WO2009135601A1 - Verfahren zur herstellung von gelatinepulver und damit hergestelltes gelatinepulver - Google Patents
Verfahren zur herstellung von gelatinepulver und damit hergestelltes gelatinepulver Download PDFInfo
- Publication number
- WO2009135601A1 WO2009135601A1 PCT/EP2009/003018 EP2009003018W WO2009135601A1 WO 2009135601 A1 WO2009135601 A1 WO 2009135601A1 EP 2009003018 W EP2009003018 W EP 2009003018W WO 2009135601 A1 WO2009135601 A1 WO 2009135601A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- gelatin
- stream
- gelatin powder
- aqueous
- dispersion
- Prior art date
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L89/00—Compositions of proteins; Compositions of derivatives thereof
- C08L89/04—Products derived from waste materials, e.g. horn, hoof or hair
- C08L89/06—Products derived from waste materials, e.g. horn, hoof or hair derived from leather or skin, e.g. gelatin
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
- C08J3/122—Pulverisation by spraying
-
- 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
- C09H9/00—Drying of glue or gelatine
- C09H9/04—Drying of glue or gelatine in the form of granules, e.g. beads
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2389/00—Characterised by the use of proteins; Derivatives thereof
- C08J2389/04—Products derived from waste materials, e.g. horn, hoof or hair
- C08J2389/06—Products derived from waste materials, e.g. horn, hoof or hair derived from leather or skin
Definitions
- the present invention relates to a process for the continuous production of gelatin powder and a gelatin powder produced by this process.
- Gelatine is extracted with water, mostly animal, collagen.
- type A gelatin obtained by acid hydrolysis of the raw material and type B gelatin obtained by alkaline hydrolysis of the raw material.
- the gelatin solution is concentrated strongly by vacuum evaporator and then dried in a noodle form on a belt drier.
- filtered, dried and microbiologically clean air is used, which extracts the residual water from the gelatin, mostly in countercurrent mode. Due to the relatively low decomposition point of gelatin, this usually takes place at temperatures between 30 0 C and 6O 0 C.
- the gelatin noodles are powdered by milling and then standardized and classified by sieving.
- Spray drying is used in addition to the grinding and screening.
- Spray drying is the currently favored process for obtaining fine powders from solutions by evaporation of the liquid fraction.
- the liquid base substance is sprayed through a nozzle in a drying chamber.
- the atomization creates a spray of fine droplets.
- Rotary discs with rotation frequencies between 8000 l / min and 60000 l / min support the atomization of the material to be dried.
- hot air is introduced through another inlet in the spray tower. This is done depending on the application in the DC or in the countercurrent principle.
- the temperatures of the air flow are between 80 0 C and 600 0 C.
- the liquid content can evaporate within a few seconds and be discharged with the dry gas.
- the dissolved or suspended solid collects as a fine powder at the bottom of the drying chamber.
- plasticizers such as glycerol
- dusting agents such as carbohydrates or viscosity-reducing additives
- US Pat. No. 2,824,807 describes a process for the spray-drying of gelatin and gelatin-containing solutions in which a cooling zone is located immediately below the spraying device. This cooling zone is needed for droplet formation.
- the patent describes the applicability of the process for a 12% aqueous solution of a 285 bloom gelatin and a 30% aqueous solution of a gelatin of 30 bloom.
- the drying temperature is between about 120 0 C and about 540 0 C, the preferred drying temperature is reported to be approximately 300 0 C.
- the patent DE 37 26 963 describes a process for the preparation of a cold-water-soluble, instantized gelatin.
- the aqueous gelatin solution is removed from the preparation process at a temperature of 115 ° C. and sprayed onto dry gelatin particles circulating on a fluidized bed at an air temperature of 80 ° C.
- the water content of overdried gelatin is given as ⁇ 8%.
- vitamin E powders or processes for their preparation describe vitamin E powders or processes for their preparation.
- the vitamin E powders described there are obtained by spray-drying a vitamin E oil and gelatine as well as other additives. Gelatin having a "very low bloom number" and an average molecular weight of 9,000 to 11,000 was used. Further additives are, for example, sodium benzoate, sorbic acid and silica.
