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A kind of purification method of polyethylene glycol containing ethylene oxide impurity

A refining method and technology of ethylene oxide, which is applied in the field of refining polyethylene glycol, can solve the problems of difficult removal of ethylene oxide, failure to meet high-level requirements, and high residual impurities, and achieve low cost, mild conditions, and high-quality products. The effect of stable quality

Active Publication Date: 2016-06-22
辽宁奥克药业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome the defects of difficult removal of ethylene oxide, high residual impurities and inability to meet high-level requirements in the existing polyethylene glycol production process, the purpose of the present invention is to provide a polyethylene glycol containing ethylene oxide impurity Refining method, the content of ethylene oxide in the obtained refined polyethylene glycol can be reduced to less than 1ppm, which meets the pharmacopoeia standard, and can be applied to the fields of medicine, cosmetics and other products that are in contact with the human body

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. Preparation of sodium triethylene glycol

[0025] Under the protection of nitrogen, add 751 milligrams of sodium metal to 10 grams of freshly distilled commercially available triethylene glycol, and stir at room temperature until the complete reaction of metal sodium, so that a 50% mass percent sodium triethylene glycol / triethylene glycol solution is prepared. Stored in a glass bottle under a nitrogen atmosphere for later use, referred to as highly active monomer 1.

[0026] 2. The refining of polyethylene glycol

[0027] In a well-ventilated fume hood, take 30 grams of spray and circulate 5m 3 The polyethylene glycol-4000 (residual ethylene oxide monomer containing 20ppm) produced by the ethoxylation reaction device is added in a 50 milliliter glass reaction bottle, and 2 milligrams of high activity monomer 1 are added, and after nitrogen replacement, under stirring, Maintain a negative pressure of 0.05 bar, heat to 130°C, use gas chromatography to detect the resi...

Embodiment 2

[0029] Refining of Polyethylene Glycol

[0030] In a well-ventilated fume hood, take 100 grams of spray and circulate 5m 3The Polyethylene Glycol-6000 (residual oxirane monomer containing 25ppm) that ethoxylation reaction unit produces adds in 150 milliliters of glass reaction vials, adds the highly reactive monomer 1 that 6 milligrams of embodiments 1 make, After nitrogen replacement, under stirring and maintaining a negative pressure of 0.05 bar, heat to 130°C, and detect the residual ethylene oxide monomer by gas chromatography until the residual ethylene oxide monomer content is less than 1ppm, and the reaction is about Carry out for 30 minutes, cool to 70°C, neutralize with lactic acid to pH 7, and then cool to room temperature, the residual ethylene oxide monomer content in the polyethylene glycol 6000 product produced in this way is not higher than 1ppm, which meets the pharmacopoeia standard .

Embodiment 3

[0032] The specific operation is the same as in Example 1, except that 4.473 grams of metal barium is used instead of 751 mg of metal sodium, so that the residual ethylene oxide monomer content in the polyethylene glycol 4000 product is not higher than 1ppm, which meets the Pharmacopoeia standard.

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PUM

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Abstract

The invention provides a method for refining polyethylene glycol containing ethylene oxide impurities. The crude polyethylene glycol to be refined is mixed with an initiator containing active hydrogen in the presence of a highly active ethoxylation reaction unit. The ethylene oxide impurities contained therein are removed through ethoxylation to obtain refined polyethylene glycol; wherein, the highly active ethoxylation reaction unit is selected from triethylene glycol, tetraethylene glycol or polyethylene glycol Metal salts of diols. The refining method provided by the invention can effectively remove the trace amount of ethylene oxide impurities in polyethylene glycol products, so that its content is reduced to below 1ppm, which meets the requirements of pharmaceutical grade; the refining method of the present invention will not introduce new impurities, and the obtained The product quality of polyethylene glycol is guaranteed and the product batch repeatability is good, and the product quality is stable; the refining method of the present invention has short reaction time, mild conditions, simple operation, friendly environment, high production efficiency and low cost, and is very suitable for use for industrial applications.

Description

technical field [0001] The invention relates to the field of pharmaceutical excipients, in particular to a method for refining polyethylene glycol containing ethylene oxide impurities. Background technique [0002] The structural formula of polyethylene glycol (PEG) is H(OCH 2 CH 2 ) n OH, n represents the average addition number of ethylene oxide, n can range from 4 to 900, and the corresponding average molecular weight is 180 to 40,000. PEG is usually produced by ethoxylation of ethylene oxide with water, ethylene glycol, and diethylene glycol (US2007 / 0179199A1 Polyethyleneglycolandproducingofthesame.). Pharmaceutical polyethylene glycol is often in contact with human skin, and it can also be taken orally or injected into the body, for example, it can be used as a solvent for active ingredients of medicines, a fixative for spices in medicinal dripping pills, a liquid component in injections, dietary supplements Ointment bases in tablets, tablets and suppositories, solv...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/46
Inventor 孔凡志朱建民刘兆滨仲崇纲
Owner 辽宁奥克药业股份有限公司
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