Alkoxylations in microstructured capillary reactors
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IPC분류정보
국가/구분
United States(US) Patent
등록
국제특허분류(IPC7판)
C07C-041/03
B01J-010/00
출원번호
UP-0083172
(2005-03-17)
등록번호
US-7858829
(2011-02-24)
우선권정보
DE-10 2004 013 551(2004-03-19)
발명자
/ 주소
Hubel, Roland
Markowz, Georg
Recksik, Manfred
Rudek, Markus
Wewers, Dietmar
Zeller-Schuldes, Florian
출원인 / 주소
Evonik Goldschmidt GmbH
대리인 / 주소
Frommer Lawrence & Haug LLP
인용정보
피인용 횟수 :
5인용 특허 :
4
초록▼
The invention relates to a process and to an apparatus for preparing polyether alcohols by alkoxylating alcohols, and also long-chain polyether alcohols having a narrow product distribution. The process is preferably carried out continuously in the liquid phase in a microstructured reactor. An alkyl
The invention relates to a process and to an apparatus for preparing polyether alcohols by alkoxylating alcohols, and also long-chain polyether alcohols having a narrow product distribution. The process is preferably carried out continuously in the liquid phase in a microstructured reactor. An alkylene oxide or different alkylene oxides are metered at one or more points into the channels of the microreactor. The channels are cooled with the aid of a cooling medium or heated with the aid of a heating medium.
대표청구항▼
What is claimed is: 1. A process for preparing polyether alcohols of the general formula (I) by alkoxylating compounds of the general formula R1(XR′)m in a microstructured reactor with parallel-connected channel arrays for carrying out chemical reactions between substantially liquid react
What is claimed is: 1. A process for preparing polyether alcohols of the general formula (I) by alkoxylating compounds of the general formula R1(XR′)m in a microstructured reactor with parallel-connected channel arrays for carrying out chemical reactions between substantially liquid reactants, optionally in the presence of a solid catalyst, the chemical process taking place in spaces which are formed by two or more substantially plane-parallel plates or layers, wherein the reactants are mixed individually in each reaction channel in monophasic liquid form and a heat exchanger apparatus, specifically a cooling or heating apparatus, is provided, and the reactor is designed for pressures of up to about 800 bar and temperatures in the range from —about 30° C. to about 400° C., wherein the hydraulic diameter of the channels is less than 2 mm; which comprises mixing the compound R1(XR′)m and a suitable catalyst and introducing them into the reactor, feeding thereto a number of equivalents of alkylene oxide selected from the group consisting of from about 1 to about 300 and from about 2 to about 150, directly or at a plurality of points, into the reactor and mixing them with the compound R1(XR′)m, catalyst and/or subsequent products thereof, reacting them in the reaction channels at a temperature in the range from 50 to 300° C. and a pressure in the range of from 11 to 800 bar, and subsequently cooling the product mixture, where R1 is a mono- or polyvalent organic radical, m is a an integer of from 1 to 10, n is an integer from 1 to 200, R2 in the molecule is uniformly or differently hydrogen and/or a substituted or unsubstituted organic radical, X is O, S, NH or NR′, and each R′ is independently, a hydrogen, a substituted or unsubstituted organic cyclic or acyclic wherein the residence time of the reaction mixture in the reaction channel is selected from the group of times consisting of from about 1 to about 600 seconds, from about 50 to about 400 seconds and from about 100 to about 300 seconds. 2. The process as claimed in claim 1, which is operated continuously. 3. The process as claimed in claim 1, wherein the reaction temperature in the reaction channels is selected from the group of temperature ranges consisting of from about 80 to about 200° C. and from about 120 to about 200° C. 4. The process as claimed in claim 1, wherein the pressure in the reaction channels is selected from group of pressure ranges consisting of from about 40 to about 500 bar and from about 60 to about 180 bar. 5. The process as claimed in claim 1, wherein X is O. 6. The process as claimed in claim 5, wherein alkylene alcohols and/or alkyl alcohols, are used. 7. The process as claimed in claim 5, wherein fatty acids, phosphoric esters and/or phosphoric acids are used. 8. The process as claimed in claim 1, wherein X is NR′. 9. The process as claimed in claim 1, wherein the alkylene oxide is ethylene oxide, propylene oxide, butylene oxide, styrene oxide, dodecene oxide and/or allyl glycidyl ether. 10. The process as claimed in claim 1, wherein the catalyst is used in an amount of from 0.001 to 30% by weight, based on the amount of the compound of the general formula R1(XR′)m. 11. The process as claimed in claim 10, wherein the catalyst is selected from the group consisting of a base, an alkali metal methoxide and an alkali metal hydroxide. 