- the state of the art currently has the following possibilities for subjecting pure gelatine to spray-drying from an aqueous solution:
- the spray-drying of aqueous gelatin solutions of relatively high molecular weight gelatin with a very low dry matter content of less than 5% is known.
- the high water content of over 95% requires a lot of energy to dry this gelatin solution. Such a method is therefore very expensive.
- a second possibility is the use of hydrolyzed or partially hydrolyzed gelatin.
- This type of gelatin has a low molecular weight and forms only a very weak gel, which limits the possible applications.
- the tablettability of higher molecular weight gelatin is far better than that of low molecular weight gelatin.
- a higher amine content present in hydrolyzed gelatin will result in unpleasant odors when dissolved.
- hydrolyzed gelatin has a darker yellowish-brownish hue, which is undesirable in both the food and pharmaceutical industries.
- a third possibility consists in the mentioned establishment of a cooling zone directly below the atomizing member. This allows the formation of droplets of the aqueous gelatin solution, which are then dried in the heating zones of the spray tower.
- This device increases the maximum sprayable gelatin dry substance content to 12% with a gelatin bloom number of 285. If low molecular weight gelatin with a bloom number of 30 is used, the dry substance content of an aqueous gelatin solution can amount to a maximum of 30% in order to be spray-dried.
- the disadvantage here is that much energy must be applied to evaporate the least 70% water contained in the solution.
- Another disadvantage of this method is the use of very hot air (up to 540 0 C) as a dry medium. Resulting oxidation and temperature effects favor unwanted molecular degradation of the gelatin.
- the invention has for its object to provide a process for the preparation of gelatin powder, with which even high molecular weight gelatin efficiently powder with high purity, i. can be produced with the lowest possible proportion of undesirable foreign substances.
- Optionally valuable substances can be present in the resulting powders, if desired also in large proportions by weight.
- a method for the continuous production of gelatin powder comprising the steps specified in claim 1. Accordingly, a first stream of an aqueous gelatin-containing starting mixture under pressure and a second stream of compressed carbon dioxide and / or nitrogen are provided. Then, by combining these two streams, a dispersion is prepared under pressure. The dispersion obtained is expanded in a flash chamber whose temperature is above the dew point. line of the resulting mixture of the two streams resulting mixture of water and carbon dioxide and / or nitrogen.
- the starting mixture is a solution of gelatin in water.
- the gelatine powders to be produced additionally contain dispersed valuable substances, the starting mixture, i. the solution of gelatin in water, the desired recyclable material in dispersed form.
- the valuable substance may be lipophilic or lipophobic and mixtures of lipophilic and lipophobic recyclables may also be used.
- high molecular weight gelatin can be concentrated in high concentrations, i. up to a gelatin content of the aqueous starting solution of about 60 wt .-%, powdered in an energy-efficient manner and dried at the same time.
- the bloom number of the gelatin which can still be processed by the process according to the invention, starting from an aqueous solution with 50% by weight gelatin content, can be up to about 300.
- the average molecular weight of the gelatin used can be up to about 200,000 daltons.
- the process according to the invention requires, apart from the specified substances, no further additives for the formation of a powder, in particular therefore no shaping additives, so that high-purity gelatin powders with high gel power can be produced. Due to the gentle production by means of the method according to the invention, the average molecular weight of the gelatin used is hardly changed, which is why the resulting gelatin powder has a white color and releases no unpleasant odors when dissolved in water.
- the gelatin used in the process according to the invention may be type A or type B, and it is also possible to process gelatine mixtures.
- the residual moisture of the resulting gelatin powder is between 0.1 and 15 wt .-%, preferably between 6 and 13 wt .-%.
- the process according to the invention is also suitable for the production of valuable substances which are encapsulated with high molecular weight gelatin.
- valuable substances may be solid or liquid water-soluble, sparingly water-soluble or preferably water-insoluble, be lipophilic substances. Due to the encapsulation in high molecular weight gelatin, such ready-made valuable substances are for example well suited for tableting and are, for example, able to form an emulsion when dissolved in water.
- the step of dispersing at a temperature of 150 0 C or less is performed.
