ROTARY EVAPORATOR Rotary Evaporator - Qrfy

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ROTARY EVAPORATOR A Rotary Evaporator, also popularly known as a Rotavapor or Rotovap, is specialized and extremely Versatile Equipment for chemical processes. A rotary evaporator is a piece of machinery or equipment used in the creation of some cannabis concentrates. A rotary evaporator evaporates and recovers pricey ethanol from ethanol-extracted concentrates. Rotary evaporators are one of the key steps in creating butane hash oil (BHO) and other cannabis concentrates. Using the rotary evaporator helps effectively concentrate the oil to a concentration of 15 to 40 per cent. It also purges the solvents from the finished product and recovers them, making the oil exceptionally pure. Rotary Evaporator Principle The Evaporator is essentially working on the same principles as a distillation unit i.e. separation of components having different boiling points. However, few special design features make the functioning of the Rotovap unique and versatile. They are: Operation under high vacuum of 1 torr, thereby reducing the solvent boiling points under vacuum considerably as compared to the boiling point under atmospheric conditions. Constant rotation of Rotary flask results in a thin layer of process media on the inner wall, thereby ensuring uniform heating across the entire mass and less possibility of bumping. The rotation of flask immersed in the bath increases the surface area of evaporation greatly, thereby increasing the speed of distillaiton. The rotation mechanism also makes it suitable for volatile and heat-sensitive process media, wherein the properties can alter if direct high heat is applied for longer time. This is because due to rotation, the process feed is evenly mixed. Plug and Play type of construction making it easy to switch the configuration for different applications. The Rotary Evaporator is normally always operated under high vacuum. The Feed is charged inside the rotary flask from the feed tube made of PTFE. Ideally, feed up to a maximum of 70– 80% capacity of the rotary flask is desired for optimum results. Once the feed is charged, the rotation is started. Also, the utility circulation in the condenser is started. This rotation action creates a thin film of process feed on the wall of the rotating flask. Next the heating is started. The rotary evaporator procedure is very crucial for efficient performance. Once the oil in the bath starts heating, and this heat is indirectly passed to the process feed inside the flask. As the process feed gets heated, the low boiler converts into vapours, and goes up the vapour tube and into the condenser, where the condensate is formed. This condensate can either be refluxed back into the rotary flask for higher purity applications, or collected in the receiver.

Working 1. Preparations Pour the mixture of solvent and required compound in a round bottom flask, which should be fiiled less than half full of the solution. Fill the rotovap cold traps with dry ice. Attach a glass “bump trap” to prevent any solution from entering the main part of the rotovap. Secure with a clip. Connect the flask and bump trap to the adaptation part with a clip. Lower the flask into the water bath, preventing the flask from disconnection. 2. Operation The working process of rotary evaporator is a consecutive process under a reduced environment. There are several steps for the operation: Under reduced pressure, the evaporation the evaporation flask was continuously rotated while the solvent was being distilled. The evaporation flask is a pear-shaped or round-bottomed flask with a standard ground mouth connection. It is connected with the pressure reduction pump through a serpentine condenser. After substances get evaporated by heating, the gas-phase substances will go into condensing part to get condensed. In this step, gas substances are transferred through the glass tubes. After gas-phase substances got condensed into liquid-phase, the liquid-phase substances will be transferred into receiving flask, which is the final destination of extracted substances. And then users will take the receiving flask out of rotary evaporator equipment. During the whole working process, there is always a vacuum pump providing a vacuum environment for the rotary evaporator, which guarantees the whole system work in a reduced environment and the automatic feeding system formed by the pressure difference between atmosphere pressure and vacuum pressure. Three Things Make Rotary Evaporators So Quick at Removing the Solvent from a Round Bottom Flask The things influencing the working efficiency of a rotary evaporator include steam temperature, vacuum degree and cooling water temperature. Restricted by some material’s thermolability, the steam temperature may have certain limitation when working, so high vacuum degree and low cooling water temperature are two main factors for efficiency improving (can select cryopump to lower the temperature).

