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Method for extracting theophylline sodium salt or theophylline by styrene type macroporous resin

A technology for theophylline sodium salt and theophylline, which is applied in the field of extraction of theophylline sodium salt or theophylline, which can solve the problems of loss of octanol and other organic solvents, high recovery costs, loss of target isolates, etc., to enhance competitiveness , Adapt to large-scale production and reduce extraction costs

Active Publication Date: 2012-02-08
SUNRESIN NEW METERIALS CO LTD XIAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] This method requires the use of organic solvents such as octanol as extractants. These extractants are volatile and have certain toxicity. At the same time, organic solvents such as octanol have certain solubility in the water phase, and a part of octanol and theophylline remain in the raffinate. , resulting in loss of target isolate
Therefore, in the process of operation, it will not only cause certain air and water pollution, loss of organic solvents such as octanol, but also cause loss of theophylline, and the recovery cost remains high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A manufacturer produces the mother liquor of theophylline sodium salt, and the content of theophylline sodium salt in the mother liquor is 0.8%. Add 4% hydrochloric acid to adjust the pH to pH 5.0, and filter out the suspended impurities in the mother liquor. In a stainless steel resin column with a diameter of 200 mm and a height of 2000 mm, 50 L of LX-18M styrene type macroporous adsorption resin produced by Xi'an Lanxiao Technology Co., Ltd. was loaded. The mother liquor from which impurities are filtered out is passed through the resin column at a flow rate of 50-100L / h, and a total of 600L of mother liquor is passed through. Use 4% NaOH solution to desorb the resin, the flow rate is 25L / h, and the dosage is 50L. Recover 50 L of the desorption solution, add 32% NaOH solution to adjust the pH value to pH 14, then let it stand, centrifuge, and dry to obtain 4.5 kg of theophylline sodium salt crude product with a content of 92.0%.

Embodiment 2

[0038] A manufacturer produces mother liquor of theophylline, the content of theophylline in the mother liquor is 1.0%. Add sulfuric acid with a concentration of 3%, adjust the pH value to pH4.8, and filter out the suspended impurities in the mother liquor. In a stainless steel resin column with a diameter of 200 mm and a height of 2000 mm, 50 L of LX-18M styrene type macroporous adsorption resin produced by Xi'an Lanxiao Technology Co., Ltd. was loaded. The mother liquor from which impurities are filtered out is passed through the resin column at a flow rate of 100-200L / h, and a total of 500L of mother liquor is passed through. Use 6% KOH solution to desorb the resin, the flow rate is 30L / h, and the dosage is 50L. Recover 50 L of the desorption solution, add 30% sulfuric acid solution to adjust the pH value to pH = 5.0, then let it stand, centrifuge, and dry to obtain 4.8 kg of theophylline crude product with a content of 91.0%.

Embodiment 3

[0040] A manufacturer produces the mother liquor of theophylline sodium salt, and the content of theophylline sodium salt in the mother liquor is 0.2%. Add citric acid with a concentration of 4%, adjust the pH value to pH6, and filter out the suspended impurities in the mother liquor. In a stainless steel resin column with a diameter of 200 mm and a height of 2000 mm, 50 L of LX-20 styrene-type macroporous adsorption resin produced by Xi'an Lanxiao Technology Co., Ltd. was loaded. The mother liquor from which impurities are filtered out is passed through the resin column at a flow rate of 200-300L / h, and a total of 900L of mother liquor is passed through. Use 30% KOH solution to desorb the resin, the flow rate is 5L / h, and the dosage is 20L. Recover 20 L of the desorption solution, add 20% citric acid solution to adjust the pH value to pH 11, then let it stand, centrifuge, and dry to obtain 1.5 kg of crude theophylline sodium salt with a content of 86.0%.

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PUM

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Abstract

The invention discloses a method for extracting theophylline sodium salt or theophylline from a theophylline sodium salt or theophylline mother solution by a styrene type macroporous resin adsorption method, which comprises the following steps: (1) regulating the pH value of the theophylline sodium salt or theophylline mother solution; (2) filtering the mother solution and removing suspended impurities in the mother solution; (3) adsorbing the mother solution by adsorption resin; (4) desorbing the adsorption resin after adsorption saturation by a desorbing agent to obtain a desorption solution; (5) regulating the pH value of the desorption solution, standing and crystallizing theophylline sodium salt or theophylline; (6) centrifugally filtering; and (7) drying to obtain solid theophylline sodium salt. The method provided by the invention has the advantages that the theophylline sodium salt or theophylline crude product has better quality, the operation safety is better, the extraction efficiency is higher, the extraction cost is low, and the method is more suitable for mass production and facilitates realizing automatic operation. With the method disclosed by the invention, the extraction cost of the theophylline sodium salt and theophylline can be reduced, the extraction yield of the theophylline sodium salt and theophylline is increased, and the competitiveness of enterprises is enhanced.

Description

technical field [0001] The present invention relates to a method for extracting theophylline sodium salt or theophylline, in particular to a method for extracting theophylline sodium salt or theophylline from theophylline sodium salt or theophylline mother liquor by using a styrene-type macroporous resin adsorption method, which belongs to The method of separating organic matter from organic synthesis chemical mother liquor is also a kind of chemical environmental protection technology. Background technique [0002] Theophylline sodium salt is an organic substance slightly soluble in water. During the production process of synthesizing theophylline or theophylline sodium salt, a certain amount of chemical mother liquor will be produced. The mother liquor contains a small amount of theophylline or theophylline sodium salt. For a long time , bringing great burden and difficulty to wastewater treatment. [0003] In recent years, domestic and foreign research institutes and man...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/08
Inventor 袁永生郭福民寇晓康刘琼
Owner SUNRESIN NEW METERIALS CO LTD XIAN
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