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Method for producing polyether alcohols with DMC catalysts using compounds containing SIH combinations as additives

A technology of polyether alcohol and catalyst, which is applied in the field of preparing polyether alcohol by using compounds with SiH groups as additives and using DMC catalysts, which can solve the problems of not being able to approach polydispersity

Inactive Publication Date: 2013-06-26
EVONIK DEGUSSA GMBH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0018] As strongly demonstrated by ZHANG et al. (AIChE Annual Meeting, Conference Proceedings Nov. 7-12, 2004, 353B), the kinetics of alkoxylation using DMC catalysts are of such a unique nature that even when using backmixing ( Loop flow, etc.) reactors, the method of producing a narrow molecular weight distribution cannot be directed towards a higher polydispersity

Method used

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  • Method for producing polyether alcohols with DMC catalysts using compounds containing SIH combinations as additives
  • Method for producing polyether alcohols with DMC catalysts using compounds containing SIH combinations as additives
  • Method for producing polyether alcohols with DMC catalysts using compounds containing SIH combinations as additives

Examples

Experimental program
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Effect test

Embodiment 1a

[0103] At first under nitrogen, add 215.7g polypropylene glycol (weight average molecular weight M in the autoclave of 3 liters) w =2000g / mol), 0.03g of hexacyanocobaltate (III) zinc DMC catalyst and 5.9g of heptamethylhydrotrisiloxane (Rhodia) (CAS[1873-88-7] with a SiH content of 4.5eq / kg ), and heated to 130°C with stirring. The reactor was evacuated to an internal pressure of 30 mbar in order to remove by distillation any volatile constituents present. To activate the DMC catalyst, a 40.0 g portion of propylene oxide was added. After the reaction had started and the internal pressure had dropped, a further 944 g of propylene oxide were metered in continuously within 60 minutes with cooling to 130° C. and a maximum reactor internal pressure of 1.5 bar. The reaction was continued at 130° C. for 30 minutes, followed by a degassing step. This removes volatile components such as residual propylene oxide by distillation at 130°C under reduced pressure. The resulting polyethe...

Embodiment 1b

[0107] In other comparative experiments carried out similarly to Example 1a, no additives were added to the polypropylene glycol / DMC catalyst mixture at the start of the alkoxylation according to the current state of the art.

[0108] The resulting long-chain, low-viscosity polypropylene glycol has an OH value of 9.8 mg KOH / g, a viscosity (at 25°C) of 7100 mPas, and according to GPC, its polydispersity M w / M n 1.4 (relative to polypropylene glycol standard).

[0109]

[0110] Preparation of mixed ethylene oxide / propylene oxide-based polyethers with addition of additives by the process of the invention

Embodiment 2a

[0112] First add 180.0g polypropylene glycol monoallyl ether (weight average molecular weight M to 3 liters of autoclave under nitrogen) w =400g / mol), 0.08g of zinc hexacyanocobaltate DMC catalyst and 5.25g of heptamethylhydrotrisiloxane (CAS[1873-88-7]), and heated to 130°C with stirring. The reactor was evacuated to an internal pressure of 30 mbar in order to remove by distillation any volatile constituents present. To activate the DMC catalyst, a 36.0 g portion of propylene oxide was added. After the reaction had started and the internal pressure had dropped, a mixture of 396 g of ethylene oxide and 1269 g of propylene oxide was metered in continuously within 90 minutes while cooling to 130° C. and a maximum reactor internal pressure of 1.5 bar. The reaction was continued at 130°C for 30 minutes, followed by a degassing step. This removes volatile components such as residual propylene oxide by distillation at 130°C under reduced pressure. The resulting polyether is coole...

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Abstract

Process for preparing polyether alcohols with elevated polydispersity by polymerization via using double metal cyanide catalysts (DMC catalysts), is claimed, where before or during the polymerization, one or more, optionally mixed additives consisting of compounds having one or more hydrogen (H) atoms bonded to one silicon (Si) atom as Si-H additive are added to the starting reaction mixture comprising the hydroxy (OH)-functional starting compound and the DMC catalyst. An independent claim is included for a composition comprising polyether alcohols of formula (R11-[(CR6R2-CR5R3-O) nH] m) (Va), (R11-[(CR5R3-CR6R2-O) nH] m) (Vb), (R11-[(CHR2-CH(CH 2OR4)-O) nH] m) (Vc), (R11-[(CH(CH 2OR4)-CHR2-O) nH] m) (Vd) with increased polydispersity, where the polydispersity of the polyether alcohols is higher when compared to a polyether alcohol which has been prepared without using the Si-H-additive using the same reaction conditions. In formula (Va)-(Vd), R11 : hydroxyl radical or a radical having at least one carbon atom; m : 1-8, preferably 1-6; n : 1-12000, preferably 1-800; and R2, R3, R5, R6 : H or a saturated or optionally mono- or polyunsaturated, optionally mono- or polyvalent hydrocarbon radical which may also have further substitution, where R5 and R6 radicals are each a monovalent hydrocarbon radical.

Description

technical field [0001] The present invention relates to a method for controlling the molar mass distribution of hydroxyl compounds and epoxide monomers in the alkoxylation of specific hydrosiloxanes and silanes as additives, using double metal cyanide catalysts, wherein the additives have at least A negatively charged hydrogen atom directly attached to a silicon atom. Background technique [0002] Polyether alcohols, which are often also abbreviated and used synonymously as polyethers, have been known for some time and are produced industrially in large quantities and, among other applications, by reaction with polyisocyanates for the preparation of polyurethanes or for Starting compounds for the preparation of surfactants. Most processes for the preparation of alkoxylation products (polyethers) use basic catalysts such as alkali metal hydroxides and alkali metal methoxides. The use of KOH is particularly common and has been known for many years. Typically, a typical low ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/28C08L71/02C08G18/48C08G77/46B01F17/52C09K23/52
CPCC08G65/2663C08G65/22C08G65/2609C08G2650/58
Inventor W·克诺特F·舒伯特
Owner EVONIK DEGUSSA GMBH
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