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Method for producing short-chain polyfunctional polyether polyols utilizing superacid and double-metal cyanide catalysis

A technology of double metal cyanide and short-chain polyether, applied in the field of producing short-chain polyether polyols

Active Publication Date: 2013-12-25
DOW GLOBAL TECH LLC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Another problem with superacid catalysis is the formation of cyclic volatile by-products

Method used

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  • Method for producing short-chain polyfunctional polyether polyols utilizing superacid and double-metal cyanide catalysis
  • Method for producing short-chain polyfunctional polyether polyols utilizing superacid and double-metal cyanide catalysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1 to 7 and comparative example A

[0067] "Sorbitol", greater than (>) 99% pure, available from Aldrich;

[0068] "Glycerin", greater than (>) 99.5% pure, available from Aldrich;

[0069] "VORANOL TM CP450" is a glycerol initiated oxypropylene triol polyether polyol having a molecular weight of about 450, available from The Chemical Company;

[0070] "PO" is propylene oxide, >99.9% pure, available from The Dow Chemical Company;

[0071] "TFA" is trifluoromethanesulfonic acid (trifluoromethanesulfonic acid), >98% pure, available from Fluka; and

[0072] "DMC" is a double metal cyanide catalyst trade name ARCOL TM A3, available from Bayer.

[0073] Tests are performed according to the following methods:

[0074] "Hydroxyl value" is measured in mg / g of potassium hydroxide (KOH) according to the protocol of ASTM D4274D;

[0075] "Acid value" is measured in potassium hydroxide (KOH) mg / g and is determined by potentiometric titration of the sample in methanol with standard KOH in methanol (0.01 N: certified, ...

Embodiment 1

[0085] 686.5g (3.77mol) of crystalline sorbitol and 0.17g of 85% phosphoric acid were placed in a 5L stainless steel alkoxylation reactor. The reactor was thermostated at 120°C and a vacuum (1 mbar) was applied to the reactor. Once the sorbitol had melted inside the reactor, stirring was started (200 rpm) and a nitrogen sparge was applied from the bottom of the reactor while the vacuum pump was still running so that the total pressure inside the reactor was maintained at 10 mbar. The reaction mixture was dried under these conditions for 2 h. Turn off the sparge and vacuum, reduce the reactor temperature to 100 °C, and the reactor with 1 bar (100 kPa) N 2 Pressurize, open, and add 0.03 g trifluoromethanesulfonic acid (22 ppm based on product weight). The reactor was closed; vacuum was applied to the reactor to reduce the internal pressure to below 1 mbar. The stirring rate was increased to 400 rpm and PO (657 g, 11.31 mol) was fed into the reactor at an average feed rate of ...

Embodiment 2

[0088] 701.9 g (1.97 mol) of polyether polyol from Example 1 and DMC catalyst (0.247 g, 180 ppm based on product weight) were placed in a 5L stainless steel alkoxylation reactor. The reactor was thermostated at 150°C. Vacuum was applied to the reactor to reduce the internal pressure to below 1 mbar and agitation at 400 rpm was applied. PO (686 g, 11.81 mol) was fed into the reactor at an average feed rate of 6.2 g / min over a period of 110 min. The initial reaction rate was measured to be 6x10 -5 g / ppm / min with a reaction rate of 2x10 measured at the end of the PO feed -4 g / ppm / min. After the feed was complete, the total pressure in the reactor was equilibrated to 0.2 bar (20 kPa) over 130 min. The product was vacuum stripped at 120 °C for 1 h. A colorless viscous liquid is obtained.

[0089] The resulting polyether polyol has the following properties: OH value: 480 mg KOH / g; acid value: 0.09 mg KOH / g; total unsaturation: 0.0046 meq / g; water: 350 ppm; total volatile matte...

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Abstract

A two stage alkoxlyation process for preparing a short-chain polyether polyol from a starter compound comprising from 3 to 9 hydroxyl groups and at least one alkylene oxide, wherein said starter compound has a hydroxyl equivalent weight of from 22 to 90 Da. Said process comprises a first stage alkoxlyation using a superacid catalyst to prepare an oligomeric alkoxylated starter compound that is further alkoxylated to the short-chain polyether polyol of the invention in a second stage using a DMC catalyst. The process of the present invention may be performed continuously, in a batch, or semi-batch process.

Description

technical field [0001] The present invention relates to a method for producing short-chain polyether polyols using superacids and double metal cyanide catalysts. Background technique [0002] Polyether polyols are produced by polymerizing alkylene oxides in the presence of starter compounds. The starting compound has one or more functional groups with which the alkylene oxide can react to initiate polymer chain formation. The primary function of the starter compound is to provide molecular weight control and establish the number of hydroxyl groups the polyether polyol will have. [0003] Polyether polyol is the key raw material for the production of polyurethane. Short-chain polyfunctional polyether polyols are especially well suited for the production of rigid polyurethane foams and are therefore sometimes referred to as rigid polyether polyols. Polyether polyols for rigid applications use high functionality starter compounds such as sucrose and sorbitol. Rigid polyethe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/00
CPCC08G65/2678C08G65/2684C08G65/2696C08G65/00C08G65/10C08G18/48C08J9/00C08G2101/00C08G18/3206C08G65/2609
Inventor P·L·舒托夫H·R·范德瓦尔J-P·马希D·A·巴布
Owner DOW GLOBAL TECH LLC
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