1. for products that cannot be separated by distillation or thermal instability due azeotrope formation

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1 Purification of -CON in U Introduction 1.1 Application of melt crystallization Melt Crystallization in following cases: 1. for s that cannot be separated by distillation or thermal instability due azeotrope formation. to achieve an ultra high purity Condition: the must have a suitable pour point (U700: between 0 and 160 C). 1. Purification of -CON in U700 In U700, -CON with a purity of 85-88% by melt crystallization purified to 98% aqueous -CON.. Principle melt crystallization The melt crystallizer () consists of 64 tubes of 8 m long. It uses two films: 1. to purify the on the inside (tube side) of the tubes. oil on the outside (shell side). Melt Crystallization consists of the following three phases:.1 Formation of the crystal layer This phase happened in steps:.1.1 Nucleation: A limited amount pumped about crystallizer. The oil is very slowly cooled. Arise germs crystals (pure ) deposits on the inside of the pipes. This is called nucleation. Nucleation is highly sensitive step. If we bring too much on the column and is cooled too quickly, then crystallize the as a block and hit the pipes clogged..1. Grow the crystal layer After a first layer of pure was deposited, in allowing the oil to cool further and a larger amount of pumped. The crystal layer grows layer by layer. The oil must be continually cooled, and this for two reasons: 1

2 1. The thicker the layer, the larger the temperature gradient on the layer. The running pump -CON is always impure, causing its crystallization temperature decreases. After sufficient crystallization stops with one pump. Flows downward and the residue is released.. The oil is then very gradually increased. This diffusee residual impurities in the crystal layer outside. This is called sweating. The sweating- that contains impurities is drained off a bit remelted crystals..3 Melting After it heats the oil strongly. The crystal layer melts. This melts the purified. 3. Description -CON purification process in U700 The purification of -CON is a batch process. There is one or two work placements. An internship consists of crystallization, sweating and melting. They work in two stages, the collection of the end s of the initial stages, the power for the second stage (possibly a part-recyclable residue or sweating to get desired concentration). Since this power is cleaner than in the first stage, one needs less cooling and more heat to crystallize from sweating and melting Withdraw -CON : coumaranone or -CON (85-88% purity) with P700 from the vacuum container to melt the cockpit sucked C713, where the temperature at about 60 C regulated. The is then pumped through filter for F713A, F713B and after filter P713 pump, storage tank between the.

3 3.1. Stage Crystallization stage 1 -CON is pumped from to, bottom barrel with a steam coil (hot water). Stap1: (85%) (85%) is filled (with approximately 500 kg of -CON) and heated with hot water (± 60 C) to prevent the crystals formed in bulk or small quantities of already formed crystals smelten. The head of the head crystallization is heated in column with hot water in order to prevent crystals off and cause clogging of the inlet. The unfinished is placed on the crystallization column using pump. The column may not currently be at nucleation temperature or lower, as this one could cause premature crystallization (block crate all in ). Therefore, the first column is heated with hot oil (65 C) and then very gradually cooled to nucleation temperature (37 C). After a while germs arise crystals deposited on the wall (nucleation). Currently, a temperature rise of 3-5 C observed at the outlet of the column (crystallization heat) and a weight decrease of. 3

4 Step : First layer of pure 1 (85%) (± 68,7%) (± 35%) Then just about any is sent to the column. deflating. What remains in the column is a first layer deposition of pure. is filled (up to 1450 kg) with crude and also sweating and residue (crystallization phase) of the previous batch of [1]. The unfinished is something so dirty and this results in an initial concentration of 85 to 88% -CON is obtained. This is to always under constant conditions to work. is heated and the is circulated on for better heat distribution []. This is to prevent crystal formation in. 4

5 Step 3: of C713 Crystallow-up purified CON B707 B709 P709 Product is then sent over the column. Oil temperature gradually lowering. As the crystal layer grows, the oil temperature decrease for two reasons. First, the temperature gradient on the layer to overcome. And also because, by deposition of pure crystals, the running pump increasingly impure thereby widening its crystallization drops. During the crystallization decreases the weight of. We obtain a crystal layer of purified CON (97%) of residue and. The residue from the crystallization is released to B709. From there, most to the residue storage B707 and sent one last part to intermediate storage. 5

6 3.1.. stage 1 Step 4: Crystal layer being further purified CON Waste B707 B709 P709 The crystallization column is now very gradually heated. Leftover impurities in the crystal layer diffuse to the surface and flow away (this result with a little pure ). This process is called "sweating" mentioned. The sweating is collected in and B709 in drained (weighting) and then pumped to be (from storage). 6

7 Melting stage 1 Step 5: B705 1 End 3 End Product (purified CON) residue 5 B707 End Product (empty 4 6 B709 P709 The crystal layer is now using the molten column hot oil (65 C). The melt is circulated over the column for all to drag [1]. The added heat is used for the first crystal layer to melt (melting heat). The less it is melting, the heat delivered to the melt. When the temperature of the melt 60 C and the weight of is constant, it is insured that the entire crystal layer has been melted. Then the purified CON (97.6%) collected in to B709 and drained (more accurate weighting). [] Product of the previous batch of B705 to drained. [3] Then the finished pumped into B709 B705. [4] Below relieved to B709 (weighting). [5] Weighs B709 less than 500 kg, then no nd stage run (or re internships 1) and the end of the previous batch merged with the current end of B705. [6] There is thus proceeded, so that one individual quantities produced final can weigh in B709. If B709 weighs more than 500 kg after step [4] (see figure), then half done with the final placement of internship as a starting point for stage 7

8 3.. Stage 3..1 Crystallization stage Step 6: 3 5 B705 End stage 1 current batch 1 4 End last batch (1 stage) B707 B709 P709 6 Part of end of stage 1 (current batch) is released from B705 to [1]. B709, 500 kilograms of finished from the previous batch pumped to B705 (so the rest of the final stage of a batch of current) []. The end of an internship is circulated over the column crystallization [3]. Again the first column is heated with hot oil (65 C) and then very gradually cooled to the nucleation temperature (45 C). The nucleation temperature is higher than in the first stage, because the food is cleaner. After a while germs arise crystals deposited on the wall (nucleation). Currently, a temperature rise of 3-5 C observed at the outlet of the column (crystallization heat) and a weight decrease of. There is just no longer on the column sent. deflating. What remains is a first layer deposition of pure. The rest of the final (mixture of current and previous batch) from B705 to is relieved [4]. Product is then sent over the column [5]. Oil temperature gradually lowering. The crystallization temperature is higher than in the first stage, because the food is cleaner. We obtain a crystal layer of purified CON in and the residue is allowed to drain 8

9 into. Then the rest of the end of last batch of B709 to B705 pumped up empty B709 [6]. 3.. stage Step 7: Crystal Layer purified - CON B705 End stage 1 sweating stage Stage 1 stage B707 C B709 P709 The residue from the crystallization phase is drained to B709 [1] and from there pumped to C713 (with crude ) []. The crystallization column is very gradually heated (to 50 C). The sweating ( bit of pure impurities) will go into and B709 is released to [3] and pumped to B705 (at final stage 1) [4]. 9

10 3..3 Melting stage Step 8: 1 B705 End stage 1 sweating stage End stage Stage 1 B707 stage C713 3 End Stage B706 The crystal layer is melted by means of column hot oil (65 C). The melt is circulated over the column for all to drag [1]. The melt is then circulated on, so a sample can be taken []. Is the sample after analysis approved, the operator pushes the OK button and the end is relieved to end storage B706 [3]. 10

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