Classifications

• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
  • B01D61/14—Ultrafiltration; Microfiltration
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
  • B01D61/14—Ultrafiltration; Microfiltration
  • B01D61/145—Ultrafiltration
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
  • A23J1/00—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
  • A23J1/001—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from waste materials, e.g. kitchen waste
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
  • A23J3/00—Working-up of proteins for foodstuffs
  • A23J3/04—Animal proteins
  • A23J3/06—Gelatine
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
  • B01D61/14—Ultrafiltration; Microfiltration
  • B01D61/145—Ultrafiltration
  • B01D61/146—Ultrafiltration comprising multiple ultrafiltration steps
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
  • B01D61/14—Ultrafiltration; Microfiltration
  • B01D61/16—Feed pretreatment
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
  • B01D61/58—Multistep processes
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09H—PREPARATION OF GLUE OR GELATINE
  • C09H3/00—Isolation of glue or gelatine from raw materials, e.g. by extracting, by heating
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
  • B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
  • B01D61/025—Reverse osmosis; Hyperfiltration
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
  • B01D61/14—Ultrafiltration; Microfiltration
  • B01D61/147—Microfiltration

Definitions

• This invention is generally directed to a process for recovery, purifying and
• Gelatin and gelatin derivatives are used to encapsulate the products of several
• the amount of the encapsulating material and the encapsulated material e.g. vitamins
• the amount lost as waste of the encapsulating material is lost. Frequently, the amount lost as waste of the encapsulating material
• solvents usually water
• softening agents and oil coatings when desired
• colorings and preservatives may also be added.
• chlorinated solvents such as, for example, 1 ,1 ,1 ,-trichloroethane with naphtha.
• solvents including isopropyl alcohol, methyl isobutyl ketone, toluene, hexane, heptane,
• deionized water is added to the waste material thereby
• the lower phase is hot filtered to remove any remaining
• Clear gelatin contains no dye, colorants or the like. It is used to make clear
• the suspension particles such as titanium dioxide which impart a color to the
• the gelatin contains suspended particles (e.g. a colorant).
• the present invention is generally directed to the recovery of waste gelatin alone
• waste material containing gelatin comprising:
• the second liquid may be concentrated by removing at least some of
• solvent solvent soluble active ingredients, softening agent, dyes and other solvent
• Figure 1 is a schematic view of an embodiment of the method of gelatin recovery
• Figure 2 is a schematic view of a further embodiment of the invention similar to
• Gelatin is a protein derivative of collagen obtained, in general, by the boiling of
• Agents such as glycerin, sorbitol, or other similar polyols are desired.
• Glycerin is a preferred softening agent.
• the soft elastic capsule-forming material may be used to enclose active
• Oils such as
• vitamin A vitamin A, vitamin E, and beta-carotene, for example, are frequently encapsulated by
• oils like mineral oil or medium chain triglycerides (MCT's) may be used.
• MCT's medium chain triglycerides
• waste product of the encapsulation process may have, in addition to
• gelatin and a softening agent such as glycerin, many components (e.g. oily), many components (e.g. oily
• coloring agents and preservatives may
• methylparaben methylparaben, propylparaben, and sorbic acid.
• gelatin starting material i.e. gelatin ribbon
• gelatin ribbon gelatin ribbon
• the present invention provides a novel and efficient method of purifying
• glycerin is
• Suitable solvent such as deionized (D.I.) water is added through a conduit 2 in an
• dissolution/separation vessel 4 which may be provided
• the solvent is preheated to a temperature of from about 30 to 70°C to make the waste gelatin in a convenient flowable condition.
• waste gelatin material is then charged either batchwise or continuously to the
• conduit 5 which may be made of stainless steel
• dissolution/separation vessel 4 may also be provided with a conventional agitation
• the waste material to be recovered is diluted with
• the solvent e.g. deionized water
• the solvent typically at atmospheric pressure under heating at a
• gelatin and the softening agent e.g. glycerin.
• a solution of gelatin and glycerin i.e. solvent based layer (e.g. aqueous layer)]
• non-solvent based layer e.g. non-aqueous layer
• solvent based layer shall mean a layer or phase in which the components
• non-solvent based layer shall
• aqueous layer aqueous layer.
• concentration level of gelatin from about 8% to 45% is a
• solvent based layer e.g. non-aqueous layer
• a lower solvent based layer e.g.
• the upper non-aqueous layer is either discarded or sent via a conduit
• oils may be separated into oily components including, but not limited to, vitamins (for
• vitamin containing products e.g. vitamin E
• mineral oil e.g. olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, olive oil, garlic oil, garlic oil, fish oil, beta
• based layer e.g. aqueous layer
• non-aqueous layer e.g. aqueous layer
• non-aqueous layer within the vessel 4 can be facilitated by a sight glass incorporated
• an oil skimmer may be employed to remove the non-aqueous layer, as previously indicated, which is discarded
• aqueous layer of the recycling system can be accomplished by a variety of processes
• distillation is a process in which a liquid is vaporized, recondensed
• the liquid which has vaporized is collected in a receiver.
• the resultant liquid i.e. condensed vapor
• the condensate or distillate is referred to as the condensate or distillate.
• Distillation is a process for purifying liquids by separating the liquid into its
• the vapor pressure of a liquid is related
• Fractional distillation is the separation and purification, by distillation, of two or
• distillates or fractions distillates or fractions.
• a fractionating column is used to essentially perform a large
• a fractionating column may be packed with glass
• Short path distillation is especially suitable for substances that cannot be distilled
• the substance has a residence time in the presence of heat which is very short so
• a short path distillation apparatus typically includes a rotating still. Materials are
• the degree of vacuum is controlled to collect the distillate effectively at the
• the pressure can be as low as 1 ⁇ m Hg.
• Short path distillation as described herein is also known as molecular, wiped film,
• Reverse osmosis is a process whereby dissolved solids or a miscible liquid are
• the semipermeable membrane allows water to flow therethrough, but does not
• Reverse osmosis equipment is commercially available from companies such as Pall Filtron in
• the dissolved gelatin is separated into a solvent based layer
• non-solvent based layer e.g. non-aqueous layer
• non-solvent based layer e.g. non-aqueous layer
