For the successful distillation of heat sensitive materials

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1 CTS CHEMTECH SERVICES, INC. Short Path Distillation Services Laboratory Tel: Cell: Fax: For the successful distillation of heat sensitive materials Distill from kg/hr Distillation temperatures to 400 C Distillation pressure to mmhg KDL Series - Short Path Distillation Systems for the Laboratory

2 Food Products Monoglycerides Palm Oil Tocopherols Fish Oil Rice Bran Oil Fatty Acids Seed Oils Diglycerides Butter Pharmaceuticals Acid Chlorides Amino-acid Esters Vitamin E Glucose Derivatives Indoles Terpene Esters Natural & Synthetic Vitamins Beta-carotene Chemicals Alcohols Glycol Ethers Herbicides Halogenated Hydrocarbons Insecticides Silicon Oils Tall-tan Oil Waxes Applications of Short Path Vacuum Distillation Plastics Acrylics Epoxy Resins Deoxidized Oils Isocyanates Phenolics Plasticizers Polyethylene Stabilizers Thermoplastic & Thermosetting Resins Mineral Oils Base Oil Bright Stock Lube Oils Paraffinic Oils Pitch, long & short chain Tar Cosmetics Wool fatty Acids Wool Alcohols Extracts from: Algae Broom Brown Moss, Flowers Roots, & Capsicum

3 Page Distilling Heat Sensitive Materials 1 Just the basics 3 KDL-4 4 KDL-4 High Vacuum 5 KDL-4 Pro 6 KDL-4 Pro Plus 7 KDL-4 Pro Gold 8 KDL-4 High Temp 9 KDL-4 High Temp Plus 10 KDL-4 Unjacketed Page 11 KDL-4 Electrically Heated 12 Key Operating Considerations 13 Order Guide 14 Just What You Asked For 15 Conditions of Sale 16 Table of Contents

4 Tempe rature ( C) The distillation of heat sensitive materials can be complicated; especially when the temperature at which distillation must be performed is high enough to cause thermal decomposition. Although the risk of thermal damage can be greatly reduced by distillation under vacuum, the duration of exposure to even moderate temperatures must also be considered. While, in most cases, the risk of thermal decomposition increases exponentially with temperature, it also increases linearly with the duration of thermal exposure. thermal decomposition no thermal decomposition Short path distillation addresses each of Pressure (mm Hg) these factors by permitting distillation at the lowest possible pressure with the shortest possible residence time. Unlike conventional "pot" distillation, the residence time of heat sensitive materials in short path distillation is limited to the time it takes the mixture being distilled to travel under force of gravity from the top to the bottom of the heated evaporator surface. Though this depends somewhat of the viscosity of the material being distilled, the residence time of heat sensitive materials in a KDL-4 short path distillation unit is generally less than 10 to 20 seconds. Distilling Heat Sensitive Materials As the material to be distilled (i.e., the feed stock) enters the evaporator of a KDL-4 short path distillation system, it is immediately distributed as a uniform thin film on the heated interior surface. As gravity draws the film downward, hot oil circulating through the surrounding jacket of the evaporator transfers enough heat to the thin film to cause more volatile components of the feed mixture to evaporate. Once liberated from the surface of the thin film in this way, the resulting vapors travel the short distance or "short path" to the internal condenser where they are returned to the liquid state and travel downward to be recovered as distillate. Meanwhile, remaining constituents of the film are agitated by three strands of rotating wiper rollers which serve to maintain film thickness and uniformity while aiding the diffusion of more volatile components to the surface of the film where their concentration has just been reduced by evaporation. All components of the mixture remaining in the film as it reaches the bottom of the heated evaporator surface are recovered as residue. At any given time, however, it is worth noting that only that portion of the original feed material comprising the thin film is and exposed to the temperature required to effect distillation. The rest of the feed material remains in the feed vessel. Also worth noting is the close proximity of the condenser to the heated evaporator surface. In more conventional wiped film or falling film distillation systems, limits to the pressure at which distillations can be performed are implicit in the pressure drop across the connection between the evaporator in which the concentration of vapors is high and the condenser in which the concentration of vapors is much lower. By locating the condenser internally, this pressure drop is minimized to the point where it can generally be disregarded. This, more than anything, is what makes KDL-4 short path distillation systems ideal for the distillation of heat sensitive materials at pressures as low as mbar. 1