Rotary Evaporator Remove Water A rotary evaporator is widely used in removing water from materials, which is to concentrate substances. Removing water by using a rotary evaporator is commonly used in kitchen, for example, concentrate fruit juice, which is to remove water from fruit juice. Besides, there are other examples of removing water from substances. Depending on the design features, a lot of different process possibilities are there, but the basic operating principle essentially remains as indicated above. The main components of a rotary evaporator 1.A motor unit that rotates the evaporation flask or vial containing the user’s sample. 2.A vapor duct that is the axis for sample rotation, and is a vacuum-tight conduit for the vapor being drawn off the sample. 3.A vacuum system, to substantially reduce the pressure within the evaporator system. 4.A heated fluid bath (generally water) to heat the sample. 5.A condenser with either a coil passing coolant, or a “cold finger” into which coolant mixtures such as dry ice and acetone are placed. 6.A condensate-collecting flask at the bottom of the condenser, to catch the distilling solvent after it re-condenses. 7.A mechanical or motorized mechanism to quickly lift the evaporation flask from the heating bath. Generally, the component liquids of interest in applications of rotary evaporation are research solvents that one desires to remove from a sample after an extraction, such as following a natural product isolation or a step in an organic synthesis. Liquid solvents can be removed without excessive heating of what are often complex and sensitive solventsolute combinations. Rotary evaporation is most often and conveniently applied to separate “low boiling” solvents such a n-hexane or ethyl acetate from compounds which are solid at room temperature and pressure. However, careful application also allows removal of a solvent from a sample containing a liquid compound if there is minimal co-evaporation (azeotropic behavior), and a sufficient difference in boiling points at the chosen temperature and reduced pressure. 2. Rotary Evaporator Construction

The Main Components of a Standard Rotary Evaporator are enlisted below: The water/oil bath is a heated bath which encloses the main rotary flask and is used to indirectly heat the contents of the process. The bath is usually equipped with electric heaters which can be ATEX-compliant or weather-proof, depending on the application area’s Hazardous Zone Classification. As a safety feature, the bath is appropriately insulated so that the outside surface is not too hot to touch. The Rotary Flask is the main component where the process fluid is initially charged, and is made of Borosilicate Glass 3.3 raw material. The Flask’s construction is of prime importance for the smooth rotation along the central axis. Our advanced manufacturing techniques ensure that the evaporating flask is rotating perfectly along the central axis, thereby ensuring that the entire surface area comes in contact for the same time with the heating media in bath. The Mechanical Seal, along with the motor unit connected to the flask is responsible for smooth and leak proof rotation of the flask at a constant speed. An RTD is placed just above the vapour tube to measure the vapour temperature before it goes into condenser. The RTD is inserted inside the vapour tube in a glass thermowell. This ensures that the contact parts are strictly Borosilicate Glass 3.3 and PTFE only and the metal tip of PT-100 sensor does not come in direct contact with the process vapour.

A Shell & Coil type condenser of suitable heat transfer area is chosen so that there is no pressure build-up due to excessive un-condensed vapours. The condenser is preferably placed in vertical orientation for efficient condensation. Different configurations with single and double condensers are available depending on the application. As a standard, a single condenser is provided. A vent is provided at the top of the condenser. This can be used for venting in the case of excessive pressure build-up. We can also connect the vacuum pump here. Alternatively, the vacuum pump connection can be made at the receiver vent nozzle. All such vent outlets are equipped with suitable valves with leak-proof PTFE bellow to glass connections. The vent valve is provided with GL18 thread at the end, where BOLA connectors can be placed and hose pipe connected. This arrangement provides seamless connection without any leakages. The Liquid feed is used to feed the process feed into the rotary flask without breaking the process vacuum. Since the system is already under vacuum, the process feed easily flows into the system. This valve too is provided with GL thread and BOLA connector. This valve is connected with a PTFE tube which travels throughout the vapour tube, directly into the rotary Flask. This ensures that the feed does not get carried to the receiver directly along with the vapour or condensate flowing in the vapour tube. A Product Cooler is essential to cool down the condensate, before moving it to the receiver. The product cooler is essentially a Shell & Coil type heat exchanger with the process fluid in the coil side and utility in the shell side. This arrangement ensures rapid cooling in a short time. The receivers are spherical vessels with multiple nozzles of a suitable size. The units usually have either one or two receivers, connected in parallel. The receiving vessel has a short drip tube to ensure that the solvent drops down directly into the vessel and not flow along the walls. A Control Panel is an integral part of the Rotary Evaporator. This is a highly customized part and Ablaze can offer partial to full automation of the process through the control panel, depending on the client’s process requirement. As a standard, the basic model has