• aqueous layer is then treated by any of the above described methods to recover the oils
• the separated aqueous layer contains particulates and/or oily type materials
• the aqueous layer may then be treated, to remove residual oils and/or particulates
• the aqueous layer is sent through a heated transfer conduit 14, to a hot filtration
• the hot filtration assembly 18 is particularly desirable if the aqueous layer
• micro/micro-filtration liquid.liquid coalescers, absorbents and filter aids such as, but not
• diamataceous earth activated carbon, clay or activated clay, colloidal silica,
• porous acrylic resins and the use of oil soluble salts to break any emulsion that may
• Liquid:liquid centrifugation is based on the principal that the rate of separation
• centrifugal force which can typically range from 10 to hundreds of thousands. Relative
• centrifugal force can be controlled by varying the speed or the centrifuge head or rotor.
• the aqueous layer to be hot As a method of hot filtration in the subject invention, the aqueous layer to be hot
• filtered is maintained at a temperature sufficient to allow flow into the centrifuge; higher
• temperatures and/or higher dilutions may also enhance an efficient separation by
• dilution volume of up to 5 volumes, preferably from about 0.5 to 5
• a suitable solvent such as water
• the efficiency of separation may be enhanced by employing a relatively higher
• aqueous layer containing gelatin and glycerin is collected for reuse and the residual oils and/or particulates are either discarded or collected for potential recovery as discussed
• Liquid:liquid:solid centrifugation can also be utilized to achieve separation of the
• gelatin and softening agent e.g. glycerin
• the coloring system e.g. titanium dioxide
• Micro or sub-micro filtration refers to a method of removing small particles from
• Particulates as used herein include, but are not limited to, solid particulates
• Micro or sub-micro filtration can
• micron or sub-micron pore sized filters including, but not
• cartridge type filters also known as “depth” or “dead end” filters and
• Tangential flow type filters are the preferred filters for this
• the pore size of the preferred filters is typically in the range of from about 0.1
• a suitable solvent such as water
• Micro or sub-micro filtration equipment is commercially available from suppliers
• a liquid:liquid coalescer may be used to remove residual oils from the aqueous
• the coalescer enhances the collection of the oil droplets (the dispersed phase
• a multiple stage system may be employed.
• Such systems remove the designated materials in stages such as by first removing
• the remaining liquid may then be
• a suitable solvent such as water
• Filter aids containing diatomaceous earth can be employed for removal of
• Diatomaceous earth more commonly known as Celite
• Filter Aid is a very pure and inert material which forms a porous film or cake on a
• filter medium such as, but not limited to, filters made from paper, nylon and
• polypropylene as are typically used in filtration systems using filtration apparatus such
• Diatomaceous earth can be employed: 1 ) by forming a slurry with an appropriate
• a suitable solvent such as water
• filter aids besides diatamaceous earth include, but are not limited
• silica acrylic resins, clay and activated carbon.
• Absorbents which may be used to treat the solvent based layers include zeolitic
• the lower aqueous phase may be heated, preferably hot filtered in
• the filtration assembly 18 if particulates and/or residual oils are present at a temperature of approximately the same as above (i.e. from about 30°C to 70°C) preferably through
• plate filters or coated plate filters like, for example, a
• sparkler filter The preferred material of construction for these type of filters is stainless
• nutche filters of the Rosenmund type or cartridge filters may be
• agent e.g. glycerin
• the filtrate may be returned directly to gelatin mass manufacturing or the filtrate
• concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly 16 which may be transported via heated conduit 22 to a concentration assembly
• solvent e.g. water
• the aqueous solution may be charged
• the filtrate may be subjected to short path distillation as
• waste gelatin material is diluted with solvent (e.g. water) at a
• the distillation should preferably result in a distillate: residue ratio of 50:50.
• the distillation should preferably result in a distillate: residue ratio of 62.5:37.5.
• the residue contains the gelatin and glycerin for recycle. Diafiltration may be employed at the concentration assembly 16 to remove
• Diafiltration is a technique using ultrafiltration membranes to remove or
• membrane retains macromolecules that are larger than the nominal molecular weight
• the macromolecules must be "washed" using multiple wash volumes to
• diafiltration i.e. filtration using
• macromolecules e.g. gelatin
• Discontinuous diafiltration involves first concentrating the macromolecule (e.g.
• diafiltration may be accomplished by first heating the
• Such filters include screen filters including open channel filters
• gelatin capable of separating gelatin (typically having a molecular weight of from about 30,000
• the recovered aqueous gelatin solution is concentrated to a final solids (gelatin)
• purified recycled gelatin may be sent back to the gelatin dissolving step via a conduit
• Impurities such as dyes, actives, water, preservatives and glycerine can be
• distillation systems including fractional distillation, short path distillation
• glycerol may contain from about 1 % to 10% by volume of glycerol in water, typically from about
• the process stream 30 is treated at temperature of from about
• glycerol is at least 65% by volume, more typically from about 65% to 95%, most preferably from
• dyes and pigments that are used to color gelatin capsules are used to color gelatin capsules
• the gelatin include use of, for example, activated clay, carbon cartridge filtration; carbon
• diafiltration can be performed to obtain recovered gelatin.
• Entrapped air may be a consideration during the process of manufacturing
• gelatin capsule manufacturing industry is to manufacture the gelatin mass under
• gelatin mass can be transferred by air pressure or pumps.
• gelatin mass examples of appropriate pumps may be, but are not limited to, peristaltic,
• the ultrafiltration process of the present invention can generate flow rates in
• the flow rates generated may nonetheless, introduce some air into the gelatin.
• the air may nonetheless, introduce some air into the gelatin.
• micron membrane filter and/or 2) sparge the water and/or organic solvent with an inert
• a membrane filter e.g. 0.45 micron
• the filter could be incorporated into the diafiltration system 16
• the diafiltration system 16 is first treated as described above to remove impurities via
• the recovered gelatin may then be filtered with a membrane filter to
• the degassing operation may be performed in another embodiment of the present invention.
• recovered gelatin is sent via the conduit 26 to a conduit 27 which leads to a degassing
• the degassed gelatin is sent via the conduit 31 to be recycled or recovered. It is understood that the above described recycling system may be incorporated

