Method for separation of cresol isomers by liquid phase adsorption
A technology of isomers and cresols, which is applied in the field of separation of para-isomers, can solve problems such as difficulty in obtaining high purity, and achieve the effect of improving adsorption and separation performance
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[0022] The preparation method of nano-scale X molecular sieve crystal grain spherical autopolymer of the present invention comprises the following steps:
[0023] (1) Silicon source, aluminum source, water and sodium hydroxide are SiO according to molar ratio 2 / Al 2 o 3 = 2 ~ 25, Na 2 O / Al 2 o 3 = 3 ~ 30, H 2 O / Al 2 o 3 = 100-500 ratio mixing, aging at 0-60°C for 1-72 hours to make a directing agent,
[0024] (2) Mix the inorganic base, potassium source, aluminum source, silicon source, the directing agent prepared in step (1) and water to form a molecular sieve synthesis system, and the molar ratio of each material is: SiO 2 / Al 2 o 3 =1.9~5.0, M 2 O / SiO 2 = 0.6 ~ 4.2, H 2 O / SiO 2 =40~120,K + / (K + +Na + )=0.05~0.95, wherein M is K and Na, Al in the added directing agent 2 o 3 The amount and the total Al in the molecular sieve synthesis system 2 o 3 The molar ratio is 0.01% to 20%,
[0025] (3) The molecular sieve synthesis system in step (2) is hydroth...
example 1
[0054] Prepare the spherical self-aggregation of nano-scale X molecular sieve crystal grains described in the present invention.
[0055] (1) Preparation of directing agent
[0056] With 4.02kg sodium hydroxide, 7.81kg deionized water, 5.32kg low alkalinity sodium metaaluminate solution (Al 2 o 3 The content is 9.99% by mass, Na 2 O content is 10.93 mass %) and 23.24kg water glass (SiO 2 The concentration is 0.2017g / g, Na 2 O concentration is 0.0632g / g) was added into the reaction kettle, stirred and mixed evenly, left to age at 35°C for 24 hours to obtain the directing agent. The molar ratio of each material in the directing agent is SiO 2 / Al 2 o 3 =15,Na 2 O / Al 2 o 3 =16,H 2 O / Al 2 o 3 =320.
[0057] (2) Preparation of X molecular sieve grain spherical autopolymer
[0058] With 2.46kg sodium hydroxide, 4.15kg potassium hydroxide, 56.90kg deionized water, 31.48kg low alkalinity sodium metaaluminate solution (Al 2 o 3 The content is 9.99% by mass, Na 2 O con...
example 2
[0062] Prepare the sorbent.
[0063] (1) Rolling ball forming: take 92 kg (basis weight, the same below) of the powdered X molecular sieve spherical autopolymer a prepared in Example 1 and mix evenly with 8 kg of kaolin, put it into the turntable and spray an appropriate amount of it while rolling. Ionized water makes the solid powder gather into small balls, and the amount of water sprayed into when rolling the ball is 8% by mass of the solid powder. After sieving, pellets with a particle size of 300-850 μm were taken, dried at 80° C. for 10 hours, and calcined at 540° C. for 4 hours.
[0064] (2) In-situ crystallization: 64 kilograms of pellets calcined in step (1) are placed in 200 liters of sodium hydroxide and potassium hydroxide mixed solution, and the hydroxide ion concentration in the mixed solution is 0.3mol / L, K / (Na+K) molar ratio is 0.2, in-situ crystallization treatment at 95°C for 4 hours, the crystallized solid is washed with water until the pH of the washing s...
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