- the pressure in the expansion chamber in the process according to the invention is preferably 5 bar or less, more preferably about 1 bar.
- the step of preparing a dispersion is preferably carried out in a so-called static mixer known to those skilled in the art, but such is not necessarily required.
- At least part of the gas expanded in the expansion space (C0 2 and / or N 2 ) is dried, heated and returned to the expansion space. In this way, the fresh gas requirement of the method according to the invention can be reduced.
- Another object of the present invention is to provide a preferably high purity powder of high molecular weight gelatin.
- the bloom number of the gelatin contained in the gelatin powder according to the invention is up to about 300.
- the average molecular weight of the gelatin is up to about 200,000 daltons.
- the residual moisture of the gelatin powder according to the invention is between 0.1 and 15 wt .-%, preferably between 6 and 13 wt .-%.
- the gelatin powder of the present invention is one of high molecular gelatin, i. having an average molecular weight in the range of
- gelatin powders and gelatin-encapsulated recyclables prepared by the present invention are microcapsules for pharmaceutical agents. Due to the biocompatibility of gelatine, its widespread use in the pharmaceutical sector and the pH-dependency of the resuspension behavior, so-called controlled release systems can also be used. Also conceivable is the encapsulation of aroma substances for use in the food sector, if desired also with delayed release. Oxidation- and temperature-sensitive recyclables can be processed by the process according to the invention readily to give gelatine powders according to the invention, optionally as powder composites consisting of valuable materials dispersed in high molecular weight gelatin.
- a generally designated 10 apparatus for performing the method for gelatin powder production comprises a reservoir 12 for aqueous, gelatin-containing starting mixture 14 and a further reservoir 16 for the gas used in the process, in the example shown for carbon dioxide.
- the starting mixture is a solution of gelatin in water.
- the solution of gelatin and water is added to a valuable substance or mixture of useful substances. If it is a hydrophilic recyclable, it can be dispersed and dissolved in the solution of gelatin and water. If it is a lipophilic valuable substance, it is only dispersed in the solution of gelatin and water.
- a mixer for example, according to the rotor-stator principle (Ultaturrax), can be used.
- a liquid pump 18 sucks starting mixture 14 from the reservoir 12 and pumps the starting mixture 14 under pressure into a first supply line 20.
- a gas pump or a gas compressor 22 is supplied with carbon dioxide from the reservoir 16 and brings the carbon dioxide to a in a second Zuglassleii- 24 desired pressure.
- a heat exchanger 26 which flows through the compressed carbon dioxide and in which it is brought to a desired temperature.
- the two supply lines 20 and 24 open into a dispersion section designed here as a static mixer 28, in which a dispersion is produced from the two streams flowing through the supply lines 20 and 24.
- the dispersion obtained is expanded by means of a relaxation device 30, for example by means of a nozzle, in a first product container 32, one
- This relaxation room i. the interior of the product container 32, is maintained at a temperature which is above the dew point line of the mixture of carbon dioxide and water, which has formed in the dispersing by the merging of the two said streams.
- the aqueous fraction of the dispersion expanded in the product container 32 evaporates completely and dry, fine gelatin particles form, which collect at the bottom of the product container 32 and can be withdrawn therefrom.
- a starting mixture is used in which a lipophilic valuable substance is emulsified, then a dry powder is contained in the expansion space in which the lipophilic valuable material is dispersed in gelatin and at least partially encapsulated.
- a line 34 leads into a second product container 36, which serves to separate finest gelatin particles which have not separated in the first product container 32, but remain suspended in the gas flowing out through the line 34. These fines accumulate at the bottom of the second product container 36 and can be removed from there.
- a suction fan 38 draws the moist gas phase, ie the gaseous mixture of carbon dioxide and evaporated water, from the top of the second product container 36 and leads it either to the ambient atmosphere or, after appropriate treatment, to reuse.
- the suction fan 38 keeps in the product containers 32 and 36 constantly a slight negative pressure, which is a Ent- soft from carbon dioxide in the environment of the product container 32 and 36 reliably prevented.
- an aqueous solution of type B gelatin having a bloom number of 200 and an average molecular weight of 160,000 is charged.
