Winterization

Winterization
Safety
  • SDS Sheets: Available upon request on all chemicals used in this process
Preparations
  • Required Materials/Media:
  1. Silica Gel
  2. Activated Alumina
  3. n-Heptane, Hexane or Ethanol
Procedure
  1. Warm crude to 30c
  2. Fully dissolve crude in a solvent, 10:1 (1L Crude: 10L EToH)
  3. Allow mixtures to cool to room temperature
  4. Filter over a bud of Alumina on top of Silica Gel in a filter funnel
  5. Cool solution to 0c
  6. Repeat step 4
  7. Take a representative sample of the solution and add dry ice until the solution stops bubbling
  8. Repeat steps 4 with sample
  9. If more solids are filtered out in Step 8, repeat steps 7 and 8 with entire solution.
  10. If no solids were present in step 8, or after step 9, proceed to next process

At this point you have two options:

If pursuing a single pass end result, or you do not wish to process your distillate between the first and second passes, adsorbent scrubbing the crude while still in the solvent solution is appropriate.

If the situation allows for it, adsorbent scrubbing post first pass distillation, in an alkane solution (n-Heptane, Hexane) is more effective.

Pre-First Pass Adsorbent Scrubbing Method

  1. In a well ventilated area or fume hood, heat your oleo-resin to 90c
  2. Measure 5% of total material volume in T-41 and slowly add to oil (1000g oleo-resin: 50g T-41)
  3. Stir for 20-30 minutes while maintaining a minimum of 90c temerature.
  4. Allow solution to cool to approximately 40c, then add carrier solvent such as Ethanol, Hexane or n-Heptane and filter through alumina/silica over filter funnel
  5. Repeat steps 1-4, 2 to 3 times depending on color remediation necessary.

(*Hardwood Activated Carbon can replace T-41 for the first scrub if multiple scrubs are performed. Degumming would be appropriate before first pass as well)

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