DK146191B - PROCEDURE FOR THE PREPARATION OF AN EATABLE COLLAGEN BEARS, SUCH AS A POULTRY ARM - Google Patents

Description

(1

(19) DENMARK

(12) PUBLICATION MANUAL OR 146191 B

DIRECTORATE OF

THE PATENT AND TRADEMARKET SYSTEM

(21) Patent Application No .: 4662/68 (51) Int.CI.3: A 22 C 13/00 (22) Filing Date: Sep 27, 1968 (41) Aim. available: 28 Mar 1969 (44) Submitted: 25 Jul 1983 (86) International Application No: - (30) Priority: 27 Sep 1967 US 670998 16 Sep 1968 US 759931 (71) Applicant: 'JOHNSON &JOHNSON; New Brunswick, US.

(72) Inventor: Paul Vincent 'Fagan; US.

(74) Clerk: Th. Ostenfeld Patentbureau A / S

(54) Process for preparing an edible collagen tube such as a sausage casing

The present invention relates to a process for preparing an edible collagen tube, such as a sausage casing, by extruding and inflating an optionally softener-containing, acid-swollen collagen mass to form a tube which is then dried and wrinkled. The product of the process according to the invention is especially intended for use as edible coating for fresh pork sausages to be cooked by the consumer.

From the specification of U.S. Patent No. 3,123,653, it is known that an extremely thin-walled collagen arm can be prepared from a liquid mass of acid-swollen collagen fibrils having a solids content of the order of about 3.5¾ to 5¾ by extrusion of 2) the liquid mass into a concentrated solution of ammonium sulfate which 2 coagulates and cures the tubular body. The cured tubular ^ body is washed, tanned and softened by passing through successive y baths, after which it is dried, while being inflated with gas Ω under pressure. The known method results in continuous lengths of a thin-walled intestine which can be stopped with pork tenderness, knotted on a so-called "FAMCO linker" and prepared by grilling, steaming or roasting in fat. However, the extrusion of a liquid mass of low fat collagen fibrils into a liquid coagulation bath and the subsequent handling of the extruded tubular body as it moves through the detergent, tanning and plasticizer solutions present difficult problems in manufacture. The extrusion of such a low solids aqueous material provides an extremely brittle tubular body which must be handled very carefully and carefully during subsequent treatments in which they are coagulated, cured, softened and dried.

Ώδϊϊ disclosed in U.S. Patent No. 3,123,653 to the manufacture of a tubular collagen arm requires four separate dissolution systems for treating the extruded material. It is a disadvantage of this method of preparation that the concentration of each solution must be kept at the proper value. This increases manufacturing costs as storage tanks, pumps, pipelines and instruments must be used and maintained ·

Another disadvantage of the above known method is that personnel are required to constantly examine the intestine as it enters and exits various solutions. Quality control is complicated by the large number of variables, such as the concentration, flow rate, temperature and processing time of the solutions. The intestine can be lost as a result of nodes, fractures and tears resulting from the transfer of the wet, weak intestine over cylinders and through the solution. In addition, significant losses of chemicals occur (ammonium sulfate, alum, citric acid, glycerol, carboxymethyl cellulose) and the problems of waste removal increase.

It has now been found that an extruded tube of acid-swollen collagen fibrils, while impermeable to air, is permeable to gaseous ammonia. Therefore, if the collagen tube, when formed, is inflated with a gas containing ammonia, the shape and diameter of the tube can be retained while neutralizing the acid present in the extrusion mass to form ammonium salts in the walls of the tube. The presence of ammonium salts in the walls of the tube does not alter the permeability of the tube to ammonia gas, which can penetrate through the wall of the tube and neutralize the acid-swollen collagen fibrils in its outer surface.

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The present invention is based thereon, and the method is characterized in that the tube is inflated when formed, at the extruder's nozzle, with a gas containing ammonia, that the tube is supported until the ammonia has neutralized the acid present in the extrusion mass, and if desired, when the collagen mass does not contain plasticizer, the neutralized tube washes and before drying it passes through a liquid plasticizer bath.

Therefore, in the process of the present invention, a homogeneous mass of acid-swollen collagen fibrils made of leather skin can be extruded directly into the atmosphere, avoiding the ammonium sulfate coagulation bath used in the above known process, and avoiding the curing step entirely. Therefore, much of the apparatus required by the known method for containing the various treatment baths and for transferring the wet intestine through these baths can be eliminated. Therefore, in the process of the invention, the collagen mass can be extruded and processed faster and better control of the process is achieved. An unexpected advantage of the process of the invention may be due to the ammonium salts which form and remain in the intestine. It has been noted that when such intestines are stopped, they have improved attachment properties, being readily attachable on a so-called "FAMCO linker" to form perfect "pig tails" as opposed to "open ends" which sometimes occur in certain types. extruded collagen casings.

