| 91%Chromat. |
With hydrogen; at 220℃; under 150015 Torr; for 12h; |
In a 0.31-stirring autoclav, 100 ml adipodimethylester was reacted at catalyst 1. The mixture was stirred for 12 hours at a hydrogen pressure of 2·107 Pa (200 bar) and a temperature of 220 C. A conversion of 98% and a yield with respect to hexandiol of 91% based on the introduced amount of adipodimethylester was determined by a gaschromatic analysis of the obtained product. |
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With hydrogen;catalyst having composition of 58percent CuO/22percent Al2O3/5percent La2O3/15percent Cu; at 210℃; under 150015 Torr; for 168h;Product distribution / selectivity; |
Example 6; Hydrogenation of Methyl Adipate Over Catalysts 1, 2, 3, 4 or 5; <strong>[627-93-0]Dimethyl adipate</strong> was hydrogenated continuously in trickle mode with recycling (feed/recycle ratio=10/1) at an hourly space velocity of 0.3 kg/(l*h), a pressure of 200 bar and reaction temperatures of 210 bar and 190 C. in a vertical tubular reactor which had been charged in each case with 200 ml of catalysts 1, 2, 3, 4 or 5. The experimental duration was a total of 7 days. GC analysis detected, in the reactor effluent at 190 C., ester conversions of 99.9%, a hexanediol selectivity of 97.5%. After deinstallation, the catalyst was still fully preserved and had a high mechanical stability. The experimental results are compiled in Table 1.The data in Table 1 which follows show that the inventive catalysts have significantly higher hydrogenation activities, i.e. higher conversions of <strong>[627-93-0]dimethyl adipate</strong> at 190 C. than the comparative catalyst, and also higher product-of-value selectivities, i.e. contents of the hexanediol target products in the effluent. |
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With hydrogen;catalyst T4489 (60percent CuO/30percent Al2O3/10 MnO2), steam treated; at 190℃; under 150015 Torr; for 168h;Product distribution / selectivity; |
Example 6; Hydrogenation of Methyl Adipate Over Catalysts 1, 2, 3, 4 or 5; <strong>[627-93-0]Dimethyl adipate</strong> was hydrogenated continuously in trickle mode with recycling (feed/recycle ratio=10/1) at an hourly space velocity of 0.3 kg/(l*h), a pressure of 200 bar and reaction temperatures of 210 bar and 190 C. in a vertical tubular reactor which had been charged in each case with 200 ml of catalysts 1, 2, 3, 4 or 5. The experimental duration was a total of 7 days. GC analysis detected, in the reactor effluent at 190 C., ester conversions of 99.9%, a hexanediol selectivity of 97.5%. After deinstallation, the catalyst was still fully preserved and had a high mechanical stability. The experimental results are compiled in Table 1.The data in Table 1 which follows show that the inventive catalysts have significantly higher hydrogenation activities, i.e. higher conversions of <strong>[627-93-0]dimethyl adipate</strong> at 190 C. than the comparative catalyst, and also higher product-of-value selectivities, i.e. contents of the hexanediol target products in the effluent. |
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With hydrogen;catalyst T4489 (60percent CuO/30percent Al2O3/10 MnO2); at 190℃; under 150015 Torr; for 168h;Product distribution / selectivity; |
Example 6; Hydrogenation of Methyl Adipate Over Catalysts 1, 2, 3, 4 or 5; <strong>[627-93-0]Dimethyl adipate</strong> was hydrogenated continuously in trickle mode with recycling (feed/recycle ratio=10/1) at an hourly space velocity of 0.3 kg/(l*h), a pressure of 200 bar and reaction temperatures of 210 bar and 190 C. in a vertical tubular reactor which had been charged in each case with 200 ml of catalysts 1, 2, 3, 4 or 5. The experimental duration was a total of 7 days. GC analysis detected, in the reactor effluent at 190 C., ester conversions of 99.9%, a hexanediol selectivity of 97.5%. After deinstallation, the catalyst was still fully preserved and had a high mechanical stability. The experimental results are compiled in Table 1.The data in Table 1 which follows show that the inventive catalysts have significantly higher hydrogenation activities, i.e. higher conversions of <strong>[627-93-0]dimethyl adipate</strong> at 190 C. than the comparative catalyst, and also higher product-of-value selectivities, i.e. contents of the hexanediol target products in the effluent. |
