# US 2022/0033331 A1 · Shut-down process for the production of glycols > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 2022/0033331 A1 - Document ID: US20220033331A1 - Status: Published application - Kind: A1 - Application number: 17/277,261 - Filed: 2019-09-10 - Published: 2022-02-03 - Earliest claimed: 2018-09-13 - Assignees: Shell Oil Company - Applicants: Shell Oil Company - Inventors: Dionysius Jacobus Maria DE VLIEGER; Pieter HUIZENGA; Munro MACKAY; Lucas Petrus Simon KEYZER; Duraisamy MUTHUSAMY - Web page: https://patentgrep.com/patent/US20220033331A1 ## CPC - C07C 29/132: by reduction of an oxygen containing functional group - B01J 8/0015: {Feeding of the particles in the reactor; Evacuation of the particles out of the reactor} - B01J 19/0013: {Controlling the temperature of the process} - B01J 23/30: Tungsten - B01J 2208/00637: Means for stopping or slowing down the reaction - B01J 2219/00245: Avoiding undesirable reactions or side-effects - C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS - B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS ## Abstract The invention provides a shut down method for a process for the preparation of glycols from a starting material comprising one or more saccharides in the presence 5 of hydrogen and a catalyst system comprising one or more retro-aldol catalysts comprising tungsten and one or more catalytic species suitable for hydrogenation in a reactor, said method comprising removing the one or more retro-aldol catalysts from the reactor whilst also in the presence of one or more agents suitable to suppress tungsten precipitation. ## Claims ### Claim 1 A shut-down method for a process for the preparation of glycols from a stream comprising one or more saccharides in the presence of hydrogen and a catalyst system comprising one or more retro-aldol catalysts comprising tungsten and one or more catalytic species suitable for hydrogenation in a reactor, said method comprising removing the one or more retro-aldol catalysts from the reactor whilst also in the presence of one or more agents suitable to suppress tungsten precipitation. ### Claim 2 (depends on 1) The method according to claim 1, wherein the one or more agents suitable to suppress tungsten precipitation comprise at least one of organic oxygenates or buffer systems comprising one or more organic acids, their corresponding conjugated bases with alkali-metal as their counterions, and mixtures thereof. ### Claim 3 (depends on 2) The method according to claim 2, wherein the one or more agents suitable to suppress tungsten precipitation comprise at least one of organic oxygenate solvents, the stream comprising one or more saccharides, glycols, sugar alcohols, carboxylic acids, other products formed during the process, and mixtures thereof. ### Claim 4 (depends on 1) The method according to claim 1, wherein the one or more retro-aldol catalysts are removed from the reactor prior to or along with removal of the one or more agents suitable to suppress tungsten precipitation. ### Claim 5 (depends on 1) The method according claim 1, wherein the reactor temperature is lowered to less than 160° C. prior to the removing the one or more retro-aldol catalysts. ### Claim 6 (depends on 1) The method according to claim 1, wherein the stream comprising one or more saccharides continues to be fed to the reactor after the removal of the one or more retro-aldol catalysts. ### Claim 7 (depends on 1) The method according to claim 1, wherein the stream comprising one or more saccharides are selected from the group consisting of monosaccharides, disaccharides, oligosaccharides, polysaccharides, or a mix of these. ### Claim 8 (depends on 1) The method according to claim 1, wherein the one or more retro-aldol catalysts comprise at least one of silver tungstate, sodium metatungstate, sodium tungstate, ammonium metatungstate, sodium polytungstate, tungstic acid, alkali and alkaline earth metal tungstates, alkali and alkaline earth phosphotungstates, phosphotungstic acid, mixed tungstates and molybdates and silicotungstic acid. ### Claim 9 A shutdown process for the preparation of monoethylene glycol from a stream comprising one or more saccharides in the presence of hydrogen and a catalyst system comprising one or more tungsten based retro-aldol catalysts in a reactor comprising one or more catalytic species suitable for hydrogenation, said process comprising: a. reducing the reactor temperature to less than 160° C.; b. removing the one or more tungsten based retro-aldol catalysts from the reactor; and c. removing the one or more agents suitable to suppress tungsten precipitation from the reactor. ### Claim 10 (depends on 9) The process according to claim 9, wherein the removing of the one or more retro-aldol catalysts occurs after or concurrently with the reducing the reactor temperature. ### Claim 11 (depends on 9) The process according to claim 9, wherein the removing of the one or more retro-aldol catalysts occurs prior to or concurrently with removing the one or more agents suitable to suppress tungsten precipitation from the reactor. ### Claim 12 (depends on 9) The process according to claim 9, further comprising removing the one or more saccharides from the reactor after all the one or more tungsten based retro-aldol catalysts have been removed from the reactor. ### Claim 13 (depends on 12) The process according to claim 12, further comprising introducing water to the reactor to remove all of the organics from the reactor. ### Claim 14 (depends on 12) The process according to claim 12, wherein the introducing the water occurs concurrently with the removing the one or more saccharides from the reactor. ### Claim 15 (depends on 9) The process according to claim 9, wherein the one or more agents suitable to suppress tungsten precipitation comprise at least one of organic oxygenate solvents, glycols, sugar alcohols, or buffer systems comprising one or more organic acids, their corresponding conjugated bases with alkali-metal as their counterions, and mixtures thereof.