zro 2 Polycrystalline ceramic foam catalyst, its preparation method and its use
A foamed ceramic and catalyst technology, applied in physical/chemical process catalysts, ceramic products, chemical instruments and methods, etc., can solve the problem of inability to completely solve biodiesel acid reduction corrosion, emulsification and waste water pollution, immature process, complex preparation, etc. problems, to achieve the effect of ensuring long service life, avoiding corrosion, and preventing crystal transformation
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[0028] The present invention also provides a ZrO 2 The preparation method of polycrystalline foamed ceramic catalyst comprises:
[0029] Step by step ZrOCl 2 •8H 2 O, AlCl 3 and TiCl 4 (N zirconium: N aluminum: N titanium = 5: 2.2 ~ 3.5: 0.2) dissolved in deionized water to make a precipitation mother liquor with a concentration of 20 ~ 40%, and then containing 10 ~ 13g / L template agent (CTAB) and a certain The ethanol solution of concentrated urea (N urea: N zirconium oxychloride=1:1~3:1) is slowly added to the precipitation mother liquor, and at the same time, the mass fraction of 5~10% Y 2 o 3 concentrated nitric acid until the pH is 2-3, heated to 80-100°C under vigorous stirring, and kept for 12-24 hours. After the reaction, adjust the pH to 2-3 with dilute nitric acid, and crystallize at 40-60°C for 6-12 hours. After the crystallization is completed, vacuum filter and wash with deionized water until it does not contain Cl -1 , washed with absolute ethanol for 2 t...
Embodiment 1
[0032] Add biodiesel (acid value 20mg KOH / g) and biodiesel by-product glycerol (content 85%) into a 5L glass reactor at a mass ratio of 3:1, start the stirrer, set the speed at 350rpm / min, and weigh the oil Heavy 0.3% ZrO 2 The polycrystalline foam ceramic catalyst is slowly added into the reaction kettle. Turn on the vacuum pump, wait until the vacuum pressure of the device is stabilized at -0.1MPa, and after stirring evenly, set the temperature of the constant temperature oil bath to 220°C, turn on the low-temperature condensation device, until the temperature of the material in the reactor rises to 220°C, and stabilize the reaction for 6 hours. The catalyst was separated by centrifugation, and the obtained product was allowed to stand and separate into layers. The acid value of the upper methyl ester layer was measured to be 0.3 mg KOH / g, and the esterification rate was 98.5%. The light yellow liquid in the upper layer then enters the vacuum rectification device to separat...
Embodiment 2
[0034] Add biodiesel (acid value 20mg KOH / g) and biodiesel by-product glycerol (content 85%) into a 5L glass reactor at a mass ratio of 4:1, start the stirrer, set the speed at 500rpm / min, and weigh the oil Heavy 1.0% ZrO 2 The polycrystalline foam ceramic catalyst is slowly added into the reaction kettle. Turn on the vacuum pump, wait until the vacuum pressure of the device is stabilized at -0.1MPa, and after stirring evenly, set the temperature of the constant temperature oil bath to 220°C, turn on the low-temperature condensation device, until the temperature of the material in the reactor rises to 220°C, and stabilize the reaction for 6 hours. The catalyst was separated by centrifugation, and the obtained product was allowed to stand and separate into layers. The acid value of the upper methyl ester layer was measured to be 0.1 mg KOH / g, and the esterification rate was 99.5%. The light yellow liquid in the upper layer then enters the vacuum rectification device to separat...
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