- the concentration of gelatin in water is 40% by weight.
- Reservoir 12 is set to 85 0 C.
- the solution is compressed by means of the pump 18 to a pressure of 85 bar and fed as stream 1 to a static mixer.
- the mixer is fed as stream 2 compressed and preheated carbon dioxide, which is taken from a tank system liquid and undercooled, compressed in the pump 22 and brought to a temperature of 180 0 C in the heat exchanger 26.
- the mass flow of stream 1 is 2.1 kg / h.
- the mass flow of carbon dioxide is 46 kg / h.
- the static mixer the two streams are dispersed.
- At the end of the mixing section an average temperature of 142 ° C is measured.
- the dispersion of stream 1 and stream 2 is relaxed.
- the pressure in the expansion chamber 32 is about 1 bar.
- the relaxation room has a temperature of 55 ° C.
- a dry gelatin powder having a residual moisture content of 11% by weight is obtained.
- the average molecular weight is 130,000.
- a wet gas stream is withdrawn together with fines of dried gelatin powder. The fine fraction is separated from the moist gas stream in a downstream cyclone.
- an aqueous solution of type A gelatin having a bloom number of 100 is introduced in the receiving vessel 12.
- the concentration of gelatin in water is 40% by weight.
- the temperature in the reservoir 12 is set to 7O 0 C.
- the solution is compressed by means of the pump 18 to a pressure of 85 bar and fed as stream 1 to a static mixer.
- the mixer is fed as stream 2 compressed and preheated carbon dioxide, which is taken from a tank system liquid and undercooled, compressed in the pump 22 and brought to a temperature of 180 0 C in the heat exchanger 26.
- the mass flow of stream 1 is 2.5 kg / h.
- the mass flow of carbon dioxide is 60 kg / h.
- the two streams are dispersed.
- an average temperature of 132 0 C is measured.
- the dispersion produced from the stream 1 and stream 2 is released.
- the pressure in the expansion chamber 32 is about 1 bar.
- the relaxation room has a temperature of 67 ° C.
- a dry gelatin powder having a residual moisture content of 8% by weight is obtained.
- a wet gas stream is withdrawn together with fines of dried gelatin powder. The fine fraction is separated from the moist gas stream in a downstream cyclone.
- an aqueous solution of type B gelatin having a bloom number of 200 and an average molecular weight of 160,000 is charged.
- the concentration of gelatin in water is 50% by weight.
- soybean oil is dispersed by means of a rotor-stator mixer (Ultraturrax).
- the mass ratio of gelatin solution to oil is 3 to 1.
- the temperature in the reservoir 12 is set to 75 ° C.
- the mixture of gelatin, water and soybean oil is compressed by means of the pump 18 to a pressure of 70 bar and fed as stream 1 to a static mixer.
- the mixer is fed as stream 2 compressed and preheated carbon dioxide, which is taken from a tank system liquid and undercooled, compressed in the pump 22 and brought to a temperature of 155 ° C in the heat exchanger 26.
- the mass flow of stream 1 is 7 kg / h.
- the mass flow of carbon dioxide is 80 kg / h.
- the two streams are dispersed.
- At the end of the mixer an average temperature of 135 ° C is measured.
- the dispersion produced from the stream 1 and stream 2 is released.
- the pressure in the expansion chamber 32 is about 1 bar.
- the relaxation room has a temperature of 55 ° C. At the bottom of the flash room, a dry gelatin powder having a residual water content of 9% by weight is obtained.
- This gelatin powder contains 40% by weight of soybean oil.
- a wet gas stream is withdrawn together with fines of dried gelatin soybean oil powder. The fine fraction is separated from the moist gas stream in a downstream cyclone.
- an aqueous solution of type A gelatin having a bloom number of 200 is introduced in the receiving vessel 12.
- the concentration of gelatin in water is 25% by weight.
- soybean oil is produced by means of a rotor-stator mixer
- the mass ratio of gelatin solution to oil is 8 to 1.
- the temperature in the reservoir 12 is set to 75 ° C.
- the mixture of gelatin, water and soybean oil is compressed by means of the pump 18 to a pressure of 74 bar and fed as stream 1 to a static mixer.
