High Vacuum Distillation Unit And Application On Natural Product Development

High vacuum distillation is a process technology used to separate and purify substances with boiling points that are too high or too close together for traditional distillation methods.

This process involves applying a high vacuum with multi stages vacuum pumps to the distillation system, which lowers the boiling points for process operation and offers a more efficient and cost-effective method of separating and purifying substances.

The process is highly versatile and can be tailored to meet the specific needs of each industry. Additionally, the use of high vacuum distillation can lead to higher yields, greater purity, and a reduced environmental impact.

Why Do We Use High Vacuum Distillation?

High vacuum distillation equipment plays a crucial role in modern process applications. In order to reduce the loss of heat-sensitive substances, product processing shall be carried out at lower temperatures and pressures to obtain a nutritionally complete natural product.

The benefits of high vacuum distillation are numerous and depend on the industry in which it is used.

  • In the oil refining industry, high vacuum distillation is used to separate crude oil into its various components.
  • In the pharmaceutical industry, it is used to purify active pharmaceutical ingredients and ensure their safety for human consumption.
  • In the food and cosmetic industry, it is used to extract natural flavors and fragrances.

The process offers increased efficiency, cost-effectiveness, versatility, and improved yields and purity. It is a key technology for modern industrial chemical processes and will continue to play an important role in the future.

Which Materials Are Separated By High Vacuum Distillations:

High vacuum distillation assembly unit combined with a scraping film evaporator and short-path distillers are wildly applied in process operations. A large amount of low boiling material is removed in the scraping film evaporator, and the bioactive product is separated and purified in the short path distillation.

Application IndustryMaterial Name
Food IndustryMonoglycerides, palm oil, tocopherols, cod liver oil, squalene, rice bran oil, fatty acids and their derivatives, dienoic acids, vegetable oils, diglycerides, lactic acid, linseed oil, conjugated linoleic acid
PharmaceuticalAmino acid esters, vitamin E, glucose derivatives, terpene esters, natural or synthetic vitamins, beta-carotene, curcumin, capsaicin
ChemicalEruvic acid amides, alcohols, oleic acid amides, glycerides, herbicides, haloalkanes, pesticides, silicone oils, waxes, binary fatty acids, dimeric acids
Plastics IndustryEpoxy resin, Uranium epoxide, Isocyanate, Plasticizer, Stabilizer
PetroleumBase oil, bright oil, lubricating oil, Vaseline, cold cedar oil, residual tar, waste lubricant
Cosmetic IndustryWool fatty acids, lanolin, lanolin alcohol, alkyl polysaccharides, rose oil, ginger oil, paprika red pigment, etc., extracts of algae, plants, pepper and other pepper plants

The advantages of using high vacuum distillation include:

  • Higher efficiency: High vacuum distillation is more efficient than traditional distillation because it operates at lower temperatures and pressures, which reduces the heating, cooling, and power energy required for the processing line.
  • Higher purity: High vacuum distillation can produce purer components because it operates at lower temperatures, which reduces the chances of thermal degradation and protect bioactive ingredient.
  • Higher yield: High vacuum distillation can produce higher yields because the relative volatility increases, which reduces the chances of thermal decomposition and polymerization, less heat loss, and disappearance of the azeotropic mixture.
  • Reduced environmental impact: High vacuum distillation can reduce the amount of waste generated by traditional distillation methods.

Types of High Vacuum Distillation Equipment

There are several types of high vacuum distillation equipment available for industrial process applications, and each type is designed to meet specific process requirements.

  • Short Path Distillation:

Short path distillation is a common type of high vacuum distillation used for the concentration and purification of heat-sensitive materials.

The process involves heating the substance in the system at a higher vacuum, typically 0.001-0.003 mbar. This low pressure reduces the boiling point of feed materials and allows for lower processing temperatures (about 100-220°C).

This minimizes thermal damage to heat-sensitive compounds. The substance then travels a short distance from the heating surface to the condenser, where it is cooled and collected. This type of distillation is often used in the cannabis industry to purify CBD oils. Check Here with more details.

The used examples are essential oils, natural extracts, vitamin E, fatty acids, etc. They operate at very high vacuum (0.001 mbar) and low temperatures to minimize product degradation.

It can achieve concentration levels of 30-70% for most oils and extracts. Some systems with multiple stages can reach 60-80% concentration. The wiped film and short path package designs prevent fouling even with viscous and waxing materials.

  • Molecular Distillation:

Molecular distillation is a non-equilibrium distillation carried out under high vacuum conditions, usually ≤ 0.1 Pa. Its major characteristic is that the distance between the evaporating surface and the condensing surface is within the average free travel of the molecules of the distilled material. The vapor molecules must be condensed at a shorter distance than the average free travel.

