Method for preparing 1,6-hexandiol by hydrogenation of 1,6-adipic acid dimethyl ester
A technology of dimethyl adipate and hexanediol, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of organic compounds, etc., can solve the complex process, high requirements of hydrogenation reaction equipment, and high energy consumption And other issues
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Embodiment 1-2
[0016] Dissolve 148.12 grams of copper nitrate and 81.86 grams of zinc nitrate in distilled water to form a mixed salt solution. Dissolve 25.18 grams of aluminum hydroxide in distilled water to form a suspension solution. Under heating and stirring, use sodium hydroxide in an alkaline solution And, control the pH=7-8, while producing precipitation, after filtering and washing, drying at 120°C for 4 hours, calcining at 400°C for 4 hours, and forming. The catalyst is reduced in a hydrogen stream at 130-300°C for 4 hours before use to obtain a hydrogenation catalyst I containing three components of copper oxide, zinc oxide and aluminum oxide.
[0017] (1). Feed the raw material 1,6-dimethyl adipate into the mixer and mix with hydrogen. The flow of hydrogen is controlled by a mass flow meter. The molar ratio of hydrogen to dimethyl adipate is in the range See Table 1;
[0018] (2). After the reacted material in step (1) is preheated by the heat exchanger, it enters the reactor to cont...
Embodiment 3-4
[0022] Using the hydrogenation catalyst I prepared in Example 1-2, the preparation method of Example 1-2 and the conditions in Table 2 were used to prepare 1,6-hexanediol. The results are shown in Table 2.
[0023] Table 2 Reaction conditions and results (catalyst I)
[0024] Catalyst bed
Embodiment 5-6
[0026] Dissolve 216.13 grams of copper nitrate and 361.38 grams of zinc nitrate in distilled water to form a mixed salt solution, and dissolve 45.28 grams of aluminum hydroxide in distilled water to form a suspension solution. Under heating and stirring, use sodium hydroxide in an alkaline solution Mix the salt solution and suspension, control pH=7-8, and produce precipitation at the same time, after filtering and washing, drying at 120°C for 4 hours, calcining at 400°C for 4 hours, and forming. The catalyst is reduced in a hydrogen stream at 130-300°C for 4 hours before use to obtain a catalyst hydrogenation catalyst II containing three components of copper oxide, zinc oxide and aluminum oxide.
[0027] (1). Feed the raw material 1,6-dimethyl adipate into a mixer and mix with hydrogen. The flow of hydrogen is controlled by a mass flow meter. The molar ratio of hydrogen to dimethyl adipate is in the range See Table 3;
[0028] (2). The reacted materials in step (1) are preheated b...
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