Hydrocyanation method for ethylenically unsaturated organic compounds
An organic compound, hydrocyanation technology, applied in the field of hydrocyanation, can solve problems such as polluting equipment
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Embodiment 11
[0139] Embodiment 11) prepare Ni / TSTPP catalytic solution
[0140] will be 500cm 3 350 mmol of an aqueous solution of trisulfonated triphenylphosphine (TSTPP) sodium salt was added to a 1 liter round bottom glass flask equipped with a magnetic stir bar and an upward reflux condenser; the solution was degassed. Subsequently, under stirring and under argon flow, 21.40 g (78 mmol) of Ni(cyclooctadiene) were added 2 , then add 350cm 3 Pre-degassed o-xylene.
[0141] The mixture was heated at 45°C for 15 hours. After cooling, the two-phase system was separated by settling and the dark red aqueous phase was discharged. Through analysis and determination, its nickel content is 134mmol / kg. 2) Isomerization of 2-methyl-3-butenenitrile
[0142] The following ingredients were added to a 2 liter glass reactor flushed with hydrogen and stirred by a turbine:
[0143] 2-Methyl-3-butenenitrile (2M3BN): 770g (9.50mol)
[0144] - Catalytic solution: 250cm 3 (39.5mmol Ni and 175.5mmol T...
Embodiment 2
[0153] will be 35cm 3 As in Example 1, the aqueous suspension described in §2 was added to 150 cm 3 In a glass reactor flushed with argon and equipped with an automatic suction turbine. While stirring (1200 rpm) at 50°C, 0.265 ml of hydrocyanic acid was injected into the reactor head space at a constant flow rate for 1 hour via a syringe thermostated at -10°C. After injecting HCN and returning to room temperature, the mixture was kept stirring in a closed vessel for 1 hour, then the headspace of the reactor was flushed with a flow of argon for about 1 hour. Through such treatment, a homogeneous aqueous solution is obtained: the solution has no obvious sediment after standing. For Millipore Millex-HV The sample that filter (Hydrophilic PVDF, 0.45 μ m) leaches adopts elemental analysis and polarization analysis to carry out quantitative measurement of total nickel and nickel (II) respectively, obtains following result: [Ni]=129mmol / kg and [Ni(II) )]=38mmol / kg([Ni 0 ]=91mm...
Embodiment 3
[0155] will be 35cm 3 As in Example 1, the aqueous suspension described in §2 was added to 150 cm 3 In a glass reactor flushed with argon and equipped with an automatic suction turbine. While stirring (1200 rpm) at 70°C, 0.265 ml of hydrocyanic acid was injected at a constant flow rate into the reactor headspace for 1 hour via a syringe thermostated at -10°C. After injecting HCN, returning to room temperature, the mixture was kept stirring in a closed vessel for 1 hour, and then, the headspace of the reactor was flushed with a flow of argon for about 1 hour. Through such treatment, a homogeneous aqueous solution is obtained: the solution has no obvious sediment after standing. For Millipore Millex-HV The sample that filter (Hydrophilic PVDF, 0.45 μm) leaches adopts elemental analysis and polarization analysis to carry out quantitative measurement of total nickel and nickel (II) respectively, obtains following result: [Ni]=122mmol / kg and [Ni(II) )]=30mmol / kg([Ni 0 ]=92mm...
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