It incorporates a vertical condenser located extremely close to the evaporator surface, sometimes just 2-5 cm away. This virtually eliminates the loss of light molecules for optimal separation of very low molecular weight compounds.

In some cases, the system can operate at an ultra-high vacuum, from 0.0005 to 0.0001 mbar. This high vacuum and low pressure are suitable for materials with very low boiling points (70-180°C). It is most suitable for the isolation of individual aromatic molecules or geometric isomers.

Molecular distillation technology requires a high vacuum exhaust system, it is high-cost equipment and high maintenance cost per production volume. The system requires the use of special pumps capable of achieving and maintaining ultra-high vacuum levels like diffusion pumps or turbo molecular pumps. Standard rotary vane pumps cannot reach this level of high vacuum.

Typically the system is used for high-value fragrances and flavor ingredients like synthetic essential oils, menthol crystals, Geraniol, Linalool, etc. The short residence time in the evaporator at a very low temperature minimizes heat damage to these delicate molecules.

  • Wiped Film Distillation:

Wiped film distillation is a high vacuum distillation method that is used for the concentration, purification, and molecular distillation of viscous liquids, fats, and oils.

It is equipped with mechanical wipers to reduce fouling. Commonly used for fish oils esters, biodiesel, and nutraceuticals. They typically operate at 0.001-0.05 mbar vacuum and temperatures of 120-260°C.

Wiped Film Evaporator and Short Path Distillation Equipment Assembly for fish oil ester concentration

The substance travels down a heated surface, which is wiped by rotating wiper blades. The substance is then collected at the bottom of the system. This type of distillation is often used in the chemical and food industries.

  • Thin Film Distillation:

Thin film distillation is similar to wiped film evaporators but without mechanical wipers. It is used for non-viscous or heat-sensitive materials.

Such as wastewater treatment, natural extracts, diffuser oils, and industrial solvents. The process operates at 0.001-0.01 mbar and 100-220°C.

Each of these types of high vacuum distillation equipment has its own unique benefits and is suited to specific applications. When choosing the right equipment for your specific process, we need to consider factors such as production scale, chemical compatibility, operation parameters, output quality, costs, etc.

How to Choose the Right High Vacuum Distillation Equipment?

When it comes to choosing the right high vacuum distillation set-up for your needs, you want to make sure you get it right. This isn’t like buying an off-the-shelf gadget – these systems require custom engineering for your specific use case. As we have designed various distillation systems over the years, let me give you some advice.

  • Determine your concentration objectives.

For essential oils, are you aiming for 70% or 99% purity? For fish oil, do you need 60% or 99% concentration? The level of purity and triglyceride/ethyl esters concentration required will determine whether continuous distillation, short path distillation, or molecular distillation is suitable.

In general, the higher the concentration needed, the more advanced the distillation system required. So you may evaluate your feed material characteristics and consider the viscosity, heat sensitivity, boiling point range, and propensity to foul or polymerize.

These attributes will dictate design aspects such as the need for wiped film vs thin film evaporators, stainless steel types, and more aggressive heating and vacuum systems. For very heat-sensitive materials with low boiling components, a molecular distiller is recommended.

  • Target fraction and working conditions.

Next, think hard about what exactly you want to distill. The characteristics of your material determine a lot – like temperature control, flow rates, and equipment materials.

If you have a heat-sensitive compound or something gummy that fouls equipment, special considerations need to be made. It’s best to be upfront about these details with your equipment manufacturer.

  • Choose an appropriate vacuum level.

The vacuum level impacts boiling point, residence time, product quality, and equipment selection. Higher vacuum means lower temperatures can be used, which is critical for thermolabile materials.

It also allows the use of specialized vacuum screw pumps, vacuum roots pump and equipment like diffusion pumps, molecular pumps. As a guide, use 0.001-0.003 mbar for short path distillation, 0.0005-0.0001 mbar for molecular distillation, and 0.04-0.07 mbar for crystallization.

  • Determine your production volume requirements.

Distillation systems range from small 0.5-liter benchtop units up to industrial scale 2000 liter+ configurations. Select a system size that will meet your current production needs with room for expansion. Also, consider batch vs. continuous processing based on production volume.

  • Partner with a reputable manufacturer.

Work with a distillation company that has expertise in high vacuum design, equipment manufacturing, and your specific application. They will get the nuances like stainless steel grades, precision welding techniques, and proprietary designs that can impact product quality and operational costs. Their specialized expertise will ensure the highest quality at the lowest operational cost.

  • Installation and after-sales support.

For larger, more complex systems especially, having the equipment supplier also handle the installation and train your operators is ideal. Their in-house experts will troubleshoot issues and help you start well.

If chosen well for your needs, the right high vacuum distillation system becomes an invaluable asset. Partnering with a specialized manufacturer, you gain a tailor-made solution and advisor to help you produce the purest compounds efficiently for years to come. Distillation equipment is a long-term investment, so take your time and choose wisely!

