Method for combined production of 3-methyl-1,5-pentanediol and C1-C6 alcohols
A technology of pentanediol and methyl, which is applied in the field of preparation of 3-methyl-1,5-pentanediol, can solve problems such as difficult separation, harsh reaction conditions, equipment corrosion, etc., to overcome easy loss and avoid side effects Response, economical improvement effect
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Embodiment 1
[0080] Preparation of heteropoly acid catalyst (hollow molecular sieve supported heteropoly acid catalyst)
[0081] Configuration of tetrapropyl ammonium hydroxide aqueous solution (or simply "alkali solution"): configuration containing tetrapropyl ammonium hydroxide and NaNO with a concentration of 0.4mol / L respectively 3 Aqueous solution.
[0082] Preparation of hollow molecular sieve nanotubes: Take 1kg of pure silicon molecular sieve S-1 (Dalian Polytechnic Qiwangda Chemical Technology Co., Ltd.) with a particle diameter of 120nm, and place it in 5L of the alkali solution of the aforementioned configuration, and continuously stir at 150°C for 24h ; After filtering, wash with 10 times distilled water, then dry at 120°C and normal pressure for 2 hours, and calcinate at 450°C in air atmosphere for 4 hours.
[0083] Preparation of heteropoly acid aqueous solution: Na with a molar ratio of 12:1 2 WO 4 And Na 2 SiO 3 A total of 100g dissolved in 5L distilled water;
[0084] The preparat...
Embodiment 2
[0095] Ligand preparation
[0096] Add 50g of phosphorus trichloride to a reactor equipped with a circulating water condenser, dissolve 7.2g of 2-2'-biphenol powder in 50g of ethylene glycol dimethyl ether, and gradually add phosphorus trichloride in 30 minutes with stirring The reaction is carried out, and the reaction is continued for 1 h after the addition; the phosphorus trichloride and hydrogen chloride are removed by washing three times with 50 g of water each time, and the product solution is ready for use. Add 17.04g of 2,6-di-tert-butyl-4-methylphenol into a reactor equipped with a circulating water condenser. After heating and melting, the reaction temperature is controlled at 150~160℃ and N is passed through. 2 In bubbling operation, the product solution prepared above was gradually added dropwise to 2,6-di-tert-butyl-4-methylphenol under stirring for 1 hour, and the reaction was continued for 2 hours after the addition, and the hydrogen chloride was washed three times ...
Embodiment 3
[0099] The process and equipment of the hydroformylation reaction can be found in figure 1 Shown.
[0100] Add 10 g of the product (prenyl acetate) prepared in Example 1 into a 100 ml pressurized stirred reactor 5, the reaction temperature is 125°C, the synthesis gas pressure is 10 MPa, CO: H 2 Volume ratio=1:1, with 0.01gRh(CO) 2 (AcAc), 8g of the organophosphine ligand prepared in Example 2 (tetrakis (2,6-di-tert-butyl-4-methylbenzene)-2,2'-biphenyl diphosphite) as a catalyst, with 50ml of 3-methyl-1,5-pentanediol was used as a solvent and reacted for 24h. Sampling was sent to GC analysis, the conversion rate of isopentenol acetate was about 90%, and the selectivity of the reaction product 3-methyl-5-aldehyde-pentanol acetate was about 90%.
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