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Method for synthesizing polyether glycol in microstructure reactor

A microstructure reactor and polyether polyol technology, applied in the field of polyether polyol preparation, can solve the problems of limited heat and mass transfer effect, reduced molecular weight of polyether polyol, and high requirements for process condition control, and can avoid large problems. The molecular weight of polyether polyol is generated, the polymerization reaction rate is increased, and the effect of overcoming the excessive polymerization

Inactive Publication Date: 2015-08-12
上海睿瓦科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the traditional preparation process mainly has the following three problems: (1) the reaction initiation time is long, resulting in the entire reaction cycle up to more than ten hours; The heat is very large, so the reaction temperature needs to be strictly controlled in the reaction process to avoid implosion due to temperature runaway; (3) due to the limited heat and mass transfer effect of the tank reactor, hot spots are easily generated in the reaction process, and the local reaction temperature is easy to exceed High, the transfer reaction of the active molecular chain increases, resulting in a decrease in the molecular weight of polyether polyols, an increase in unsaturated double bonds, and a broadening of the molecular weight distribution of the product
Although the spiral reactor can continuously prepare polyether polyols in the form of pseudo-turbulent flow, the inner diameter of the spiral reaction tube is at least 6.3mm, and the mixing effect is limited, resulting in too long residence time
At the same time, multiple temperature-changing operations also increase the difficulty of operation.
[0006] To sum up, the batch process has the problems of long initiation time, low operating efficiency, and easy reaction implosion, and the continuous process has the problems of complex equipment, high requirements for process condition control, and long residence time.

Method used

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  • Method for synthesizing polyether glycol in microstructure reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The catalyst solution produced by the reaction of propylene oxide, 1,3-propanediol and potassium hydroxide is fed at a molar ratio of propylene oxide to 1,3-propanediol of 16:1, and pumped into the micro-mixer and extended residence time respectively. In the microstructure reactor composed of tubes, the content of potassium hydroxide is 3000ppm, the inner diameter of the channel of the micromixer is 45um, and the outlet of the micromixer is connected to a 25m residence time extension tube with an inner diameter of 0.5mm and a material of 316L. Control the reaction time to be 120s, the reaction temperature to be 190°C, and the reaction pressure to be 10MPa. The collected products go through the steps of neutralization, adsorption, degassing, and filtration in sequence to obtain a refined polyether polyol, which is designated as sample A1. The obtained product has a hydroxyl value of 162 mgKOH / g and a relative molecular mass of 1034 g / mol.

Embodiment 2

[0018] The mixture of propylene oxide and ethylene oxide (mass fraction of ethylene oxide is 15%), glycerin and potassium hydroxide react the catalyst liquid that generates with the mixture of propylene oxide and ethylene oxide and glycerine Alcohol is fed at a molar ratio of 35:1 and pumped into a microstructure reactor composed of a micromixer and a residence time extension tube, wherein the content of potassium hydroxide is 3000ppm, and the channel size of the micromixer has an inner diameter of 45um , the outlet of the micro-mixer was connected to a 50m residence time extension tube with an inner diameter of 0.5mm and a material of 316L, the reaction time was controlled to be 240s, the reaction temperature was 190°C, and the reaction pressure was 10MPa. The collected product goes through the steps of neutralization, adsorption, degassing, and filtration in sequence to obtain refined polyether polyol, which is designated as sample A2. The hydroxyl value of the obtained prod...

Embodiment 3

[0020] The catalyst solution generated by the reaction of propylene oxide, glycerol and potassium hydroxide is pumped into the microstructure reactor composed of micro-mixer and residence time extension tube respectively (wherein the molar ratio of propylene oxide and glycerin is 4:1 is fed, and the content of potassium hydroxide is 3000ppm), and the inner diameter of the channel size of micro-mixer is 25um, and the micro-mixer outlet connection 6m inner diameter is 0.5mm, the residence time extension tube of titanium tube material, and the control reaction time is 30s, the reaction temperature is 175°C, and the reaction pressure is 3MPa. The collected product goes through the steps of neutralization, adsorption, degassing, and filtration in sequence to obtain refined polyether polyol, which is designated as sample A3. The hydroxyl value of the obtained product is 519 mgKOH / g, and the relative molecular mass is 324 g / mol. The infrared spectrum of sample A3 is as follows figu...

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Abstract

The invention relates to a method for synthesizing polyether glycol in a microstructure reactor, which comprises the following steps: respectively pumping oxyalkylene and a catalyst liquid generated by reacting an alkaline catalyst and an initiator into the microstructure reactor composed of a micro-mixer and a retention time prolonging pipe, reacting while controlling the reaction temperature and pressure, neutralizing the reaction solution, adsorbing, degassing and filtering to obtain the refined polyether glycol. The hydroxyl value of the refined polyether glycol is 50-550 mgKOH / g, and the relative molecular mass is 300-3300 g / mol. The method overcomes the defects of long initiation time and low operational efficiency in the intermitted technique, solves the problems of complex equipment, high requirements for technological condition control and long retention time in the continuous technique, implements quick and continuous production, and has the advantages of short reaction time, simple technique, high safety, high controllability, high adjustment flexibility, continuous operation and the like.

Description

technical field [0001] The present invention relates to a preparation method of a class of polyether polyols, in particular to a method for synthesizing polyether polyols in a microstructure reactor, using polyols or polyamines as initiators, oxyalkylenes as monomers, and alkaline Catalyst for rapid and continuous preparation of polyether polyols in microstructure reactors. Background technique [0002] Polyether polyol is an important chemical raw material, widely used in industries such as papermaking, textile, printing and dyeing, synthetic leather, coating, adhesive, elastomer, foam plastic, sealant and petroleum development. The main raw material of the product. Polyether polyols are formed by ring-opening polymerization with low molecular weight polyols, polyamines or compounds containing active hydrogen as initiators, and alkylene oxides under the action of catalysts. Its conventional industrial production is usually carried out in a tank reactor. In this method, an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C08G65/26
Inventor 张利雄丁荣王重庆沈如伟
Owner 上海睿瓦科技有限公司
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