Diglyme synthesis

12synthesis methods

Product Name:Diglyme
CAS Number:111-96-6
Molecular formula:C6H14O3
Molecular Weight:134.17

265 g (2.5 mol) of diethylene glycol, 320 g (10.0 mol) of methanol, and 14.3 g (0.0125 equivalents) of NAFION 1100 EW Polymer (H+ form) were charged to a one-liter autoclave. After sealing and pressure testing, the contents of the autoclave were agitated, and the autoclave was pressurized to 100 psi with nitrogen. After 5 minutes of agitation, the autoclave was depressurized. This process was repeated two more times to ensure complete deoxygenation. After deoxygenation, the autoclave was heated to a temperature of 198 ℃, and the contents of the autoclave were agitated at 1900 rpm for 5 hours at temperature (198-200 ℃). A pressure of 810 psi was obtained. After 5 hours, the autoclave was cooled and sampled. By analysis, a total of 77.2% by weight of the diethylene glycol (1.93 moles) was converted in the reaction, producing 0.335 mol of Diglyme. The co-product includes 1,4 dioxane and the intermediate diethylene glycol monomethyl ether. Diethylene Glycol Dimethyl Ether

553-90-2 Synthesis

553-90-2
331 suppliers
$10.00/5g

96-35-5 Synthesis

96-35-5
336 suppliers
$5.00/5g

111-96-6
517 suppliers
$16.00/25mL

Yield:-

Reaction Conditions:

with hydrogen in methanol at 200 - 350; under 750.075 - 15001.5 Torr; for 4 h;Temperature;

Steps:

3

General procedure: Cu(NO3)2 was formulated with 0.3 mol/L aqueous solution with deionized water, a solution of 157 ml of this solution was placed in a beaker, while stirring slowly add ammonia, the pH of the solution in the beaker was 9.5 to 10.5. weighed 12 g of silica was added to the above-mentioned beaker containing Cu(NO3)2 solution, in the 30 °C water bath stirring aging 4h, heated to 90 °C steamed ammonia, until the beaker solution has a pH of 7 to 8. the resulting precipitate was filtered and washed to a filtrate at a pH of about 7. the washed precipitate was dried at 120 °C for 12 h, 450 ° C calcination 4h, tablet crushing to 20 ~ 40 mesh, pre-reaction reduction to obtain catalyst A: 20 wt% Cu/silica. The above catalyst performance was evaluated in a continuous flowing gas solid phase reactor, The catalyst loading was 1.0g. using a pure hydrogen normal pressure 350 ° C reduction catalyst, flow rate of 100mL/min, the temperature is raised from room temperature to 350 ° C at a rate of 1 to 2 ° C/min, and keep 4h, down to the reaction temperature after the introduction of H2, a 15 wt.% DMO solution of methanol was poured into an advection pump. control the hydrogen ester ratio 150, The system pressure is 2.0 MPa, the reaction temperature was 200 ° C. chromatographic analysis raw materials dimethyl oxalate (DMO) and the product of methyl glycolate (MG), ethylene glycol (EG), ethanol (EO), 2-methoxyethylether (2-MEO), 1,2-propanediol (1,2POD), 1,2-butanediol (1,2BOD).The evaluation results of the catalyst performance are shown in Table 1. The catalyst preparation and evaluation procedure was the same as in Example 1, except that 12 g of silica was changed to 12 g of HZSM-5 to obtain catalyst D: 20 wt% Cu / ZSM-5. the evaluation results of the catalyst performance are shown in Table 1.

References:

CN105622418,2016,A Location in patent:Paragraph 0020; 0021; 0026; 0027

67-56-1 Synthesis