Method and system for preparation of glycerin alkyl ether
A technology of glycerin alkyl ether and glycerin, which is applied in the field of preparation of glycerin alkyl ether, can solve the problems of long reaction time, reduced catalyst life, catalyst deactivation, etc., and achieves the effects of lowering reaction temperature, controlling selectivity, and reducing residence time
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[0040] The reaction system for preparing glycerol alkyl ether provided by the present invention, the preferred embodiment includes: glycerin storage tank (1), tert-butanol storage tank (2), mixing tank (3), isobutylene storage tank (4), fixed bed reaction device (5), reaction product storage tank (6), evaporator (7), gas compression liquefaction system (8), evaporator (9), condenser (10), evaporator (11), isobutylene dimer storage Tank (12), water tank (13), water washing tower (14), phase separation tank (15), evaporator (16), evaporator (17), polyether product storage tank (18), condenser (19) , the line (20) used to transport raw glycerin from the glycerol storage tank (1) to the mixing tank (3), the line used to transport tert-butanol from the tert-butanol storage tank (2) to the mixing tank (3) (21), for the pipeline (22) that glycerol and tert-butanol mixture is transported from the mixing tank (3) to the fixed bed reactor (5), for transporting isobutylene from the isobu...
Embodiment 1
[0057] 10.0 g of macroporous sulfonic acid catalyst KC111 agent (Hebei Kairui Chemical Co., Ltd.) was filled in the fixed-bed reactor on the high-pressure micro-reactor test device. Preparation of glycerin feed: tert-butanol added to glycerol at a ratio of n-tert-butanol: n-glycerol = 1:2 to obtain a glycerol / tert-butanol solution with greatly improved fluidity.
[0058] (1) Response:
[0059]Fixed bed KC111 agent 10.0g (layer height 22cm), glycerol / tert-butanol solution feed rate 0.28ml / min (n tert-butanol: n glycerin = 1:2); liquid isobutene feed rate 0.64ml / min (n Isobutene: n glycerol = 4:1), the residence time is 1.0 h, the reactor temperature is 80° C., and the nitrogen back pressure is 2.0 MPa.
[0060] Test results: the conversion rate of glycerol is 100.00%; the selectivity of monosubstituted glycerol alkyl ether is 4.92%, the selectivity of polysubstituted glycerol alkyl ether is 95.08% (the selectivity of disubstituted glycerol alkyl ether is 77.99%, The selectivi...
Embodiment 2
[0067] 10.0 g of macroporous sulfonic acid catalyst KC111 agent (Hebei Kairui Chemical Co., Ltd.) was filled in the fixed-bed reactor on the high-pressure micro-reactor test device. Preparation of glycerin feed: Add tert-butanol to glycerin at a ratio of n-tert-butanol:n-glycerin=1:2 to obtain a glycerin / tert-butanol solution with greatly improved fluidity.
[0068] (1) Reaction: In fixed bed KC111 agent 10.0g (layer height 22cm), glycerol / tert-butanol solution feed rate 0.11ml / min (n tert-butanol: n glycerol=1:2); liquid isobutene feed rate 0.27ml / min (n isobutene: n glycerol = 4:1), the residence time is 2.5h, the reactor temperature is 70°C, and the nitrogen back pressure is 2.0MPa.
[0069] Test results: the conversion rate of glycerol is 100.00%, the selectivity of monosubstituted glycerol alkyl ether is 3.01%, the selectivity of polysubstituted glycerol alkyl ether is 96.99% (the selectivity of disubstituted glycerol alkyl ether is 72.92%, the selectivity of trisubstitut...
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