalic acid to precipitate calcium ions and then enters the subsequent concentration and esterification units. The diketone-based gluconate solution has not undergone any purification. The darker the color, the subsequent decolorization burden is heavier. On the other hand, there may be small floc calcium sulfate and bacteria in the filtrate that cannot be completely filtered out by the plate frame, which seriously interferes with the crystal formation during the crystallization process.
[0010] 4. Severe fouling of pipelines and evaporative concentrators: Since sulfuric acid and oxalic acid cannot completely remove calcium ions in the diketone-gluconic acid solution, the pipelines and concentrators are prone to scaling
After fouling, on the one hand, the heat transfer effect of the concentrator is poor, resulting in energy waste; on the other hand, it is easy to cause uneven heating of the feed liquid during the concentration process, resulting in local overheating
Therefore, the scale cleaning of pipelines and concentrators must be very frequent, seriously disturbing the production order, and the replacement of pipeline equipment is also relatively frequent
[0011] 5. Heavy burden on environmental protection: due to the traditional calcium salt method, a large amount of solid waste such as calcium sulfate will be generated, which cannot be treated, causing serious environmental pollution and bringing a heavy environmental burden to manufacturers

Method used

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  • Process for producing isovitamine C by membrane-resin method

Examples

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Effect test

Embodiment 1

[0038] Diketogluconate sodium mature fermentation liquid is used as raw material, stainless steel membrane is used as the sterilization filter membrane, and the operating pressure is controlled at 4-5kg / cm 2 , control the operating temperature at 35-40° C., filter the diketogluconate sodium mature fermentation broth, and obtain a clear and transparent diketogluconate sodium filtrate. Then the filtrate is treated with a hydrogen-type cation exchange resin, the operating temperature is controlled to be 5-50°C, and the liquid flow rate is controlled to be 2-4 times the volume of the resin per hour, so that the diketogluconate sodium in the filtrate is transformed into diketogluconate , to obtain an ion-exchange solution containing diketogluconic acid. Then, the ion-exchange solution is concentrated until there is no water and steamed out to obtain the diketo-D-gluconic acid of the present invention, and then esterified, transformed and refined to obtain the isovitamin C product. ...

Embodiment 2

[0040]Diketogluconate sodium mature fermentation liquid is used as raw material, ceramic membrane is used as filter membrane, and the operating pressure is controlled at 6-8kg / cm 2 , control the operating temperature at 60-80° C., filter the diketogluconate sodium mature fermentation broth, and obtain a clear and transparent diketogluconate sodium filtrate. Then the filtrate is treated with a hydrogen-type cation exchange resin, the operating temperature is controlled to be 5-50°C, and the liquid flow rate is controlled to be 4-7 times the volume of the resin per hour, so that the diketogluconate sodium in the filtrate is transformed into diketogluconate , to obtain an ion-exchange solution containing diketogluconic acid. Then, the ion-exchange solution is concentrated until there is no water and steamed out to obtain the diketo-D-gluconic acid of the present invention, and then esterified, transformed and refined to obtain the isovitamin C product.

Embodiment 3

[0042] Diketogluconate sodium mature fermentation broth is used as raw material, polyethersulfone membrane is used as filter membrane, and the operating pressure is controlled at 4-10kg / cm 2 , controlling the operating temperature to 10-50° C., filtering the diketogluconate sodium mature fermentation broth to obtain a clear and transparent diketogluconate sodium filtrate. Then the filtrate is treated with a hydrogen-type cation exchange resin, the operating temperature is controlled to be 5-50°C, and the liquid flow rate is controlled to be 6-9 times the volume of the resin per hour, so that the diketogluconate sodium in the filtrate is transformed into diketogluconate , to obtain an ion-exchange solution containing diketogluconic acid. Then, the ion-exchange solution is concentrated until there is no water and steamed out to obtain the diketo-D-gluconic acid of the present invention, and then esterified, transformed and refined to obtain the isovitamin C product.

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Abstract

A process for preparing isovitamin C by membrane-resin method includes such steps as membrane filtering of the fermented liquid of sodium diketogluconate, ion exchange and concentrating by ion exchange resin, esterifying, converting and refining.

Description

technical field [0001] The invention relates to a chemical process, in particular to a process for producing isovitamin C by extracting diketo-D-gluconic acid from fermentation broth by using a membrane-resin method. Background technique [0002] Sodium isovitamin C is a very safe antioxidant widely used in food processing. Diketo-D-gluconic acid is an important precursor for the production of isovitamin C sodium. Diketo-D-gluconic acid is esterified with methanol and then converted with sodium methoxide to obtain isovitamin C sodium. [0003] Currently, diketo-D-gluconic acid is produced by fermentation. During the fermentation process, with the accumulation of diketo-D-gluconic acid, the pH of the fermentation broth decreased. In order to prevent the fermentation liquid from reducing the pH and inhibit the growth of bacteria, a certain amount of alkaline substances must be added as a neutralizing agent during the fermentation process to inhibit the reduction of pH. Neut...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/62
Inventor 申雅维曹建勇刘峰葛文越林爱莲
Owner 凯能高科技工程(上海)有限公司
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