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Amino polyether polyol, preparation method thereof, polyurethane rigid foam and preparation method thereof

A technology of polyether polyol and amino polyether, which is applied in the field of polyols, can solve the problems of OTDA price soaring, surface aging surface bubble deterioration, OTDA price rising, etc., and achieve good isotropy and compatibility Improvement and low cost effect

Active Publication Date: 2019-03-19
WANHUA CHEM NINGBO RONGWEI POLYURETHANE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] At present, most of the amine polyethers used for polyurethane rigid foams are amine polyethers that use the by-product OTDA of TDI as the initiator, which has good effects on the heat conduction, surface bubbles and strength of the foam. However, due to the rise of crude oil prices and the decline of TDI production, the price of OTDA has skyrocketed, resulting in an increase in costs and a shortage of raw material procurement. Therefore, there is an urgent need for a new type of amino initiator to replace the traditional OTDA to prepare amines. Polyether, and the foam performance is better than the traditional process
[0003] Traditional OTDA polyether, due to its own catalytic effect, makes the viscosity increase too fast and the cell tendency deviation during the growth of polyurethane foam, which leads to poor foam strength, slow fluidity, surface aging and Deterioration of surface air bubbles
In "The Application and Prospect of OTDA", it is also mentioned that due to its special structure, some performance losses are caused. At the same time, due to the particularity of its production channels, the price of OTDA has been rising, and the cost is getting higher and higher.

Method used

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  • Amino polyether polyol, preparation method thereof, polyurethane rigid foam and preparation method thereof
  • Amino polyether polyol, preparation method thereof, polyurethane rigid foam and preparation method thereof
  • Amino polyether polyol, preparation method thereof, polyurethane rigid foam and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] A preparation method of amino polyether polyol, the steps are:

[0075] 1) Add water (24048.9g, 1336.05mol) and 4,4'-diaminodicyclohexylmethane conjugate (1499.7g, 3.74mol) into the reaction kettle, replace with nitrogen and test the pressure, start stirring and heat to 110°C . Add 400 g of propylene oxide into the reactor by metering a flow rate of 800 g / h. Then the reaction was continued for 1 h, and then the temperature was raised to 105° C. for another 1 h.

[0076] 2) Add 20.9 g of potassium hydroxide aqueous solution (50 wt%). Water was removed under vacuum at 115° C. for 2 h. Add remaining propylene oxide 468g by flow rate 600g / h metering. After continuing to react for 1h, the temperature was raised to 135°C for another 1h.

[0077] 3) Add 36.7g of 50wt% phosphoric acid aqueous solution to remove K ions, and process to obtain the final product polyol. In the obtained polyol, X and Y are 0 and 7 respectively, and the viscosity at 20° C. is 39155 cps. The hyd...

Embodiment 2

[0079] A preparation method of amino polyether polyol, the steps are:

[0080] 1) Add water (4424.83g, 245.82mol) and 4,4'-diaminodicyclohexylmethane conjugate (184.37g, 0.46mol) into the reaction kettle, replace with nitrogen and test the pressure, start stirring and heat to 90°C . Add 80 g of propylene oxide into the reactor by metering a flow rate of 800 g / h. Then continue to react for 0.5h, then raise the temperature to 100°C and react for another 0.5h.

[0081] 2) Add 2.86 g of potassium hydroxide aqueous solution (30 wt%). The water was removed under vacuum at 100° C. for 1 h. Add remaining propylene oxide 80g by metering flow rate 600g / h. After continuing to react for 1h, the temperature was raised to 130°C for another 1h.

[0082] 3) Add 7.51 g of 20 wt % phosphoric acid aqueous solution to remove K ions, and process to obtain the final product polyol. In the obtained polyol, X and Y are 0 and 4 respectively, and the viscosity at 20° C. is 35106 cps. The hydroxyl...

Embodiment 3

[0084] A preparation method of amino polyether polyol, the steps are:

[0085] 1) Add water (15097.01g, 838.72mol) and 4,4'-diaminodicyclohexylmethane conjugate (1136.33g, 2.83mol) into the reaction kettle, replace with nitrogen and test the pressure, start stirring and heat to 110°C . Add 461.53 g of oxyalkylene (mass ratio of propylene oxide to ethylene oxide: 1:3) into the reactor at a flow rate of 800 g / h. Then the reaction was continued for 2 hours, and then the temperature was raised to 110° C. for another 2 hours.

[0086] 2) Add 3.77 g of potassium hydroxide aqueous solution (70 wt%). Water was removed under vacuum at 120° C. for 3 h. The remaining 600 g of oxyalkylene was metered in at a flow rate of 600 g / h (the mass ratio of propylene oxide to ethylene oxide was 1:3). After continuing to react for 1.5h, the temperature was raised to 140°C for another 1.5h.

[0087] 3) Add 9.24 g of 50 wt % phosphoric acid aqueous solution to remove K ions, and process to obtain...

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Abstract

The invention relates to an amino polyether polyol, a preparation method thereof, a polyurethane rigid foam and a preparation method thereof. The amino polyether polyol is prepared by taking 4, 4'-methylene biscyclohexylamine coupling agent as a starting material to react with oxidized alkenes. The structure formula of the amino polyether polyol is shown as formula I, wherein X is an integer selected from 1-3, and Y is an integer selected from 4-10. The amino polyether polyol can be applied to preparing the polyurethane rigid foam, particularly to high-standard application such as to refrigerators, and compared with traditional OTDA (orthotoluenediamine) polyethers, is higher in properties such as energy consumption, fluidity, surface blistering and strength.

Description

technical field [0001] The invention belongs to the technical field of polyols and relates to a novel amino polyether polyol, in particular to an amino polyether polyol and a preparation method thereof, a polyurethane rigid foam and a preparation method thereof. Background technique [0002] At present, most of the amine polyethers used for polyurethane rigid foams are amine polyethers that use the by-product OTDA of TDI as the initiator, which has good effects on the heat conduction, surface bubbles and strength of the foam. However, due to the rise of crude oil prices and the decline of TDI production, the price of OTDA has skyrocketed, resulting in an increase in costs and a shortage of raw material procurement. Therefore, there is an urgent need for a new type of amino initiator to replace the traditional OTDA to prepare amines. Polyether, and the foam performance is superior to the traditional process. [0003] Traditional OTDA polyether, due to its own catalytic effec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/26C08G18/48C08G18/50C08J9/14C08G101/00
CPCC08G18/482C08G18/4829C08G18/4883C08G18/5033C08G65/2627C08J9/141C08J2203/14C08G2110/0025
Inventor 郑礼倩牟砚圃初颖
Owner WANHUA CHEM NINGBO RONGWEI POLYURETHANE
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