Methods for preparing catalyst precursor materials
A reagent and solvent technology, applied in the field of catalyst precursor material preparation, can solve the problems of batch purity change, production difficulty, thermal instability, etc.
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[0065] The embodiments are further illustrated by the following examples.
example 1
[0067] A first reagent feed tank was charged with 187 grams (g) of dichlorodiisopropylsilane (DCDIS), 388 g of bromochloromethane (BCM), and 1,781 g of tetrahydrofuran (THF) under nitrogen (N 2 ) layer under the mix. The first reagent feed tank is connected to the precooler by piping. 800 milliliters (mL) of 1.6 molar (M) hexane were introduced into the tubing. A vacuum pushes the contents of the tubing across the first heat exchanger (ie, a coil submerged in a bath filled with dry ice and acetone) and into the precooler at a flow rate of 1.2 mL per minute (1.2 mL / min). Once the contents of the tubes were introduced into the precooler, the agitator in the precooler started mixing its contents at 740 revolutions per minute (rpm). After the precooler has reached its desired capacity, its contents are introduced into the reaction zone through additional piping which fluidly connects the precooler and the reaction zone.
[0068] Once the pre-cooler started to flow into the reac...
example 2
[0082] The first reagent stream was generated by precooling a mixture of chloroiodomethane (CIM) and THF to -50°C. Simultaneously, a second reagent stream of 2.5M n-butyllithium in hexane was pre-cooled to -50°C. Pre-cooling is achieved by a separate heat exchanger (i.e., the pipe is inserted into a circulating bath with cooling silicone oil) and deposited into the first reaction zone where the mixture is mixed before being discharged into the second reaction zone. The reaction zone lasts 0.15 seconds to 0.3 seconds. The third reagent stream containing DCDIS and THF was pre-cooled to -50°C with a heat exchanger. The third reagent stream is then discharged to a second reaction zone where its contents mix with the contents of the first reaction zone.
[0083] Conditions for the continuous synthesis of catalyst precursor materials are provided in Table 3:
[0084] table 3
[0085] parameter value Residence time in the first reaction zone 0.15 seconds to 0.3...
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