Method of synthesizing methyl glycolatedimer
A technology of methyl dimer glycolate and acid activity, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problems that the synthesis of methyl dimer glycolate cannot be realized in a good way. , to achieve the effect of low cost and low energy consumption
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[0021] The preparation methods of several typical catalysts are as follows:
[0022] H-MOR molecular sieve preparation: sodium aluminate (NaAlO 2 ) is an aluminum source for preparing mordenite molecular sieves, and the silicon-aluminum ratio (Si / Al) of the sol is 10-50. First, dissolve the metered amount of sodium aluminate in water, stir to form a transparent solution, add sodium hydroxide and continue stirring. Then add a measured amount of silica sol to the above solution under stirring, continue stirring for 30 minutes, then transfer the obtained uniform gel into a stainless steel reaction kettle with a PTFE liner, and crystallize in a constant temperature oven at 180°C under rotation. 20h. The crystallized samples were filtered and washed with deionized water until neutral. Sodium mordenite molecular sieves were obtained after drying overnight at 120°C. Add a certain concentration of NH to it 4 NO 3 The solution was exchanged at 80 °C for 10 h, filtered and washed....
Embodiment 1
[0027] Fill 10 g of different types of catalysts into the fixed-bed reactor (if the two catalysts are mixed and added, mix them uniformly according to the mass ratio of 1:1) for pretreatment. Catalyst pretreatment conditions are: N 2 The flow rate is 100mL / min, starting from 25°C and rising to 500°C over 150min, and maintaining at 500°C for 180min. Using methylal as raw material, a high-pressure constant-flow pump was used at a catalyst mass space velocity of 1 h -1 Pumped into the reactor, the CO flow rate was 2000 mL / min, the molar ratio of CO and DMM was 250:1, the reaction temperature was 260 °C, and the total reaction pressure was 5.0 MPa.
[0028] Methylal conversion rate is represented by DMM, DME represents dimethyl ether, MeOH represents methanol, MF represents methyl formate, MMAc represents methyl methoxyacetate, MG represents methyl glycolate, and DMG represents methyl diglycolate. The product selectivity is calculated according to the mass selectivity. From Tab...
Embodiment 2
[0032] 10 g of silicon-aluminum ratio Si / Al = 12.5 (H-MOR-(Cs+La) 0.1M +HMOR-Py) catalyst was filled into the fixed bed reactor for pretreatment. Catalyst pretreatment conditions are: N 2 The flow rate is 100mL / min, starting from 25°C and rising to 500°C over 150min, and maintaining at 500°C for 180min. Using methylal as raw material, the catalyst mass space velocity is 1h by a high pressure constant flow pump -1 Pumped into the reactor, the CO flow rate was 2000 mL / min, the molar ratios of CO and DMM were 100:1, 125:1, 150:1, 175:1, 200:1, 250:1, and the reaction temperature was 260 °C. The total reaction pressure is 5.0 MPa.
[0033] According to Table 2, under the same reaction temperature of 260 °C and reaction pressure (5.0 MPa), as the molar ratio of the reaction raw material CO to DMM gradually increased (from 100 / 1 to 250 / 1), dimer glycolic acid methyl The ester mass selectivity increased gradually (from 39% to 76%), and when the molar ratio of CO to DMM was 250:1,...
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