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With hydrogen;catalyst having composition of 58percent CuO/22percent Al2O3/5percent La2O3/15percent Cu, steam treated; at 210℃; under 150015 Torr; for 168h;Product distribution / selectivity; |
Example 6; Hydrogenation of Methyl Adipate Over Catalysts 1, 2, 3, 4 or 5; <strong>[627-93-0]Dimethyl adipate</strong> was hydrogenated continuously in trickle mode with recycling (feed/recycle ratio=10/1) at an hourly space velocity of 0.3 kg/(l*h), a pressure of 200 bar and reaction temperatures of 210 bar and 190 C. in a vertical tubular reactor which had been charged in each case with 200 ml of catalysts 1, 2, 3, 4 or 5. The experimental duration was a total of 7 days. GC analysis detected, in the reactor effluent at 190 C., ester conversions of 99.9%, a hexanediol selectivity of 97.5%. After deinstallation, the catalyst was still fully preserved and had a high mechanical stability. The experimental results are compiled in Table 1.The data in Table 1 which follows show that the inventive catalysts have significantly higher hydrogenation activities, i.e. higher conversions of <strong>[627-93-0]dimethyl adipate</strong> at 190 C. than the comparative catalyst, and also higher product-of-value selectivities, i.e. contents of the hexanediol target products in the effluent. |
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With hydrogen;catalyst having composition of 58percent CuO/22percent Al2O3/5percent La2O3/15percent Cu, water treated; at 210℃; under 150015 Torr; for 168h;Product distribution / selectivity; |
Example 6; Hydrogenation of Methyl Adipate Over Catalysts 1, 2, 3, 4 or 5; <strong>[627-93-0]Dimethyl adipate</strong> was hydrogenated continuously in trickle mode with recycling (feed/recycle ratio=10/1) at an hourly space velocity of 0.3 kg/(l*h), a pressure of 200 bar and reaction temperatures of 210 bar and 190 C. in a vertical tubular reactor which had been charged in each case with 200 ml of catalysts 1, 2, 3, 4 or 5. The experimental duration was a total of 7 days. GC analysis detected, in the reactor effluent at 190 C., ester conversions of 99.9%, a hexanediol selectivity of 97.5%. After deinstallation, the catalyst was still fully preserved and had a high mechanical stability. The experimental results are compiled in Table 1.The data in Table 1 which follows show that the inventive catalysts have significantly higher hydrogenation activities, i.e. higher conversions of <strong>[627-93-0]dimethyl adipate</strong> at 190 C. than the comparative catalyst, and also higher product-of-value selectivities, i.e. contents of the hexanediol target products in the effluent. |
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With hydrogen;copper-comprising catalyst; at 195 - 210℃; under 45004.5 Torr;Product distribution / selectivity; |
Example 1; Adipic acid, obtainable as product of the oxidation of cyclohexanol/cyclohexanone by means of nitric acid, having a content of 4 ppm of nitrogen is esterified by means of an acidic ion exchanger as catalyst (Amberlite IR 120) and methanol to form <strong>[627-93-0]dimethyl adipate</strong>. After complete esterification and removal of the ion exchanger and excess methanol, the ester is distilled (18 mbar, boiling point: 115 C.) and obtained in a purity of 99.98%. The nitrogen (N) content of the ester was 4 ppm. The <strong>[627-93-0]dimethyl adipate</strong> is hydrogenated in the gas phase at 60 bar and 195-210 C. over a copper-comprising catalyst. The space velocity over the catalyst is 0.15 kg of ester feed/liter of catalyst per hour. The reactor is a shaft reactor preceded by a vaporizer in which the feed stream is vaporized at about 195 C. with the aid of a stream of hydrogen gas. The stream of hydrogen gas is composed of fresh gas (4.5 mol/mol of <strong>[627-93-0]dimethyl adipate</strong>) and a recycle gas stream (about 80 mol of hydrogen/mol of feed stream). Downstream of the reactor, the gaseous mixture is cooled and liquid products are taken