12. The process as claimed in claim 11, wherein the catalyst is used in an amount selected from the group of weight ranges consisting of from about 0.01 to about 30% by weight and from about 1 to about 15% by weight, based on the amount of the compound of the general formula R1(XR′)m. 13. The process as claimed in claim 10, wherein the catalyst is selected from the group consisting of an acid, an organometallic compound and a bimetallic compound. 14. The process as claimed in claim 13, wherein the catalyst is used in an amount selected from the group of weight ranges consisting of from about 0.001 to about 10% by weight, and from about 0.01 to about 3% by weight, based on the amount of the compound of the general formula R1(XR′)m. 15. The process as claimed in claim 1, wherein alkylene oxide, different alkylene oxides and/or mixtures of different alkylene oxides are fed to the reaction capillaries through a number range of inlet points selection from the group consisting of one or more inlet points and up to 20 inlet points. 16. The process of claim 1, wherein the process comprises mixing the compound R1(XR′)m and a suitable catalyst and introducing them into the reactor, feeding thereto a range of equivalents of alkylene oxide selected from the group consisting of from about 5 to about 120 and from about 10 to about 80, directly or at a plurality of points, into the reactor and mixing them with the compound R1(XR′)m, catalyst and/or subsequent products thereof, reacting them in the reaction capillaries at a temperature in the range from 50 to 300° C. and a pressure in the range of from 11 to 800 bar, and subsequently cooling the product mixture, where R1 is a mono- or polyvalent organic radical, m is an integer of from 1 to 10, n is an integer from 1 to 200, R2 is uniformly or differently hydrogen and/or an organic radical selected from the group consisting of substituted or unsubstituted C1-C12 alkyl, C2-C12 alkenyl, phenyl, CH3, C2H5, phenyl, C10H21, and allyloxymethyl, X is O, S, NH or NR′, and R′ is hydrogen, an organic cyclic, optionally substituted radical, having from 4-7 carbon atom or acyclic, optionally substituted radical, having from 1 to 26 carbon atoms, wherein the substituents are selected from the group consisting of amino, hydroxy, halogen, C1-C4 alkyl, C1-C4 alkoxy and C1-C4 acyl. 17. The process of claim 15, wherein the process comprises mixing the compound R1(XR′)m and a suitable catalyst and introducing them into the reactor, feeding thereto a range of equivalents of alkylene oxide selected from the group consisting of from about 5 to about 120 and from about 10 to about 80, directly or at a plurality of points, into the reactor and mixing them with the compound R1(XR′)m, catalyst and/or subsequent products thereof, reacting them in the reaction capillaries at a temperature in the range from 50 to 300° C. and a pressure in the range of from 11 to 800 bar, and subsequently cooling the product mixture, where R1 is a mono- or polyvalent organic radical, m is an integer of from 1 to 10, n is an integer from 1 to 200, R2 is uniformly or differently hydrogen and/or an organic radical selected from the group consisting of substituted or unsubstituted C1-C12 alkyl, C2-C12 alkenyl, phenyl, CH3, C2H5, phenyl, C10H21, and allyloxymethyl, X is O, S, NH or NR′, and R′ is hydrogen, an organic cyclic, optionally substituted radical, having from 4-7 carbon atom or acyclic, optionally substituted radical, having from 1 to 26 carbon atoms, wherein the substituents are selected from the group consisting of amino, hydroxy, halogen, C1-C4 alkyl, C1-C4 alkoxy and C1-C4 acyl. 18. The process as claimed in claim 1, wherein the residence time of the reaction mixture in the reaction channel is from about 100 to about 300 seconds and the reaction temperature in the reaction channel is from about 120 to about 200° C. 19. The process as claimed in claim 1, wherein the residence time of the reaction mixture in the reaction channel is from about 100 to about 300 seconds and the reaction temperature in the reaction channel is from about 185 to about 195° C. 20. The process as claimed in claim 1, wherein the polyether alcohols of general formula (I) have a molecular weight distribution MW/Mn of not more than 1.25. 21. The process as claimed in claim , wherein the hydraulic diameter of the channels is less than 1 mm. 22. The process as claimed in claim 20, wherein Mw/Mn is not more than 1.25, the ethylene oxide content of the polyether alcohol is less than 10 ppm, n is 25 to 90 and the conversion rate of the process is at least about 97%.
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