If desired, the collagen mass may contain a plasticizer, preferably in an amount of from 10-20% by weight based on skin solids. The tube is inflated at the time of extrusion, with a gaseous mixture of air and ammonia, which prevents the tube from collapsing and reacts with the acid present in the extrusion mass to form ammonium salts during swelling of the collagen fibrils and increase in the tube. tensile strength. The ammonia gas penetrates through the wet wall of the collagen tube, neutralizing the acid found throughout the tubular wall. If the extrusion mass contains a plasticizer, the extruded and neutralized tube can be flattened between rollers, perforated and received on a drum for later drying or passed directly into a drying chamber in the inflated state. If the extrusion mass does not contain plasticizer, the extruded tube, after neutralizing the acid present with ammonia, is washed and passed through a liquid plasticizer bath prior to drying. According to the invention, it is preferred that the extrusion mass be softened with glycerol. Glycerol also acts as a wetting agent and binds the water in the tube so that glycerol is more effective in the process of the invention than other edible plasticizers.

It is further preferred by the method of the invention that the formed tube is temporarily passed through an outer atmosphere of gas containing ammonia. In this way, the neutralization of the acid and the hardening of the pipe are achieved uniformly.

The method according to the invention will now be described in more detail in connection with the drawing, in which fig. 1 is a side view of an apparatus for use in the method of the invention; FIG. 2 is an enlarged partial view showing the drive means; FIG. 3 is a vertical cross section taken along line 3-3 of FIG. 2, FIG. 4 shows a partially horizontal section along line 4-4 of FIG. 2, FIG. 5 is a time box diagram; and FIG. 6 shows a modified embodiment with a multiple arrangement of the apparatus.

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For understanding of the physical processing steps and apparatus used, reference is now made to FIG. 1, wherein a collagen extrusion mass is pumped into a rotary plate extruder 10 of the type shown in FIG. 1 of US Patent No. 3,122,788. The intestine 12 is inflated, while forming, with air flowing under pressure from a pipeline 192 through the extruder and into the interior of the tube. At the beginning of the process, the end of the tube is closed by folding so that the tube will contain the air and be inflated. Simultaneously with the introduction of air through the conduit 192, ammonia gas is fed into this conduit and into the interior of the extruded tube 12.

A container 15 open to the atmosphere at one end 16 surrounds the mouthpiece of extruder 10 and extruded intestine 12 as it moves. The intestine can be considered while inside this container through a window 17. Ammonia gas is fed into the container 15 so as to maintain an ammonia atmosphere surrounding the intestine as it moves through the container.

The extruded tube, as it moves away from the extruder, is supported on an endless conveyor belt 13 which may be made of a polyester resin such as MILLY LARV mounted on rollers 14 and 18. The roller 14 is motor driven and moves the conveyor belt in the direction of the arrow at the linear speed. by which the tube 12 is extruded.

At the end of the conveyor belt 13: a set of driven clamping rollers 20 and 22 collapses the tube and intercepts an air bubble which goes inside the tube 12 back to the extruder 10. Since the tube is. impermeable to air, the air supply is interrupted through the conduit 192 when the air bubble is established inside the pipe. It is desirable that the tube be inflated to a diameter equal to the extrusion diameter and to be held on this diameter until the extruded tube is cured. The flow of ammonia gas through the conduit 192 and into the container 15 is continued at a rate sufficient to completely neutralize all the acid present in the tube prior to its collapse by the rollers 20 and 22. It should be noted that the movement of the conveyor belt 13 and of the clamping rollers 20 and 22 are adapted so that the bowel moves at a constant speed away from the extruder under little or no linear stretch of the bowel.

A measuring instrument 23 continuously measures the diameter of the inflated bowel 12 and controls the air pressure inside the bowel. If the diameter 'of the intestine falls below the extrusion diameter, a signal is emitted by the instrument 23 and measured by a pointer instrument. If the signal varies beyond predetermined limits, it controls an air control valve (not shown) to increase the air pressure inside the intestine, inflating it to its extrusion diameter.

The bowel moving from the conveyor belt 13 falls into a basket 24 in a water wash tank 40 and is transported through the tank by a series of cylinders 25,26,27,28,29,30 and 31. As will be seen in FIG. 3 and 4, each cylinder is driven by a shaft 32 and tapered gears 33 and 34. The gear 34 is mounted on a shaft 35 driven by a motor 36 by means of a belt 37 and a fixed pulley 38.