provision for digital display of Bath temperature, Vapour Temperature and RPM of the Rotary Flask. It also has controls to set the desired RPM and the desired Oil Bath Temperature. In a little advanced models, Vacuum control and monitoring is also provided, wherein the vacuum pump is connected via the panel and the required process vacuum can be set, monitored and controlled directly through the panel. Further customization and control can be provided, since we have a highly advanced in-house automation team. The Panel and all the electric components are housed in an ATEXCompliant Enclosure for operation in hazardous areas. The Entire Rotary Evaporator System is mounted on a Compact Skid of Stainless Steel where all the components rest and all provided appropriate support to ensure vibration free operation. This skid itself is mounted on heavy duty Castor Wheels, which can be locked, to provide easy movement of the unit in the plant or lab. A Safety Lid is placed on the rotary flask as a precaution in case of spillage risk. It is transparent and hence it provides safety without compromising on the reaction visibility. 3. Rotary Evaporator Design Variations Multiple Design Variations are available in Our Standard Rotary Film Evaporator to suit different process needs. Some of the standard design variations are: Dual Receivers— This configuration allows continuous drain without breaking the process vacuum. The two receivers are connected in parallel so that at any given point of time, the condensate is being collected in one of them. Once this receiver is full and

needs to be drained out, the valve above it is closed, and the condensate is taken in the second receiver. This way, the system vacuum is not disturbed during draining. Dual Condensers — This design is used when immediate condensation of the vapours is required. Two condensers are placed in parallel, and the condensate is directly collected in the receivers. This ensures 100% solvent recovery. This design can also be modified for continuous operation. ATEX-Compliant — The Rotavap contains a lot of electric components — two sets of drive (one for rotation and other for bath lifting) and a control panel. We do understand that a lot of applications require the Rotovap to be used in Zone 0 / 1 / 2 hazardous classified area and hence we have a model with all electrical components and connection which comply to these stringent requirements. Multiple MOCs — The contact parts with process media are strictly Borosilicate Glass 3.3 and PTFE. However, the couplings, skid etc do not come in contact with the process media and can be offered in various MOCs (Material of Construction) such as Stainless Steel grade 316 or 304, Mild Steel, etc. The couplings can also be made of Bakelite to provide good resistance to corrosion in case the environment has exposure to corrosive gases. The fasteners can be PTFE coated to improve their life.

4. Rotary Evaporator Applications The wide array of applications where a rotovap can be used shows how versatile the equipment is. It finds application in the following processes: Distillation (Continuous and Discontinuous) Concentration Solvent Recycling Solvent Evaporation and Recycling Reflux Process Reactions Component Drying Component Purification Fine Chemical Synthesis Crystallization Molecular Cooking 5. Other Evaporation Alternatives to Rotovap There are few other Process Equipments which have similar functionality as Rotary Evaporator and are used specially for Evaporation.

Falling Film Evaporator — A Falling Film Evaporator is essentially similar to a Vertical Shell & Tube Heat Exchanger in construction. The process fluid enters the evaporator from top and flows in a thin film along the walls of tubes. The same is instantly converted into vapour by the hot utility flowing in the shell. This Evaporator is completely custom designed as per the process requirement. Wiped Film Evaporator — A wiped Film Evaporator is essentially a thin film Evaporator (TFE) just like a rotovap. It works on the principle of the thermal separation of products in a mechanically generated, thin and highly turbulent liquid film along the outer surface of the evaporator. The key advantages in use of a rotary evaporator 1.that the centrifugal force and the frictional force between the wall of the rotating flask and the liquid sample result in the formation of a thin film of warm solvent being spread over a large surface. 2.the forces created by the rotation suppress bumping. The combination of these characteristics and the conveniences built into modern rotary evaporators allow for quick, gentle evaporation of solvents from most samples, even in the hands of relatively inexperienced users. Solvent remaining after rotary evaporation can be removed by exposing the sample to even deeper vacuum, on a more tightly sealed vacuum system, at ambient or higher temperature (e.g., on a Schlenk line or in a vacuum oven). A key disadvantage in rotary evaporations, besides its single sample nature, is the potential of some sample types to bump, e.g. ethanol and water, which can result in loss of a portion of the material intended to be retained. Even professionals experience periodic mishaps during evaporation, especially bumping, though experienced users become aware of the propensity of some mixtures to bump or foam, and apply precautions that help to avoid most such events. In particular, bumping can often be prevented by taking homogeneous phases into the evaporation, by carefully regulating the strength of the vacuum (or the bath temperature) to provide for an even rate of evaporation, or, in rare cases, through use of added agents such as boiling chips (to make the nucleation step of evaporation more uniform). Rotary evaporators can also be equipped with further special traps and condenser arrays that are best suited to particular difficult sample types, including those with the tendency to foam or bump. Advantages of a Rotary Evaporator The rotary evaporators are essential laboratory equipment for concentration, crystallization, drying, separation and solvent recovery in pharmaceutical,chemical and bio-pharmaceutical fields and other fields. The basic working process can be described below. The rotating flask is heated thermostatically and can rotate at a constant speed. Then the material forms a large area of thin film on the inner surface of the flask. The solvent vapor is recycled in the collecting bottle after being cooled by high-efficiency glass