5 KD L- 4Serie Feed Inlet Hot Oil Inlet Hot Oil Outlet Wiper Rollers Distillate Receiver Residue Receiver 1 Vent Valve Isolation Valve Condenser Inlet Condenser Outlet Vacuum Outlet Internal Condenser 2

6 SP ml feed vessel with isolation valve jacketed for hot oil heating 500 ml distillate flask with vent and isolation valves cryowell style cold trap suitable for liquid nitrogen or dry ice table-top support stand 115 or 230V 50/60 Hz 1 year excluding glass and consumables 3

7 SP ml feed vessel with isolation valve jacketed for hot oil heating 500 ml distillate flask with vent and isolation valves cryowell style cold trap suitable for liquid nitrogen or dry ice stainless steel vacuum manifold precision bleed valve for pressure control Pirani style vacuum sensor with power supply and digital display 5.8 m3/h (3.4 cfm) dual stage rotary vane pump with gas ballast valve and oil vapor exhaust filter 1.0 kw hot oil circulator, 250 C max. table-top support stand Temperature: C (+/ C) Vacuum: mm Hg Hot oil circulator Rotary vane pump Vacuum sensor 1 year excluding glass and consumables 4

8 5 SP ml jacketed feed vessel with isolation valve jacketed for hot oil heating 500 ml distillate flask with vent and isolation valves cryowell style cold trap suitable for liquid nitrogen or dry ice stainless steel vacuum manifold precision bleed valve for pressure control Pirani style vacuum sensor with power supply and digital display 5.8 m3/h (3.4 cfm) dual stage rotary vane pump with gas ballast valve and oil vapor exhaust filter 50 L/s air cooled oil diffusion pump 2.4 kw hot oil circulator, 300 C max. a table-top support stand Temperature: C (+/ C) Vacuum: mm Hg Hot oil circulator Rotary vane pump Diffusion pump Vacuum sensor 1 year excluding glass

9 500 ml jacketed feed vessel with isolation valve jacketed for hot oil heating 500 ml distillate flask with vent and isolation valves cryowell style cold trap suitable for liquid nitrogen or dry ice stainless steel vacuum manifold precision bleed valve for pressure control Pirani style vacuum sensor with power supply and digital display 5.8 m3/h (3.4 cfm) dual stage rotary vane pump with gas ballast valve and oil vapor exhaust filter 50 L/s air cooled oil diffusion pump 2.4 kw hot oil circulator, 300 C max. (evaporator) 2.4 kw hot oil circulator, 300 C max. (feed) table-top support stand Temperature: C (+/-0.01 C) Vacuum: mmhg Hot oil circulators Rotary vane pump 115 V or 230V, 50/60 Hz SP Diffusion pump Vacuum sensor 1 year excluding glass and consumables 6

10 SP ml jacketed feed vessel with isolation valve jacketed for hot oil heating 500 ml distillate flask with vent and isolation valves cryowell style cold trap suitable for liquid nitrogen or dry ice stainless steel vacuum manifold precision bleed valve for pressure control Pirani style vacuum sensor with power supply and digital display 5.8 m3/h (3.4 cfm) dual stage rotary vane pump with gas ballast valve and oil vapor exhaust filter 50 L/s air cooled oil diffusion pump 2.4 kw hot oil circulator, 300 C max. (evaporator) 2.4 kw hot oil circulator, 300 C max. (feed) 2.0 kw heating / 500 W cooling circulator, -30 to 200 C internal condenser) table-top support stand Temperature: C (+/ C) Vacuum: mm Hg Hot oil circulators Condenser circulator Rotary vane pump Diffusion pump Vacuum sensor 1 year excluding glass and consumables 7