off. The gaseous output is recirculated by means of a recycle gas compressor. A small part of the gas stream is discharged as offgas. The <strong>[627-93-0]dimethyl adipate</strong> conversion is about 99.9%. A little methanol was lost via the offgas stream. The collected outputs (about 30% by weight of methanol, about 68% by weight of 1,6-hexanediol, about 0.5% by weight of methyl 6-hydroxycaproate and 0.06% by weight of hexanediol ester of 6-hydroxycaproic acid, about 0.3% by weight of hexanol, 0.1% by weight of <strong>[627-93-0]dimethyl adipate</strong>, balance in each case below 0.1% by weight) have an N content of 5 ppm and are worked up by distillation. Here, predominantly methanol is removed at temperatures at the bottom of up to 140 C. and pressures of from 1013 mbar absolute to 100 mbar over a period of one hour. The remaining bottoms (about 0.08% by weight of 1,6-hexanediol methyl adipate, 0.02% by weight of the di-1,6-hexanediol ester of adipic acid, 0.3% by weight of the 1,6-hexanediol ester of 6-hydroxycaproic acid) is fractionally distilled batchwise in a distillation column (1 m packed column, reflux ratio 5, no entry of air) at 100 mbar absolute and temperatures at the bottom of about 185 C. over a period of two hours. After removal of low boilers such as residual methanol and hexanol, 1,6-hexanediol is obtained in a distillation yield of about 90% with a purity of 99.9% and an N content of 1 ppm. The N content in the remaining bottom is 15 ppm. |
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With hydrogen; at 210℃; under 60006 Torr; |
The overhead product, which had been distilled under reduced pressure in Example 2, was subjected to a hydrogenation reaction as a starting material. The hydrogenation catalyst isCuZnAlNi catalyst. The CuO content was 30%, the content of ZnO was 63%, the Al2O3 content was 5% and the NiO content was 2%. Hydrogenation tower reaction conditions, reaction temperature 180 ~ 210 , reaction pressure 6-10MPa, liquid space velocity 0.2 ~ 0.75h-1, hydrogen oil volume ratio of 600 ~ 1200: 1. Table 2 below shows the results of hydrogenation of <strong>[627-93-0]dimethyl adipate</strong>. |
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With hydrogen; In methanol; at 225 - 250℃; under 15001.5 - 37503.8 Torr; for 9h; |
The prepared <strong>[627-93-0]dimethyl adipate</strong> and methanol are mixed in a ratio of 1:4 in a ratio of 1:4, and the reaction mixture is shaken and placed in a reaction solution sample tank for use;S3, the hydrogenation reactor is vented with hydrogen:Adding a catalyst to the catalyst reaction column of the hydrogenation reactor, after installing the catalyst reaction column, turning on the power of the hydrogenation reactor, opening the pressure and flow controller, and evacuating the hydrogenation reactor at 120/min. Half an hour, and then adjust the pressure to 2MPa for 4 hours to check the airtightness of the hydrogenation reactor;S4, catalyst reduction:The reaction pressure of the hydrogenation reactor is adjusted to 2 MPa, the hydrogen flow rate is 200 /min, the reaction temperature is 250 C, and the catalyst is subjected to a reduction reaction for 5 hours;S5, reaction solution reaction:After the catalyst is reduced, the heating is turned off under the circulation of hydrogen. After the catalyst is cooled, the hydrogen is supplied at a hydrogen ester molar ratio of 200:1 to ensure a pressure of 4.7-5 MPa, and the reaction temperature is set to 225 C, and the heating is maintained and the temperature is kept at 50 C. Set, let the reactor start to raise the temperature to 225 C, after the temperature is reached, pass the peristaltic pump to send the reaction liquid obtained in S2 to the catalyst reaction column to carry out hydrogenation reaction to obtain hexanediol;S6, rectifying the prepared hexanediol:When the temperature reached 195 C or higher, 1,6-ethylene glycol was collected, the reflux ratio was 1:4, the purity of the collected hexanediol was 98.7%, and the unreacted raw materials and other by-products at a temperature of 195 C were collected. Recycling, collecting flow ratio is 1:1. |
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