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• Engineering & Computer Science (AREA)
• Chemical & Material Sciences (AREA)
• Water Supply & Treatment (AREA)
• Life Sciences & Earth Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Biochemistry (AREA)
• Food Science & Technology (AREA)
• Polymers & Plastics (AREA)
• Organic Chemistry (AREA)
• Zoology (AREA)
• Health & Medical Sciences (AREA)
• Nutrition Science (AREA)
• Separation Using Semi-Permeable Membranes (AREA)
• Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
• Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Priority Applications (4)

Applications Claiming Priority (10)

Publications (1)

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Family Applications (1)

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Cited By (5)

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Citations (3)

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• 1999
  • 1999-11-15 KR KR1020017006172A patent/KR100674488B1/ko not_active IP Right Cessation
  • 1999-11-15 AU AU16257/00A patent/AU760327B2/en not_active Ceased
  • 1999-11-15 WO PCT/US1999/027095 patent/WO2000029097A1/en not_active Application Discontinuation
  • 1999-11-15 JP JP2000582138A patent/JP2002529589A/ja active Pending
  • 1999-11-15 EP EP99958995A patent/EP1137481A4/en not_active Withdrawn
  • 1999-11-15 CA CA002350746A patent/CA2350746C/en not_active Expired - Fee Related

Patent Citations (4)

Non-Patent Citations (1)

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