A kind of method that modified l-type molecular sieve catalyzes the chlorination of glycerol to prepare dichloropropanol
A technique for catalyzing glycerin and dichloropropanol with molecular sieves, which is applied in molecular sieve catalysts, chemical instruments and methods, and the preparation of halogens, etc., to achieve the effects of high conversion rate of raw materials, mild reaction conditions, and good stability
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Embodiment 1
[0026] (1) Preparation of modified L-type molecular sieve: 65.9gKOH and 17.31gAl(OH) 3 React in 220.9mL of deionized water at 120°C for 3 hours to obtain an alkaline solution of potassium metaaluminate; mix water and silica sol at a ratio of 1:10 to form an aqueous silica sol solution; slowly add the alkaline solution of potassium metaaluminate dropwise to the silica sol In an aqueous solution, react at 35°C for 12h; put the mixture obtained above into a hydrothermal kettle, crystallize at 120°C for 96h, and dry to obtain a white solid powder; take 5g of the powder and add 37.5mL of 0.02mol L -1 La(NO 3 ) 3 Wash with aqueous solution for ion exchange reaction, dry and roast at 500°C for 5 hours; use 0.1mol L -1 NH 4 NO 3 Washed with aqueous solution, dried and calcined at 450°C for 5 hours to obtain modified L-type molecular sieve LaHL -5 , after the reaction, the product is filtered to recover the modified L-type molecular sieve catalyst, washed, dried and activated for ...
Embodiment 2
[0034] (1) The preparation of L type molecular sieve is with embodiment 1 step (1)
[0035] (2) glycerin chlorination reaction is with embodiment 1 step (2)
[0036] (3) Change the crystallization time in step (1) to 48h, 72h, and 120h to obtain the influence of L-type molecular sieve catalysts with different crystallization times on the glycerol chlorination process, as shown in Table 2.
[0037] Table 2 Effect of L-type molecular sieve catalysts with different crystallization times on the chlorination process of glycerin
[0038]
[0039] Note: 2-MCPD is 2-chloro-1,3-propanediol, 3-MCPD is 3-chloro-1,2-propanediol, 1,3-DCP is 1,3-dichloro-2-propanol, 2, 3-DCP is 2,3-dichloro-1-propanol.
[0040] It can be seen from Table 2 that the longer the crystallization time, the better the catalytic activity of the prepared L-type molecular sieve. Using L-type molecular sieve with a crystallization time of 120h as a catalyst, the yield of dichloropropanol is the highest, which is...
Embodiment 3
[0042] (1) The preparation of L type molecular sieve is with embodiment 1 step (1)
[0043] (2) glycerin chlorination reaction is with embodiment 1 step (2)
[0044] (3) Change the La(NO 3 ) 3 The dosage of the aqueous solution is 0, 15mL, and 75mL, and the effects of the L-type molecular sieve catalysts with different La loadings on the glycerol chlorination process are obtained, as shown in Table 3.
[0045] Table 3 Effect of L-type molecular sieve catalysts with different crystallization times on the chlorination process of glycerol
[0046]
[0047] Note: 2-MCPD is 2-chloro-1,3-propanediol, 3-MCPD is 3-chloro-1,2-propanediol, 1,3-DCP is 1,3-dichloro-2-propanol, 2, 3-DCP is 2,3-dichloro-1-propanol.
[0048] It can be seen from Table 3 that the catalytic activity of La-loaded L-type molecular sieves is higher than that of unloaded L-type molecular sieves, and the catalytic activity will also increase with the increase of loading, but it is not obvious. When the La lo...
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