Applications of High Vacuum Distillation

As a supplier of distillation systems for the marine oils industry, fractional distillation under high vacuum is key to refining fish oil ethyl esters. To get the highest quality omega-3 concentrates, fish oil goes through a process of ethylation and then separation using our high vacuum distillation columns.

After fish oil crude has been ethylated into fatty acid ethyl esters (FAEEs), it contains a range of ethylated compounds with varying carbon chain lengths. Our role is to separate these into purified fractions based on their boiling points and high vacuum conditions make this possible while avoiding excess heat exposure.

By lowering pressures down to around 5-0.1 Pa inside the column, boiling points drop significantly so that compounds can be vaporized at far lower temperatures. This allows for quicker separation of each fraction with less potential for degradation.

The lightest, shortest-chain FAEEs will be initially separated. Then come purified ethyl esters of C8, C10, C12, C14, C16, and C18 fatty acids and other fractions, and the ranges you are targeting. Managing the precise temperatures at each stage where fractions are drawn off is crucial for achieving optimized yields of each target compound with maximum purity.

Quick refluxing also improves separation by allowing compounds to redistill until pure. The quick strip rates under high vacuum minimize residence time, so fractions spend less time subjected to heat and pressure overall.

Aggressive condensate removal using chillers or traps to prevent build-up of heavier, waxing esters. Automatic valves control or shut down the system if condensate levels get too high.
Compared to atmospheric or low vacuum distillation, high vacuum conditions allow some fractions to emerge at lower temperatures. C12 and C14 esters, for example, can be purified at 130-160°C rather than 200°C. The lower heat means fewer opportunities for fractions to crack, recombine or oxidize which would reduce quality.
For ethylated fish oil, high vacuum fractional distillation gives us tight control to produce purified fatty acid ethyl ester fractions in the desired ranges, concentrations, and volumes. By providing quicker separation, lower operating temperatures, and shorter exposure, we can refine this sensitive starting material into high-quality omega-3 concentrates with minimal loss or waste.

High precision components like manometers, thermocouples, and flow meters to measure vacuum levels, temperatures, flow rates and other parameters accurately. Tight control of distillation requires accurate instrumentation. The key is customizing the equipment and parameters precisely for the compounds being distilled. Contact Us For Precise Solutions.

The Hazards of High Vacuum Distillation and How To Mitigate Them?

As a professional vendor designing high vacuum distillation systems, we take safety seriously. The units operate under extreme conditions of high temperature heating and low pressure, so risks must be properly mitigated.

But with tight controls and protective equipment, they can be operated safely. The high temperatures required to vaporize feed materials pose a burn risk, especially for heat transfer fluids, steam, and condensers. Insulation and alarms help avoid contact with hot surfaces. Proper ventilation removes built-up heat and prevents oxygen depletion.
Low operating pressures mean leaks can allow air to enter but not exit – creating a vacuum lock scenario. Emergency vacuum release valves prevent equipment overpressure. Leak checks before startup, during operation, and during maintenance help identify and fix cracks. Systems should also have automatic shutdown controls triggered by low vacuum levels.

Safety Procedures and Their Importance In Ensuring A Safe Work Environment?

Maintaining pressures far below atmospheric levels requires high-powered vacuum pumps and steam ejectors which pose risks like ejection of pump fluids or broken blades if they malfunction. Protection like filters, separators and sturdy pump casings reduce these risks with proper maintenance and part replacements per schedule.
There are also risks of implosion from pressures lower than equipment tolerances and oil fires if pumped hydrocarbons ignite. Thick stainless steel construction, grounding, explosion-proof electrics and fire sprinklers mitigate damage. Oil mist can coat and clog equipment, so demisters remove excess droplets.
By understanding the specific hazards of high heat, low pressure and hydrocarbon materials, we design safety into each system. With emergency stops, protective gear, leakage prevention and fire control alongside regular maintenance, high vacuum distillation can be conducted securely.

Operators receive intensive training to monitor the process vigilantly. Strict adherence to procedures allows this equipment to function safely for years when built and operated responsibly.

Conclusion

Fish oil esters contain a range of compounds with different boiling points. High vacuum distillation is key to concentrating specific fractions.

By lowering pressure to 0.1-5Pa, compounds boil at lower temperatures. This allows fractionating heat-sensitive esters that would oxidize at atmospheric pressure. Short path evaporators isolate and concentrate target compounds like EPA and DHA ethyl esters. Molecular distillers achieve over 60% purity, ideal for fish oils ethyl esters where impurities impact color and odor.

Across fish oil refining, high vacuum distillation maximizes yield of high-value Omega-3 ingredients, enabling nutraceutical, food and feed applications where purity, quality, and consistency are essential. Its mild conditions and precision make high vacuum indispensable for refining this delicate, in-demand material.

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