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Catalyst for preparing polyalkyl glycol allyl amyl ether and preparation method thereof

A technology of allyl polyoxyalkylene alkenyl ether and catalyst, applied in the field of catalysts, can solve the problems of reducing the purity of allyl polyoxyalkylene alkenyl ether and cannot be completely removed, and achieves the effect of improving the purity

Inactive Publication Date: 2011-09-07
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] ③Sodium alkoxide as a catalyst, such as sodium methoxide, sodium ethoxide, etc., reacts with the initiator allyl alcohol to form methanol, ethanol, etc., and their boiling points are lower than that of water, so they cannot be completely removed during alkoxylation , they react with alkylene oxide ring-opening to generate impurity by-product polyether, reducing the purity of allyl polyoxyalkylene ether

Method used

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  • Catalyst for preparing polyalkyl glycol allyl amyl ether and preparation method thereof
  • Catalyst for preparing polyalkyl glycol allyl amyl ether and preparation method thereof
  • Catalyst for preparing polyalkyl glycol allyl amyl ether and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Put 40Kg of allyl alcohol into a 100L reactor, cut 0.8Kg of sodium metal into small pieces and put it into the feeding device, feed nitrogen to replace the air in the reactor, keep the vent valve open and feed nitrogen, and feed the condenser Cool the water, open the feeding device, feed once every 10 minutes, 0.16Kg once, close the feed valve after adding the metal sodium, and continue the reaction until the reaction solution has no bubbles. The mass percent concentration of sodium allylate in the obtained allyl alcohol solution of sodium allylate is 7%.

[0028] Add 348g of the above-mentioned catalyst into 2.0Kg allyl alcohol, drop into a 50L autoclave while stirring, and feed N 2 Substitute three times, raise the temperature to 100°C, introduce 1.5Kg of ethylene oxide, raise the temperature to 160°C, react for about 30 minutes, continue to add 16.7Kg of ethylene oxide, keep the reaction temperature at 160°C, and carry out polymerization under the pressure of 0.3Mpa....

Embodiment 2

[0032] Put 40Kg of allyl alcohol into a 100L reactor, cut 1.6Kg of sodium metal into small pieces and put it into the feeding device, feed nitrogen to replace the air in the reactor, keep the vent valve open and feed nitrogen, and feed the condenser Cool the water, open the feeding device, feed once every 10 minutes, 0.16Kg once, close the feed valve after adding the metal sodium, and continue the reaction until the reaction solution has no bubbles. The mass percent concentration of sodium allylate in the obtained allyl alcohol solution of sodium allylate was 13%.

[0033] Add 174g of the above catalyst into 2.0Kg allyl alcohol, drop into a 50L autoclave while stirring, feed N 2 Replace three times, raise the temperature to 100°C, introduce 2.0Kg of ethylene oxide, raise the temperature to 160°C, react for about 30 minutes, continue to add 28.4Kg of ethylene oxide, keep the reaction temperature at 160°C, and carry out polymerization under the pressure of 0.3Mpa. After 2 hours ...

Embodiment 3

[0037] Put 40Kg of allyl alcohol into a 100L reactor, cut 2.4Kg of sodium metal into small pieces and put it into the feeding device, feed nitrogen to replace the air in the reactor, keep the vent valve open and feed nitrogen, and feed the condenser Cool the water, open the feeding device, feed once every 10 minutes, 0.16Kg once, close the feed valve after adding the metal sodium, and continue the reaction until the reaction solution has no bubbles. The mass percent concentration of sodium allylate in the obtained allyl alcohol solution of sodium allylate was 19%.

[0038] Add 174g of the above-mentioned catalyst into 2.0Kg allyl alcohol, drop into a 100L autoclave while stirring, and feed N 2 Replace three times, raise the temperature to 100°C, introduce 5Kg of ethylene oxide, raise the temperature to 160°C, react for about 30 minutes, continue to add 71Kg of ethylene oxide, keep the reaction temperature at 160°C, and carry out polymerization under the pressure of 0.25Mpa, co...

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Abstract

The invention discloses a catalyst for preparing polyalkyl glycol allyl amyl ether, which is an allyl alcohol solution of sodium allylate of which the mass percent concentration in the solution is 7%-37%. The preparation method comprises the following steps of: (1) putting allyl alcohol into a reaction kettle, chipping sodium metal and putting into a charging device; (2) performing nitrogen displacement, keeping an air release valve in an open state and introducing nitrogen; and (3) introducing cooling water into a condenser, adding the sodium metal in batches, controlling the temperature of the reaction system not to exceed 130 DEG C, closing a charging valve after adding the sodium metal, continuing reaction until the reaction liquid is free of bubbles, closing the air release valve, stopping introducing nitrogen, and discharging. In the process of preparing the polyalkyl glycol allyl amyl ether by the catalyst, byproducts can not be generated, thus effectively improving the purity of the polyalkyl glycol allyl amyl ether.

Description

technical field [0001] The invention relates to a catalyst, in particular to a catalyst for preparing a special polyether-allyl polyoxyalkylene ether for polycarboxylate water reducers, and a preparation method thereof. Background technique [0002] Allyl polyoxyalkylene ether is the main raw material for the production of this type of polycarboxylic acid-based high-performance water-reducer. The polyether has good water solubility and will not be hydrolyzed and deteriorated. The synthetic water-reducer has a high water-reducing rate. The reinforcement effect is good, the steel bar is not corroded, and it is green and environmentally friendly. Therefore, it is very important to produce allyl polyoxyalkylene ethers with high double bond activity. Domestic manufacturers of polyether raw materials mainly produce through anionic ring-opening polymerization of alkylene oxide, and most manufacturers use catalysts that more or less bring in impurities during the polymerization pro...

Claims

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Application Information

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IPC IPC(8): C08G65/28C07C43/178C07C41/03
Inventor 王自为裴继凯李军平窦琳王正波
Owner SHANXI UNIV
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