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Synthesis of monomethoxy polyglycol

A technology of polyethylene glycol and monomethoxyl, which is applied in the field of synthesizing monomethoxypolyethylene glycol, can solve the problems of polyethylene glycol separation difficulties, decreased reaction selectivity, catalyst deactivation, etc., and achieve the molecular weight of the product The effect of narrow distribution, high purity of reaction products and high reaction selectivity

Inactive Publication Date: 2009-02-18
NANJING UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The principle of molecular sieve water removal is physical adsorption. Although it can be used repeatedly, its water removal ability is poor, and it can only reduce the water in ethylene oxide to 100ppm.
The existence of moisture has many adverse effects on the polymerization reaction. The moisture will react with the catalyst sodium methoxide to generate methanol and sodium hydroxide, which will deactivate the catalyst, slow down the reaction rate or even make the reaction impossible, and the molecular weight of the reaction product can only reach five thousand
Moisture also reacts with ethylene oxide to generate polyethylene glycol, which is easier to carry out than the reaction between methanol and ethylene oxide, that is, the main reaction, so that the reaction selectivity is greatly reduced. Polyethylene glycol and monomethoxy It is difficult to separate the base polyethylene glycol, and the cost of post-processing increases

Method used

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  • Synthesis of monomethoxy polyglycol
  • Synthesis of monomethoxy polyglycol
  • Synthesis of monomethoxy polyglycol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Such as figure 1 As shown, 1.20kg of ethylene oxide (moisture content is 200ppm) is added to a 10-liter evaporator through a drier equipped with 50g of calcium hydrogen (a total of 125kg of ethylene oxide can be processed), and a condenser and a condenser are connected after the evaporator. A receiving tank. During the heating and evaporation process, the steam is condensed by the condenser and then collected into the receiving tank. The ethylene oxide was then transferred to a dry ethylene oxide tank to obtain 1.10 kg of ethylene oxide with a moisture content of 10 ppm and a yield of 91.67%.

[0024] 0.5 liter of anhydrous toluene (moisture content: 4.8 ppm) was added to a 5 liter autoclave. The kettle has a solid feeding pipeline, an ethylene oxide feeding pipeline with a distributor, a stirrer, a thermometer and a explosion-proof membrane (8Kg / cm 2 ) and explosion-proof piping for pressure gauges. Anhydrous toluene was heated to 90°C. Stir for 30 minutes (the sp...

Embodiment 2

[0031] Put 1.30kg of ethylene oxide (moisture content is 200ppm) into a 10-liter evaporating kettle through a drier equipped with 50g of calcium hydrogen (a total of 125kg of ethylene oxide can be processed), and a condenser and a receiving tank are connected behind the evaporating kettle . Heating and evaporating, the steam is condensed by the condenser and then collected into the receiving tank. Ethylene oxide is transferred to dry ethylene oxide tank again, and 1.20kg oxirane is received. The moisture content is 9ppm, and the yield is 92.31%.

[0032] 0.5 liter of anhydrous toluene (moisture content: 4.8 ppm) was added to a 5 liter autoclave. The kettle has a solid feeding pipeline, an ethylene oxide feeding pipeline with a distributor, a stirrer, a thermometer and a explosion-proof membrane (8Kg / cm 2) and explosion-proof piping for pressure gauges. Anhydrous toluene was heated to 90°C. Stir for 30 minutes (the speed of the mixer is 500 rpm), and ensure that the two fe...

Embodiment 3

[0038] Add 1.25kg of ethylene oxide and 0.5g of calcium hydrogen into a 10-liter evaporator with agitator, and connect a condenser and a receiving tank behind the evaporator. After half an hour of vigorous stirring (the speed of the stirrer is 500 rpm), keep stirring and heat to evaporate, and the steam is condensed by the condenser and then collected into the receiving tank. The ethylene oxide was then transferred to a dry ethylene oxide tank to obtain 1.10 kg of ethylene oxide with a water content of 7 ppm and a yield of 88%.

[0039] Add 0.5 liter of anhydrous diethylene glycol dimethyl ether (moisture content: 5 ppm) to a 5 liter autoclave. The kettle has a solid feeding pipeline, an ethylene oxide feeding pipeline with a distributor, a stirrer, a thermometer and a explosion-proof film (8Kg / cm 2 ) and explosion-proof piping for pressure gauges. Anhydrous diglyme was heated to 90°C. Stir for 30 minutes (the speed of the mixer is 500 rpm), and ensure that the two feeding ...

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Abstract

The invention discloses a method for synthesis of monomethoxy poly(ethylene glycol), including the steps that ethylene oxide is transferred to a dried ethylene oxide tank after calcium-hydrogen treatment, the autoclave is processed, dried methyl alcohol is added into the potassium methoxide to prepare solution with 10-30 percent of mass fractions; the achieved solution is added into the autoclave, the autoclave is heated to 90 DEG C, the ethylene oxide is added into the autoclave and stirred under 120 plus and minus 2 DEG C continuously until the pressure of the reaction system approaches to normal pressure, then the temperature is lowered to 80 DEG C, and the product of reaction is transferred out; the pH of the reaction product is adjusted to be 7.0 by citric acid; finally, the desired monomethoxy poly(ethylene glycol) is achieved after being dried. The purity of the product is proved very high by gel permeation chromatography, and the molecular weight distribution is very narrow. The polyoxyethylene compound used as the initial medical material is mainly applied to drug release system.

Description

technical field [0001] The invention relates to a chemical synthesis process, specifically a method for synthesizing monomethoxypolyethylene glycol (mPEG). Background technique [0002] Monomethoxypolyethylene glycol (mPEG) is used as a starting material for polyoxyethylene compounds modified at one end, and is used in the field of medicine, especially for chemically modifying some physiologically active proteins such as polypeptides and enzymes. The compound is also used in drug delivery system to chemically modify liposomes and polymer capsules. At present, there are few companies in China that can produce qualified (high-purity narrow molecular weight distribution) pharmaceutical-grade mPEG products. The latest foreign production technology is to use molecular sieves as a water-removing agent to treat ethylene oxide, and then use sodium methoxide as a catalyst Synthesis of monomethoxy polyethylene glycol. The principle of molecular sieve water removal is physical adsorp...

Claims

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Application Information

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IPC IPC(8): C08G65/28
Inventor 芮必胜顾浩黄友林吴仁荣陈兴国高正松康彦彪
Owner NANJING UNIV
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