Preparation method and application of Cu-MOF catalyst in acetylene hydrochlorination reaction
A technology of acetylene hydrochlorination and catalyst, which is applied in the direction of catalyst activation/preparation, organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, etc. It can solve the problem of poor conversion rate of acetylene and poor catalyst stability, etc. problems, to achieve huge energy and economic benefits, good stability, and mild conditions
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[0038] Example 1
[0039] (1) Synthesis of UIO-67: 90 mg of 4,4'-biphenylene terephthalic acid, 67mg ZrCl 4 50 ml of polytetrafluoroethylene (PPL) lining was added, then 15 mL N, N-dimethylformamide (DMF) and 3 ml of acetic acid were added. After the ultrasonic dissolution, the PPL lining is placed in a stainless steel reaction vessel, sealed and heated to 120 ° C, reacted 24 h, naturally cooled to room temperature. The resulting precipitate, centrifugation was separated, washed multiple times with DMF, and after multiple solvent exchanged with acetone, dried at 120 ° C to obtain a UIO-67 material.
[0040] (2) Preparation of Catalyst Cu-UiO-67: Take the UIO-67 purified in 20G step (1) to the container. Add 1.53g Cu (BF 4 ) 2 And 10 ml of acetonitrile dip, stirred for 2 hours, centrifugally, remove the supernatant, dry dry 10 hours at 120 ° C, then perform glow discharge treatment, the vacuum pump retention system using power is 500 W is in a vacuum state, by adjusting the air flo...
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[0042] Example 2
[0043] (1) To. 1.
[0044] (2) Preparation of Catalyst Cu-UiO-67: Take the UIO-67 in 20G Step (1) to add to the vessel. Add 4.76G Cu (BF 4 ) 2 And 15 ml of acetonitrile, stirred for 2 hours, centrifugation, remove the supernatant, 150 ° C for 10 hours, then the glow discharge treatment is performed, the vacuum pump is used to maintain the system in a vacuum state, by adjusting the air flow to make plasma The pressure of the body chamber is maintained at 100 PA, and the plasma treatment strength is adjusted by adjusting the discharge voltage value, and the applied voltage is 100 V, the treatment time is 1.5 h. The Cu-UIO-67 catalyst having a Cu (II) load is 6.42 wt% can be obtained.
[0045] (3) Tested, the catalyst was applied to acetylene hydrochlorination reaction in the fixed bed reactor, and at the reaction conditions: temperature 120 ° C, reaction pressure 0.01 MPa, N (HCl): N (c 2 Hide 2 ) = 1: 1, acetylene air speed 30h -1 . In the early stage of the reac...
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[0046] Example 3
[0047] (1) To. 1.
[0048] (2) Preparation of Catalyst Cu-UiO-67: Take the UIO-67 in 20G Step (1) to add to the vessel. Add 3.45 g of Cucl concentration of 45 wt% 2 The tetrahydrofuran solution, stirred for 2 hours, centrifugally, remove the supernatant, dried at 160 ° C for 10 hours, then the glow discharge treatment is performed, and the vacuum pump hold system of 500 W is in a vacuum state, by adjusting the air flow to make the plasma The pressure of the chamber is maintained at 100 PA, and the plasma treatment strength is adjusted by adjusting the discharge voltage value, and the applied voltage is 120 V, and the treatment time is 1.5 h. The Cu-UIO-67 catalyst having a Cu (II) load is 3.70 wt% can be obtained.
[0049] (3) Tested, the catalyst was applied to acetylene hydrochlorination reaction in the fixed bed reactor, and at the reaction conditions: temperature 120 ° C, reaction pressure 0.01 MPa, N (HCl): N (c 2 Hide 2 ) = 1: 1, acetylene air speed 30h -1...
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