- the mixer is fed as stream 2 compressed and preheated carbon dioxide, which is taken from a Tankanla- ge liquid and undercooled, compressed in the pump 22 and brought in the heat exchanger 26 to a temperature of 155 ° C.
- the mass flow of stream 1 is 4 kg / h.
- the mass flow of carbon dioxide is 80 kg / h.
- the static mixer the two streams are dispersed. At the end of the mixer, an average temperature of 135 0 C is measured.
- the dispersion of stream 1 and stream 2 is expanded.
- the pressure in the expansion chamber 32 is about 1 bar.
- the relaxation room has a temperature of 65 ° C.
- a dry gelatin powder having a residual water content of 11% by weight is obtained. This gelatin powder contains 20% by weight of soybean oil.
- This gelatin powder contains 20% by weight of soybean oil.
- 2o chamber is a wet gas stream together with fines on dried Gelati ne-soybean oil Pu I deducted.
- the fine fraction is separated from the moist gas stream in a downstream cyclone.
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Dermatology (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
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Abstract
Description
Claims
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE112009001020.2T DE112009001020B4 (de) | 2008-05-04 | 2009-04-24 | Verfahren zur kontinuierlichen Herstellung von Gelatinepulver |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102008021634.8 | 2008-05-04 | ||
DE200810021634 DE102008021634A1 (de) | 2008-05-04 | 2008-05-04 | Verfahren zur Herstellung von Gelatinepulver und damit hergestelltes Gelatinepulver |
Publications (1)
Publication Number | Publication Date |
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WO2009135601A1 true WO2009135601A1 (de) | 2009-11-12 |
Family
ID=40792926
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/EP2009/003018 WO2009135601A1 (de) | 2008-05-04 | 2009-04-24 | Verfahren zur herstellung von gelatinepulver und damit hergestelltes gelatinepulver |
Country Status (2)
Country | Link |
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DE (2) | DE102008021634A1 (de) |
WO (1) | WO2009135601A1 (de) |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2824807A (en) * | 1955-02-17 | 1958-02-25 | Gen Foods Corp | Spray drying process |
FR2628113A1 (fr) * | 1988-03-03 | 1989-09-08 | Nishibori Sadao | Procede de pulverisation de gelatine, et peinture, couche de revetement, film et tissu fini contenant la gelatine pulverisee, puis enlevee par elution |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3608083A (en) | 1968-06-05 | 1971-09-21 | Hoffmann La Roche | Vitamin e powder |
US3962384A (en) | 1972-04-10 | 1976-06-08 | Hoffmann-La Roche Inc. | Spray-drying technique for preparing agglomerated powders |
US3914430A (en) | 1972-04-10 | 1975-10-21 | Hoffmann La Roche | Free-flowing, high density, agglomerated vitamin E powder compositions |
DE2943267A1 (de) * | 1979-10-26 | 1981-05-07 | Basf Ag, 6700 Ludwigshafen | Verfahren zur herstellung von feinstverteilten carotinoiden |
DE3726963A1 (de) | 1987-08-13 | 1989-02-23 | Stoess & Co Gelatine | Kaltwasserloesliche, instantisierte gelatine und verfahren zur herstellung derselben |
-
2008
- 2008-05-04 DE DE200810021634 patent/DE102008021634A1/de not_active Withdrawn
-
2009
- 2009-04-24 WO PCT/EP2009/003018 patent/WO2009135601A1/de active Application Filing
- 2009-04-24 DE DE112009001020.2T patent/DE112009001020B4/de not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US2824807A (en) * | 1955-02-17 | 1958-02-25 | Gen Foods Corp | Spray drying process |
FR2628113A1 (fr) * | 1988-03-03 | 1989-09-08 | Nishibori Sadao | Procede de pulverisation de gelatine, et peinture, couche de revetement, film et tissu fini contenant la gelatine pulverisee, puis enlevee par elution |
Also Published As
Publication number | Publication date |
---|---|
DE102008021634A1 (de) | 2009-11-05 |
DE112009001020B4 (de) | 2016-05-25 |
DE112009001020A5 (de) | 2011-09-29 |
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