Purifying method of epoxypropane
A technology of propylene oxide and purification method, applied in chemical instruments and methods, inorganic chemistry, organic chemistry and other directions, can solve the problem of high energy consumption in distillation process, difficult to reduce acetaldehyde content, and no impurity content in propylene oxide is given. and other problems to achieve the effect of enhancing the adsorption performance
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Embodiment 1
[0031] Embodiment 1: Preparation of modified zeolite molecular sieve
[0032] (1) Preparation of ZSM-5 zeolite
[0033] ZSM-5 zeolite is prepared by traditional hydrothermal synthesis method: industrial aluminum sulfate, deionized water, sulfuric acid, sodium chloride, water glass and n-butylamine (NBA) solution are mixed and stirred evenly to obtain a gel, and the Al in the gel 2 o 3 : SiO 2 : Na 2 O: H 2 The molar ratio of O:NBA was 1:30:1.5:1000:10; then the gel was moved to a hydrothermal synthesis kettle with polytetrafluoroethylene, and crystallized at a temperature of 170°C for 48h. The crystallized product was filtered, fully washed, dried in air atmosphere at 110°C for 12 hours, and calcined in air atmosphere at 550°C for 3 hours to obtain nanometer ZSM-5 zeolite.
[0034] (2) Preparation of Y zeolite
[0035] Y zeolite is prepared by traditional hydrothermal synthesis method: the directing agent, water glass, deionized water, aluminum sulfate and sodium alumina...
Embodiment 2
[0044] Embodiment 2: prepare the preparation of the propylene oxide that contains aldehydes impurity
[0045] The raw material propylene, hydrogen peroxide and solvent methanol are continuously fed from bottom to top into a fixed-bed reaction device equipped with titanium silicalite molecular sieves. The raw material propylene, hydrogen peroxide and solvent methanol are prepared according to the molar ratio of 3:1:4.5, the fixed bed reaction temperature is 40°C, and the reaction pressure is 3.0MPa. The reactor outlet product contains impurities such as unreacted raw material propylene, solvent methanol, product propylene oxide and methyl formate, acetone and acetaldehyde. Above-mentioned product separates solvent methanol and unreacted raw material propylene by processes such as rectification, condensation, is after extracting rectification with water again, application gas chromatographic analysis learns that the content of acetaldehyde in the crude propylene oxide is 166ppm....
Embodiment 3
[0046] Embodiment 3: the propylene oxide that contains acetaldehyde impurity that purification embodiment 2 obtains
[0047] A method for purifying propylene oxide, comprising the following steps: 6 kinds of zeolites prepared in Example 1 are respectively placed in stainless steel tubular reactors (φ120mm × 1000mm) of 6 fixed-bed reactors, and fixed The temperature in the bed reaction device is adjusted to 30°C and the pressure is adjusted to 0.5Mpa; the propylene oxide containing acetaldehyde impurity obtained in Example 2 enters the reaction bed of the fixed bed reaction device from bottom to top in the form of liquid phase, Its airspeed LHSV is 3.0h -1 After 120 min, the sample was collected, and the content of acetaldehyde in the purified sample was analyzed by gas chromatography. The experimental results are shown in Table 1.
[0048] Table 1: Purification results of propylene oxide containing acetaldehyde impurity in liquid phase
[0049] Adsorbent
[0050] I...
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