Vertical surfaces 39 under each cylinder form spaces which retain the folded bowel and prevent it from becoming untidy during leaching. As will be seen from FIG. 1, water circulating in the tank 40 passes through holes 42 in the vertical plates 39 and washes the intestine ugly.

The washed intestine from the tank 40 is transferred to a softening tank 44 by the cylinder 45 which folds the intestine so that it falls into a compartment 46. The folded intestine is removed from the bottom of the compartment 46 by the cylinder 47 and transferred to the the space '48, from which it is removed by the cylinder 49. The spaces 46, 48 and 50 are formed with openings in the vertical walls which cooperate with the softening solution.

The intestine is removed from the softening tank 44 by means of a motor-driven cylinder 51 which precedes the dryer. The softened and collapsed bowel passes as it leaves the container 44, over a series of intermediate rollers, and pierces at intervals of approx. 10 cm of a reciprocating needle 52. These small bowel holes in the intestine facilitate later drying. A clamping roller 53 in combination with the driven roller 51 seals the intestine which enters the dryer, and permits inflation of the intestine with air into the dryer.

The dryer will not be described in more detail as it is similar to that disclosed in U.S. Patent No. 3,123,653. However, the drying chamber is divided into separation rooms to form three chambers, each of which can be supplied with warm air of different temperatures. The intestine is inflated again as it passes into the dryer for the drying and wrinkling operation.

Collagen materials containing between 0.6% by weight and 1.19% by weight of lactic acid have been successfully produced by the process of the present invention, but unless the gut is washed with water after the extrusion and neutralization with ammonia, it is preferred to reduce the acid concentration to the least possible which will satisfy the swelling of the collagen fibrils, 7 146191 so as to avoid excess ammonium lactate in the finished product. Other acids which form edible ammonium salts, such as acetic acid or hydrochloric acid, can be used instead of lactic acid as a swelling agent.

The invention will now be further elucidated in connection with exemplary embodiments in which all quantities are expressed in parts by weight, unless otherwise stated.

Example 1

Fresh hides were washed with cold water at 60 ° C or less in a rotating drum for 10 to 24 hours. After washing, the hides of meat were freed with a scraper, and the hairs and epidermis were cut away with a horizontal ribbon knife. This preliminary cleaning was done with the usual tanning equipment.

The remaining hair and poorly cleaned sections were cut off by hand and blend products prepared from five hides. The skin products were cut into sections of approx. 3.2 to 25.8 cm and was reduced to pulp by three passes through a meat grinder using a finer grinding for each passage. The first and second passages were made through holes 18 and 8 mm in diameter, respectively. The final grinding was carried out through holes with a diameter of 1.5 mm. During the grinding step it is important to keep the pulp below 20 ° C. This can be done by adding crushed ice to the hides as they are fed to the grinder.

The finely ground leather skin was swollen with lactic acid and mixed with cellulose fibers and glycerin as described in Example VII of U.S. Patent No. 3,123,482 to a suitable homogenizer. The extrusion mass of acid-swollen collagen fiber glasses thus obtained had the following composition:

Solid leather skin fabrics: 3.55¾ Lactic acid: 0.70¾

Cellulose: 0.71¾

Glycerin: 1.00¾

Water: 94.04¾

The homogenized mass was pumped from a storage tank through a coiled wire filter with openings of 0.4 x 2.5 mm and extruded through a plate extruder of the type shown in FIG. 1 of the United States patent no.

3,122,788 shown. With cooling water circulating through the extruder sheath, the inner and outer plate members were rotated at 91 rpm. and the collagen mass is extruded at a rate of 252 g (30 feet) per minute. minute. The fitting on this extruder, which is normally used for supplying a concentrated ammonium sulfate solution to the interior of the collagen tube (Pipeline 192), was connected to a gaseous ammonia source 8 146191, and another tube connected to the interior of the extruded tube (192 ) was connected to a source of compressed air. The airflow was adjusted to approx. 1500 cm / min and the flow of ammonia gas was adjusted to approx. 4000 cm / minute. This flow of air and ammonia provides sufficient pressure to inflate the tube as it exits the inner portion of the extruder nozzle. The flow of air was gradually lowered to avoid inflating the tank to a diameter greater than that at which it was extruded (18 mm) and could be interrupted after a few minutes of operation when the air bubble interconnected between extruder 10 and clamping rollers 20 and 22 had stabilized. . The flow of ammonia gas was continued by approx. 4000 cm / min (3.4 g NH 3 per minute).