condenser, which greatly improves the evaporation efficiency. A rotary evaporator is especially suitable for the concentration and purification of biological products which are easy to decompose and denature at high temperature. According to what we mentioned above, there are a great number of advantages of our rotary evaporators, as follows. 1. Higher evaporation efficiency There are several factors contributing to higher evaporation efficiency. Firstly, the rotating flask can rotate at a constant speed, and materials can form a widespread film on the inner surface of the flask, which improves the evaporation efficiency greatly. Secondly, the high-efficiency can improve the evaporation efficiency as well. Last but not least, continuous feeding and high vacuum degree are another factors. 2. Better security The stainless steel and aluminum alloy are widely used in the mechanical structure, and all glass parts are made of heat-resistant high borosilicate glass, which ensure a better security. Besides, the water/oil bath can be equipped with transparent covers to prevent splashing, and anti-explosion frequency changer and dynamo are available as well. All of these designs contribute to better security. 3. More convenient operation It’s much more convenient to use a rotary evaporator, because of the electrodeless speed regulation, digital display K Type Sensor and intelligent temperature control and other designs adopted by it. Disadvantages of a Rotary Evaporator Although a rotary evaporator has many advantages, there are still some disadvantages as well. They are as follows: 1. A rotary evaporator can only process a single sample. However, a short path distillation can process several sample materials at the same time in one equipment. 2. In the rotary evaporator equipment, the sealed equipment has a limited life, and needs to be replaced regularly. Therefore, it will take users more time and money to replace the sealed equipment regularly. 3. The sample materials may be exposed in the air, which will cause the contamination of the sample materials and extracted materials. The contamination of sample materials will cause the impurity of extracted materials, which decreases the quality of the experiments. 4. In the rotary evaporator equipment, the glassware needs to be cleaned very often, because a rotary evaporator needs a totally clean container to guarantee the purity of materials. If there is any impurity in the glassware, the extracted materials will be not pure.

What are Functions of a Rotary Evaporator? A rotary evaporator is an essential separation equipment, which can remove a volatile solvent from a liquid mixture through evaporation and condensation. For example, a rotary evaporator can be used to remove ethanol from the mixture of ethanol and CBD oil in order to improve the purity of CBD oil. Also, it can be used to remove water within fruit juice, in order to make the fruit juice have a higher concentration. It can be seen that a rotary evaporator has a great number of functions. What is a Rotovap Used for? A rotary evaporator (rotovap or rotatvap) refers to a kind of equipment for solvent evaporation under reduced pressure. It is primarily used for the process of evaporation, concentration, crystallization, drying, separation, and solvent recovery, and especially used for the continuous distillation of large amounts of volatile solvents under reduced pressure. With so many application purposes, there is no doubt that a rotary evaporator can be applied in many areas. For example, it can be used in the small and pilot experiments and production in the biological, pharmaceutical, chemical fields and even food-making industries. How does a Rotovap Remove Solvent? A rotavap evaporates solvents from samples by utilizing the principle that the solvent will have a lower boiling point at a reduced pressure. Specifically speaking, the stepless speed regulation is adopted to make the evaporation flask rotate at a constant speed. By the rotation, materials can form a large area of uniform thin film on the inner wall of the flask. The evaporation flask is heated evenly by a water or oil bath, and materials, with a lower boiling point, is evaporated rapidly under the vacuum condition. The solvent steam is recycled in the receiving flask after being cooled by the high efficiency glass condenser. Tips on Removing Solvent by a Rotovap 1. Users need to remove the gas within equipment to create a vacuum environment, then rotate to prevent the distillation flask from slipping. When you want to stop it, stop rotating firstly. Then hold the flask when you pass the atmosphere into equipment. Stop the vacuum pump until the vacuum gets reduced to 0.04MPa to prevent the distillation flask from falling off and sucking back. 2. Each interface, sealing surface, sealing ring and joint needs to be coated with a layer of vacuum grease before installation. 3. The heating tank must be filled with water before it is energized. It is not allowed to dry without water.

Rotary evaporators are one of the key steps in creating butane hash oil (BHO) and other cannabis concentrates. Using the rotary evaporator helps effectively concentrate the oil to a concentration of 15 to 40 per cent. It also purges the solvents from the finished product and recovers them, making the oil exceptionally pure. Rotary Evaporator Principle

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