Zirconium sol, preparation method and applications thereof

Abstract

The invention relates to a zirconium sol, a preparation method and applications thereof, wherein the zirconium sol has a corrosion rate of not more than 1 g / m<2>.h, the pH value of 2.5-4, and the viscosity of more than 1000 mPa.s. The preparation method comprises: carrying out first contact on a zirconium-containing salt and an alkali solution, wherein a molar ratio of Zr to OH<-> is 1:1-2; carrying out second contact on the first contact mixture and an acid, wherein a molar ratio of Zr to H<+> is 1:1-3, and preferably the temperature of the first contact is 20-30 DEG C higher than the temperature of the second contact; and carrying out third contact on the second contact mixture and an acid, wherein a molar ratio of Zr to H<+> is 1:1-3. According to the present invention, the zirconium sol is used for preparing catalytic cracking catalysts, can improve the sphericity of the catalyst, and can improve the hydrocarbon oil cracking reaction effect of the catalyst.

Description

technical field

[0001] The invention relates to a preparation method of zirconium sol and its application in the preparation of fluid catalytic cracking (FCC) catalyst. Background technique

[0002] Fluid catalytic cracking (FCC) is the most important means of secondary processing of crude oil. The catalyst used in fluidized catalytic cracking must meet certain strength requirements, and at the same time form microsphere particles with a particle size of 20-150 microns and an average particle size of about 60-80 microns, in order to meet the normal flow and operation of the catalytic cracking catalyst in the reaction device . As the crude oil becomes heavier, the degree of heaviness and inferiority of the FCC feed increases, and the content of the active component molecular sieve in the FCC catalyst increases, which makes the wear index and sphericity of the catalyst a very important factor in the catalyst preparation process. question.

[0003] At present, FCC catalyst p...

Examples

Embodiment approach

[0055] One embodiment, in the step (1), the zirconium-containing salt is first contacted with the alkali solution at a temperature of T1, and T1 is a value between 50-80°C, preferably 55-75°C; in the step (2), at The mixture after the first contact is contacted with the acid for the second time at a temperature of T2, and T2 is a value between 20 to 50° C., preferably 25 to 45° C.; The obtained mixture is contacted with an acid for the third time, and T3 is a value between 20-50°C, preferably 25-45°C. T1-T2 (the difference between T1 and T2) is 20-30°C, and T1-T3 (the difference between T1 and T3) is 20-30°C. The temperature of the reactor can be controlled by heating and / or cooling, and using a constant temperature water bath, so that the temperature of the reactor in each step can be controlled at T1, T2 and T3 respectively. Control the deviation of fluctuations in T1, T2 and T3 not to exceed 10°C.

[0056] FCC catalyst (catalytic cracking catalyst) preparation method prov...

Embodiment 1

[0092] Add ZrOCl to the reaction kettle 2 ·8H 2 O 35.38Kg, then add concentration according to the ratio of Zr and sodium hydroxide molar ratio 1:1 under 60 ℃ of temperature and be the sodium hydroxide solution 9.77Kg of 45% by weight, then stir 60min at the temperature of 60 ℃, obtain after reaction The first contact object, and then at a temperature of 40 ° C according to Zr:H + =1:1.5 ratio, adding concentration is 19.41Kg of hydrochloric acid 31% by weight, then stirred at a temperature of 40°C for 60min to obtain the second contact, and then at a temperature of 40°C according to Zr:H + =1:1.5 ratio, adding 19.41Kg of hydrochloric acid with a concentration of 31wt% (wt% refers to weight%) to the second contact, and stirring at a temperature of 40°C for 60min to obtain the zirconium sol provided by the present invention. The preparation conditions and proportions are shown in Table 1, and the properties of the obtained zirconium sol are shown in Table 2.

Embodiment 2

[0094] With reference to the preparation method of Example 1, add ZrOCl in the reactor 2 ·8H 2 O, then add a sodium hydroxide solution with a concentration of 45wt%, stir, then add a concentration of 31wt% hydrochloric acid, stir, then add a concentration of 31wt% hydrochloric acid, stir, and obtain a zirconium sol. The preparation conditions and proportions are shown in Table 1, and the properties of the obtained zirconium sol are shown in Table 2.

technical field

[0001] The invention relates to a preparation method of zirconium sol and its application in the preparation of fluid catalytic cracking (FCC) catalyst. Background technique

[0002] Fluid catalytic cracking (FCC) is the most important means of secondary processing of crude oil. The catalyst used in fluidized catalytic cracking must meet certain strength requirements, and at the same time form microsphere particles with a particle size of 20-150 microns and an average particle size of about 60-80 microns, in order to meet the normal flow and operation of the catalytic cracking catalyst in the reaction device . As the crude oil becomes heavier, the degree of heaviness and inferiority of the FCC feed increases, and the content of the active component molecular sieve in the FCC catalyst increases, which makes the wear index and sphericity of the catalyst a very important factor in the catalyst preparation process. question.

[0003] At present, FCC catalyst p...

Examples

Embodiment approach

[0055] One embodiment, in the step (1), the zirconium-containing salt is first contacted with the alkali solution at a temperature of T1, and T1 is a value between 50-80°C, preferably 55-75°C; in the step (2), at The mixture after the first contact is contacted with the acid for the second time at a temperature of T2, and T2 is a value between 20 to 50° C., preferably 25 to 45° C.; The obtained mixture is contacted with an acid for the third time, and T3 is a value between 20-50°C, preferably 25-45°C. T1-T2 (the difference between T1 and T2) is 20-30°C, and T1-T3 (the difference between T1 and T3) is 20-30°C. The temperature of the reactor can be controlled by heating and / or cooling, and using a constant temperature water bath, so that the temperature of the reactor in each step can be controlled at T1, T2 and T3 respectively. Control the deviation of fluctuations in T1, T2 and T3 not to exceed 10°C.

[0056] FCC catalyst (catalytic cracking catalyst) preparation method prov...

Embodiment 1

[0092] Add ZrOCl to the reaction kettle 2 ·8H 2 O 35.38Kg, then add concentration according to the ratio of Zr and sodium hydroxide molar ratio 1:1 under 60 ℃ of temperature and be the sodium hydroxide solution 9.77Kg of 45% by weight, then stir 60min at the temperature of 60 ℃, obtain after reaction The first contact object, and then at a temperature of 40 ° C according to Zr:H + =1:1.5 ratio, adding concentration is 19.41Kg of hydrochloric acid 31% by weight, then stirred at a temperature of 40°C for 60min to obtain the second contact, and then at a temperature of 40°C according to Zr:H + =1:1.5 ratio, adding 19.41Kg of hydrochloric acid with a concentration of 31wt% (wt% refers to weight%) to the second contact, and stirring at a temperature of 40°C for 60min to obtain the zirconium sol provided by the present invention. The preparation conditions and proportions are shown in Table 1, and the properties of the obtained zirconium sol are shown in Table 2.

Embodiment 2

[0094] With reference to the preparation method of Example 1, add ZrOCl in the reactor 2 ·8H 2 O, then add a sodium hydroxide solution with a concentration of 45wt%, stir, then add a concentration of 31wt% hydrochloric acid, stir, then add a concentration of 31wt% hydrochloric acid, stir, and obtain a zirconium sol. The preparation conditions and proportions are shown in Table 1, and the properties of the obtained zirconium sol are shown in Table 2.

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