One-step method for synthesizing methyl lactate from biomass glycerol
A methyl lactate, biomass technology, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds and other directions, can solve the problems of no water agent, the effect of methyl lactate is not very good, etc., to achieve equipment corrosion Low, good industrialization prospects, the effect of low reaction temperature
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Embodiment 1
[0018] The gold palladium alloy catalyst (Au 2 PD 8 / HZSM) preparation: weigh 0.0083gHAuCl 4 4H 2 O, 0.0184g Pd(NO 3 ) 2 2H 2 O and 1g HZSM-5 molecular sieve, guarantee that the amount of the total substance that makes catalyst copper-palladium alloy is 0.0001mol at every turn; Will weigh HAuCl 4 4H 2 O, Pd(NO 3 ) 2 2H 2 O and HZSM-5 were added to 60mL of 5% polyvinylpyrrolidone (PVP) aqueous solution and ultrasonically treated for 15min to disperse completely. Heat for 15min, then weigh 2g of ascorbic acid and dissolve it in 50mL of water, add the solution dropwise to the reaction solution in the round bottom flask, react in the water bath for 2.5h, then lower the temperature of the water bath to room temperature, centrifuge the reaction product, and use After washing with absolute ethanol and vacuum drying, the desired catalyst can be obtained.
[0019] Weigh 4.6g glycerol (Sinopharm Chemical Reagent Co., Ltd.) in a 100mL volumetric flask, use methanol to constant...
Embodiment 2
[0027] Gold palladium alloy catalyst (Au 5 PD 5 / HZSM) preparation: preparation conditions and steps are the same as those of Au in Example 1 2 PD 8 / HZSM catalyst preparation method is the same, 0.0083g HAuCl 4 4H 2 O and 0.0184g Pd(NO 3 ) 2 2H 2 O was changed to 0.0206g HAuCl 4 4H 2 O and 0.0115g Pd(NO 3 ) 2 2H 2 O.
[0028] Weigh 4.6g glycerol (Sinopharm Chemical Reagent Co., Ltd.) in a 100mL volumetric flask, use methanol to constant volume, add it to a 300mL autoclave, then weigh 0.46g phosphotungstic acid (Sinopharm Chemical Reagent Co., Ltd.) and 0.074 wxya 5 PD 5 / HZSM, put into the autoclave together, evacuate with high-purity nitrogen, then seal the autoclave, stir at 300rpm, heat the autoclave to 130°C and start timing, react for 4h.
[0029] After the reaction, pipette 1 mL of the reaction solution and add 20 μL of n-butanol for gas chromatography analysis. According to the analysis, the conversion rate of glycerin was 100%, and the yield of methyl l...
Embodiment 3
[0037] The gold palladium alloy catalyst (Au 8 PD 2 / HZSM) preparation: preparation conditions and steps are the same as those of Au in Example 1 2 PD 8 / HZSM catalyst preparation method is the same, 0.0083g HAuCl 4 4H 2 O and 0.0184g Pd(NO 3 ) 2 2H 2 O was changed to 0.0330g HAuCl 4 4H 2 O and 0.0046g Pd(NO 3 ) 2 2H 2 O.
[0038] Weigh 4.6g glycerol (Sinopharm Chemical Reagent Co., Ltd.) in a 100mL volumetric flask, use methanol to constant volume, add it to a 300mL autoclave, then weigh 0.46g phosphotungstic acid (Sinopharm Chemical Reagent Co., Ltd.) and 0.074 wxya 8 PD 2 / HZSM, put into the autoclave together, evacuate with high-purity nitrogen, then seal the autoclave, stir at 300rpm, heat the autoclave to 130°C and start timing, react for 4h.
[0039] After the reaction, pipette 1 mL of the reaction solution and add 20 μL of n-butanol for gas chromatography analysis. According to the analysis, the conversion rate of glycerol was 98.8%, and the yield of met...
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