11 500 ml jacketed feed vessel with isolation valve jacketed for hot oil heating 500 ml distillate flask with vent and isolation valves cryowell style cold trap suitable for liquid nitrogen or dry ice stainless steel vacuum manifold precision bleed valve for pressure control Pirani style vacuum sensor with power supply and digital display 5.8 m3/h (3.4 cfm) dual stage rotary vane pump with gas ballast valve and oil vapor exhaust filter 50 L/s air cooled oil diffusion pump 2.4 kw hot oil circulator, 300 C max. (evaporator) 2.4 kw hot oil circulator, 300 C max. (feed) 2.0 kw heating / 500 W cooling circulator, -30 to 200 C (internal condenser) 2.0 kw heating / 900 W cooling circulator, -50 to 200 C (cold trap) table-top support stand Temperature: C (+/ C) Vacuum: mm Hg Hot oil circulators Condenser circulator Cold trap circulator Rotary vane pump Diffusion pump Vacuum sensor 1 year excluding glass and consumables SP

12 9 SP ml jacketed feed vessel with isolation valve jacketed for hot oil heating 500 ml distillate flask with vent and isolation valves cryowell style cold trap suitable for liquid nitrogen or dry ice stainless steel vacuum manifold precision bleed valve for pressure control Pirani style vacuum sensor with power supply and digital display 5.8 m3/h (3.4 cfm) dual stage rotary vane pump with gas ballast valve and oil vapor exhaust filter 50 L/s air cooled oil diffusion pump 6.0 kw hot oil circulator, 400 C max. (evaporator) 2.4 kw hot oil circulator, 300 C max. (feed) 2.4 kw hot oil circulator, 200 C max. ( internal condenser) table-top support stand Temperature: C (+/ C) Vacuum: mm Hg Hot oil circulator 3P Hot oil circulator Condenser circulator Rotary vane pump Diffusion pump Vacuum sensor 1 year excluding glass and consumables

13

14 The KDL and 825 Series of evaporators were designed to utilize an external heating mantle instead of a hot oil jacket. The benefits of the heating mantle are it can achieve a higher operating temperature than a hot oil circulator (hot oil circulators for Laboratory Model Evaporators are limited to a 400 C operating temperature) at a lower cost. The disadvantage of a heating mantle is that it does not provide the same level of temperature control which can be achieved using a hot oil heating media. This limitation in temperature control and heating consistency can result in a less selective distillation of the feed material. In other words, the Gaussian distribution of molecules in the distillate and residue products will have a higher standard deviation when using an electric heating mantle compared to a hot oil jacketed evaporator. However, if your budget is limited or your heating temperature requirements exceed 400 C, the heating mantle option may represent an opportune alternative. Chemtech will be happy to answer any of your questions related to heating options associated with our evaporators. SP ml feed vessel with isolation valve 500 ml distillate flask with vent and isolation valves cryowell style cold trap suitable for liquid nitrogen or dry ice table-top support stand Temperature: 400 C max. 1 year excluding glass and consumables 11

15 500 ml feed vessel with isolation valve non-jacketed for electrical mantle heating 500 ml distillate flask with vent and isolation valves cryowell style cold trap suitable for liquid nitrogen or dry ice stainless steel vacuum manifold precision bleed valve for pressure control Pirani style vacuum sensor with power supply and digital display 5.8 m3/h (3.4 cfm) dual stage rotary vane pump with gas ballast valve and oil vapor exhaust filter 1.0 kw heating mantle, 400 C max. table-top support stand Temperature: C (+/ C) Vacuum: mm Hg Electric Heating Mantle Rotary vane pump Vacuum sensor 1 year excluding glass and consumables SP

16 CTS CHEMTECH SERVICES, INC. Short Path Distillation Services Tel: Cell: Fax: Chemtech Services, Inc Gaskin Drive Lockport, Illinois Phone: Fax: Web:

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