Synthesis of benzyloxyphenoxy phenol ligands
US-10815255-B2 · Oct 27, 2020 · US
US10532969B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10532969-B2 |
| Application number | US-201515763318-A |
| Country | US |
| Kind code | B2 |
| Filing date | Dec 11, 2015 |
| Priority date | Sep 30, 2015 |
| Publication date | Jan 14, 2020 |
| Grant date | Jan 14, 2020 |
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The present invention provides a method for directly preparing glycol dimethyl ether and co-producing ethylene glycol from ethylene glycol monomethyl ether. More specifically, the method comprises passing a feedstock containing a raw material of ethylene glycol monomethyl ether and a carrier gas through a reactor loaded with a solid acid catalyst to produce glycol dimethyl ether and ethylene glycol, at a reaction temperature range from 40° C. to 150° C. and a reaction pressure range from 0.1 MPa to 15.0 MPa; wherein a carrier gas is an optional inactive gas; and the feedstock contains water whose volume concentration in the feedstock is in a range from 0% to 95%; and the weight hourly space velocity of the raw material of ethylene glycol monomethyl ether is in a range from 0.05 h −1 to 5.0 h −1 ; and the volume concentration of the raw material of ethylene glycol monomethyl ether in the feedstock is in a range from 1% to 100%; and the volume concentration of the carrier gas in the feedstock is in a range from 0% to 99%. In the method of the present invention, using a solid acid as a catalyst and ethylene glycol monomethyl ether as a raw material, under a low temperature condition, glycol dimethyl ether and ethylene glycol are prepared directly with high selectivity; moreover, there is substantially or completely no production of by-product 1,4-dioxane that causes pollution to the environment and is harmful to the human body or animal bodies.
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The invention claimed is: 1. A method for directly preparing glycol dimethyl ether and co-producing ethylene glycol from ethylene glycol monomethyl ether, which comprises: passing a feedstock containing a raw material of ethylene glycol monomethyl ether and a carrier gas through a reactor loaded with a solid acid catalyst to produce glycol dimethyl ether and ethylene glycol, at a reaction temperature range from 40° C. to 150° C. and a reaction pressure range from 0.1 MPa to 15.0 MPa; wherein a carrier gas is an optional inactive gas; and the feedstock contains water whose volume concentration in the feedstock is no more than 95%; and the weight hourly space velocity of the raw material of ethylene glycol monomethyl ether is in a range from 0.05 h −1 to 5.0 h −1 ; and the volume concentration of the raw material of ethylene glycol monomethyl ether in the feedstock is in a range from 1% to 100%; and the volume concentration of the carrier gas in the feedstock is no more than 99%, wherein the volume concentration of all components of the feedstock is 100%; and wherein the solid acid catalyst is an acidic molecular sieve catalyst; and wherein the acidic molecular sieve catalyst is one or more molecular sieves selected from the group consisting of an MCM-22 molecular sieve, a ferrierite molecular sieve, a ZSM-5 molecular sieve, a mordenite molecular sieve, a Y molecular sieve and a β molecular sieve; wherein the atom ratio of Si to Al in the MCM-22 molecular sieve Si/Al is in a range from 5 to 100; the atom ratio of Si to Al in the ferrierite molecular sieve Si/Al is in a range from 5 to 100; the atom ratio of Si to Al in the ZSM-5 molecular sieve Si/Al is in a range from 5 to 100; the atom ratio of Si to Al in the mordenite molecular sieve Si/Al is in a range from 5 to 50; the atom ratio of Si to Al in the Y molecular sieve Si/Al is in a range from 3 to 50; and the atom ratio of Si to Al in the β molecular sieve Si/Al is in a range from 5 to 100. 2. The method according to claim 1 , wherein the water is introduced by being added to the raw material of ethylene glycol monomethyl ether. 3. The method according to claim 1 , wherein the acidic molecular sieve catalyst comprises one or more metals selected from the group consisting of alkali metal, alkaline earth metal and rare earth metal; and the mass fraction of the metal is in a range from 0.1% to 10%. 4. The method according to claim 1 , wherein the reaction temperature is in a range from 50° C. to 150° C., and the reaction pressure is in a range from 3.0 MPa to 8.0 MPa, and the weight hourly space velocity of the raw material of ethylene glycol monomethyl ether is in a range from 0.3 h −1 to 2.0 h −1 . 5. The method according to claim 1 , wherein the inactive gas is one or more gases selected from the group consisting of nitrogen, helium and argon, and the volume concentration of the carrier gas in the feedstock is in a range from 1% to 99%. 6. The method according to claim 1 , wherein the reactor is a fixed bed reactor or a tank reactor. 7. The method according to claim 3 , wherein a mass fraction of the metal is in a range from 0.1% to 4%; and the acidic molecular sieve catalyst comprises one or more binders selected from the group consisting of aluminium oxide and silicon oxide; and the mass fraction of the binder is in a range from 1% to 40%.
Zeolite Beta · CPC title
Y-type faujasite · CPC title
of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively · CPC title
of the mordenite type · CPC title
of ethers, including cyclic ethers, e.g. oxiranes · CPC title
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