Method for preparing epichlorohydrin and white carbon black by coupling process
A technology of epichlorohydrin and white carbon black, which is applied in the fields of silicon oxide, silicon dioxide, organic chemistry, etc.
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example 1
[0036] Example 1. Continuous operation in a tubular reactor
[0037] Dissolve adipic acid (catalyst) in 95% industrial glycerin (mass ratio) to prepare a 5% (mass ratio) industrial glycerin solution. Use a metering pump to press industrial glycerin containing catalyst into a tubular reactor with a total volume of 50L at a rate of 11.75kg / h. The tubular reactor is divided into two parts, the front part of which has a volume of 30L (DN40mm The tube is 24m long), and the reaction temperature is controlled at 70°C; the volume of the latter part of the tubular reactor is 20L (DN40mm tube, 16m), and the reaction temperature is controlled at 130°C.
[0038] With another metering pump, SiCl with a content of 98.5% (mass ratio) 4 Press into the above reactor at a rate of 8.5kg / h. SiCl 4 The molar ratio to glycerin is 2.3:1.0, SiCl 4 It enters the reactor in the way of multiple distribution. Among them, 50% enters the front part of the reactor in the form of three-way uniform dis...
example 2
[0042] Example 2. Tank Reactor Batch Operation
[0043] at a volume of 0.5 m 3Add 186kg of refined glycerin with a content of 99% in the external circulation reactor, add 10 kg of glacial acetic acid, close the feeding port, start the circulation pump, and press the SiCl with a metering pump at a rate of 35kg / h through the feed pipeline. 4 , the reaction temperature was controlled at 90°C by jacket water cooling. After 2 hours of reaction, the SiCl 4 The pumping rate was changed to 50kg / h, and the reaction temperature was controlled to be 120°C. This operation was continued for 2 hours, and a total of SiCl was pumped into 4 170kg, glycerin and SiCl 4 The molar ratio is 2:1, the operating pressure is 0.3~0.8MPa, and the total reaction time is 4 hours.
[0044] After the reaction is over, the reaction product is sent to a rotary drum suction filter through an external circulation pump, and the filter residue is washed with 30% dilute glycerin.
[0045] The filter residue ...
example 3
[0047] Example 3. Column Reactor Continuous Operation
[0048] Dissolve silicomomolybdic acid in 82% crude glycerin to make a 3% solution. Use a metering pump to press the crude glycerin containing catalyst into the tower reactor at a rate of 217kg / h. The tower reactor consists of two parts connected in series with an external circulation pump, the volume of the first tower is 0.4m 3 , the volume of the second tower is 0.6m 3 .
[0049] Use a metering pump to mix 98.5% SiCl 4 Press into the above-mentioned tower reactor at a rate of 170kg / h. Glycerin and SiCl 4 The molar ratio is 1.8:1. SiCl 4 It enters the tower reactor in the way of two distributions, in which 40% SiCl 4 Into the first tower reactor, the other will leave 60% SiCl 4 into the second tower reactor. The operating temperature of the first tower is controlled at 60°C and the operating pressure is 0.25~0.35MPa, and the operating temperature of the second tower is controlled at 110°C and the operating pr...
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