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5.3.3 Catalysts recovery (Units 17-22) After cooling down (unit 18) the reactor liquid product, the amine and catalysts can be recycled back to the reactor after the separation of the light phase in a decanter (unit 19). The pressure of the reactor liquid product is increased up to 130 bar (unit 17) in order to avoid a flashing of CO2 in the decanter (to ease the downstream liquid-liquid separation), which can thus be operated at a separation efficiency of 85 %: this means that 15 % of the light phase remains in the heavy phase. This separation factor is based on the operation ranges described in the patent [130], example B-3. As the catalysts are very expensive (see Appendix 1, Table 12), and to recover the maximum as possible, a second decanter is placed downstream (unit 22). This is operated at 70 bar, after a separation of flashing gases in a flash vessel (unit 21). In order to increase the catalysts recovery, the amount of amine is increased in unit 22 by adding the recycled amine stream from the purification stage (stream 39). In the model, a complete recovery of the catalysts is assumed in order to simplify the recycle calculations. As for costs purposes, it has been assumed that the catalysts are renewed once per year (see Chapter 6). 5.3.4 Methanol recovery (Units 23-26, 33 and 34) Methanol is recovered in a stripping column working at 3 bar (unit 26). Before feeding stream 29 to the column, light gases are separated at atmospheric pressure in a flash vessel (unit 24). This keeps the temperature in the condenser (unit 34) above the cooling water temperature. The purity of the bottom product from the stripping column (stream 33), is adjusted in order to fit the desired product purity of FA, approximately 85 wt % (stream 43). The top product, which contains methanol, water and dissolved CO2, is condensed and recycled back to the reactor (stream 32). The results from this step are checked with the values reported in [130], example D- 1a. In Appendix 2, Figure 25 shows the boiling point - dew point temperature curve for the binary mixture of methanol and amine of the separation occurring in the stripping column (unit 26). For costs purposes, it has been assumed that the methanol-based solvent is renewed once every ten years (see Chapter 6). 5.3.5 Formic acid formation and purification (Units 27-33) By reducing the pressure to 250 mbar and increasing the temperature to 180 °C, the dissociation of the adduct to FA and amine is initiated. This happens in a reactive distillation column where, additionally, the separation of the amine from the FA product is also taken place. For modelling purposes, the reaction and the separation happen in two separated unit operations. In an adiabatic reactor (unit 27), the adduct is decomposed into FA and amine, as follows: C18H39N HCOOHC18H39N HCOOH Eq. (14) The endothermal reaction leads to a temperature reduction from 175 °C (in stream 33) to 88 °C (in stream 34). This heat is added in the column (unit 28) in order to reach the bottom temperature of 180 °C, since this is where the reaction actually takes place. The separation of FA from the amine (in unit 28) is complex, as the mixture of FA, amine and methanol may form two liquid phases. In Appendix 2, Figure 26 shows the conditions under which the decomposition of the adduct occurs. At the conditions selected in unit 28, the decomposition into two liquids inside the column is avoided. The feeding stream (stream 34) has a FA concentration of 11 %, with 1 % of methanol, and 88 % of amine in mass basis. It forms two liquid phases. However, as most of the FA flashes at the top of the column, the liquid composition on the first tray is already outside the 3-phase region, with a composition of 3 % FA, 0.5 % methanol and 49PDF Image | evaluation of CO2 utilisation for fuel production
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