Preparation method of carboxymethyl levan and applications thereof

A technology for carboxymethyl levan and levan, which is applied in the field of preparation of carboxymethyl levan, can solve the problems of low degree of substitution of carboxymethyl inulin, inhibiting scale inhibition effect and the like, and achieves the inhibition of calcium salts. the deposition of calcium salts, or to prevent the deposition of calcium salts, the effect of mild reaction conditions

Inactive Publication Date: 2013-02-27
天津实发中科百奥工业生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method for preparing carboxymethyl inulin disclosed in Chinese Patent Application Publication No. CN101602817A uses isopropanol as a solvent, but the degree of substitution of the prepared carboxymethyl inulin is not high, which will inhibit its scale inhibition effect

Method used

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  • Preparation method of carboxymethyl levan and applications thereof
  • Preparation method of carboxymethyl levan and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of carboxymethyl levan: first weigh 3.24g levan, add 50ml of isopropanol to a reaction vessel (such as a three-neck flask), fix the flask under the stirrer, and add levan while stirring slowly. Then transfer the flask to a water bath, control the temperature of the water bath to 35°C, add 2g of solid sodium hydroxide to the mixture in batches, and stir for 30min; weigh 1.89g of monochloroacetic acid solid, put it into a 25ml beaker, and add 10ml With isopropanol, stir until monochloroacetic acid is completely dissolved, then adjust the reaction temperature to 50°C, add monochloroacetic acid isopropanol solution while stirring, and wait until the monochloroacetic acid solution is added gradually, then stir and react in a water bath at constant temperature for 3 hours. After the reaction, the reaction product was poured into a beaker, allowed to stand for precipitation, then poured off the supernatant, and the precipitation was washed 4 times with alcohol solut...

Embodiment 2

[0032] The difference from Example 1 is: take 3.24g of levan, add 60ml isopropanol in a three-necked flask, fix the flask under the stirrer, add levan while stirring slowly, then transfer the flask to a water bath In the pot, control the temperature of the water bath to 35°C, add 3.2g solid sodium hydroxide to the mixture in batches, and stir for 60 minutes; weigh 3.78g solid monochloroacetic acid, put it into a 50ml beaker, add 30ml isopropanol, and stir Until the monochloroacetic acid is completely dissolved, keep the reaction temperature at 35°C, and gradually add the monochloroacetic acid isopropanol solution while stirring. After the monochloroacetic acid solution is gradually added, stir and react in a water bath at constant temperature for 5 hours. After the reaction, pour the reaction product into a beaker, let it stand for precipitation, pour off the supernatant, and wash the precipitation 5 times with alcohol solution. The product was dried in an oven at 70°C for 3 h...

Embodiment 3

[0035] The difference from Example 1 is: take 3.24g of levan, add 50.5ml isopropanol solution in the three-necked flask, fix the flask under the stirrer, add levan while stirring slowly, then transfer the flask Put into a water bath, add 0.8g of sodium hydroxide solid to the mixed solution in batches at room temperature, and stir for 15 minutes; weigh 0.945g of monochloroacetic acid solid, put it into a 25ml beaker, add 9.5ml of isopropanol, and stir until The monochloroacetic acid was completely dissolved, and then the reaction temperature was adjusted to 80°C, and the isopropanol solution of monochloroacetic acid was gradually added while stirring. After the progressive addition of the monochloroacetic acid solution was completed, the reaction was stirred and reacted in a water bath at constant temperature for 1 hour. After the reaction, pour the reaction product into a beaker, let it stand for precipitation, pour off the supernatant, and wash the precipitation with alcohol s...

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Abstract

The invention relates to a preparation method of carboxymethyl levan, namely levan is subjected to carboxymethyl modification by adopting sodium hydroxide and chloroacetic acid as reaction system, and an organic solvent as a reaction medium. The implementation steps are as follows: weighing levan; adding the organic solvent in a reaction vessel, adding levan while stirring, and controlling the water bath temperature at 25-50 DEG C; then adding sodium hydroxide solids in batches in a mixed solution, wherein the alkalization time is 15-60 minutes; then adding a chloroacetic acid solution in which the organic solvent is dissolved; regulating the reaction temperature to be 35-80 DEG C; stirring and reacting for 1-5 hours at the water bath constant temperature when the chloroacetic acid solution is progressively increased completely; standing and precipitating a reaction product after the reaction; removing a liquid supernatant; and washing the precipitates by alcohol, thus yellowish or yellow carboxymethyl levan products are obtained through vacuum frozen drying or oven drying. According to the invention, the preparation technology is simple, the reaction condition is moderate, the degree of substitution of carboxymethyl levan is high, and the carboxymethyl levan can be applied to the field of water treatment as a novel environmentally-friendly antisludging agent.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals, and in particular relates to a preparation method and application of carboxymethyl levan. Background technique [0002] The formation of calcium carbonate precipitates is a problem in many fields such as kettles, heaters, seawater desalters, oil and gas products, laundry and many others. When the temperature of the water rises, the solubility of calcium carbonate decreases, resulting in precipitation or large-area crystallization of calcium carbonate that is difficult to remove on the product or equipment, resulting in a decline in production efficiency and an increase in production costs. Most of the currently widely used scale inhibitors are not biodegradable, and their accumulation in the environment will cause harm to the environment. Therefore, the concept of green scale inhibitors with high scale inhibitory activity, good biodegradability, non-toxic or low toxicity has been proposed ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B37/00C02F5/10
Inventor 杨坤徐勇虎李睿颖国华胡娅君刘云王永乐王珺
Owner 天津实发中科百奥工业生物技术有限公司
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