As the ammonia gas penetrates the intestine, the lactic acid is immediately neutralized, which proceeds from the intestinal wall to the outer wall. This is seen by a 5-6 ° rise in temperature between the extruded tube leaving the nozzle and a point approx. 45 cm from the nozzle, occurs. It is preferred to limit the high estrous temperature resulting from the neutralization to 34 ° C by appropriate means which may consist in cooling the extrusion mass as it enters the extruder, increasing the extrusion rate or decreasing the flow rate of the ammonia gas. Lowering the amount of ammonia to approx. 2.0 g / min will reduce the temperature rise due to neutralization, but the flow rate of ammonia gas should not be lowered to a value where the extruded intestine becomes too soft to handle comfortably. Increase in ammonia gas flow to above approx. 3.4 g per per minute will increase the temperature of the intestine due to the neutralization but has little effect on the rate at which the intestine is cured.

The wet strength of the extruded intestine will grow over time as the ammonia causes neutralization. 5 to 7 minutes after extrusion, the gut has a wet tensile strength of 336 to 376 g.

The intestine from the conveyor belt 13 can be inflated with air and passed directly to the first section (24.4 m linear) of a drying chamber which is heated to 71 ° C. The residence time of the intestine in the first section 2 of the drying chamber is approx. 2j minutes. The inflated bowel then enters another section (7.8 m linear) of the drying chamber which is heated to 56 ° C. The residence time of the intestine in the second section of the drying chamber is approx. 1 minute. The inflated intestine then enters a third section (4.2 m linear) of the drying chamber. The temperature in this third section is approx. 32 ° C and the residence time of the intestine is approx. \ minute. When the bowel exits the third section of the dryer, it is wrinkled on the apparatus disclosed in United States Patent No. 3,315,300.

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The gut thus obtained contains about 10% by weight (based on solid collagen) of ammonium lactate and can be used with excellent results in the preparation of pork sausages.

Example .1

A collagen dispersion of the following composition was prepared and extruded as described in Example I above.

Skin 3,551

Glycerin 0.751

Cellulose 0.71¾ Lactic acid 0.70¾

Glucose 0.01¾ The wet tensile strength of the clamping rollers 20,22 is 280 g. The gut from the conveyor belt 13 can be diverted to the dryer (without washing or softening) and dried at a temperature of approx. 71 ° C for approx. 3 minutes and at 55 ° C for approx. 2 minutes. The intestine is then cured by heating to a temperature of 32 ° C for a period of 8 hours, keeping the intestine at this temperature for an additional 12 hours.

The intestine thus obtained is stopped with pork, giving a product which can be knotted without difficulty, to obtain an excellent final appearance. The sausages thus obtained are well prepared.

Example .3

The procedure of Example I was repeated, using instead of lactic acid, 0.084¾ (wt.%) Hydrochloric acid to swell the collagen fibrils. The intestines thus obtained contained approx. 1% by weight ammonium chloride and were suitable for use in the production of pig sausages.

Example 4 Skin Preparation

Hides from freshly slaughtered animals were cut and corrected. They were washed and softened for approx. 16 hours in urban water at approx. 16 ° C. The following day they were scraped and taken.

For a mixing vessel with a capacity of approx. 4200 1 was set approx.

2880 kg of water and approx. 1270 kg of scraped skin. 44.5 kg (3.5¾) of lime, 26.8 kg (2.1¾) of sodium sulfhydrate and 11.1 kg (0.875¾) of sodium sulfide were added to the vessel, and the mixer ran for one hour and stopped for one hour. Then the mixing means ran for 5 minutes every 3 hours.

When 24 hours had elapsed, the vessel was emptied of liquid and the hides were washed with urban water (16 ° C) for 15 minutes, drawn and scraped. The scraped hides were returned to the mixing vessel and washed clean with spring water at 16 ° C. The washed hides were then split on a leather splitting machine and the leather skin layer was further processed to make the collagen for the extrusion.

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A large wooden drum (capacity 5500 l) was filled with 527 kg of leather skin prepared as described above. The skin was washed in the drum for 9 hours at a flow rate of 13 liters per hour. minute. The wash water was removed from the leather skin and the washed leather skin was treated in the drum with 1320 L of water containing 3.83 kg of anhydrous citric acid and 3.03 kg of sodium citrate dihydrate. The drum rotated for 8 hours, after which the citrate solution was removed and the hides washed for 2 hours with running water.

The leather skin was re-treated once more for 8 hours with a solution containing 3.83 kg of anhydrous citric acid and 3.03 kg of sodium citrate dihydrate in 1320 liters of water and finally washed with water 182 hours in the drum. The skin was shredded and ground to a particle size of approx. 6 mm.

Example 5

Preparation of extrusion mass

A mixture of 32.9 kg (15.1 kg of dry skin material) of 6 mm ground skin particles was prepared as described in Example IV, and 109 l of water at 14 ° C was passed through a fast-running cutting mill in which the skin particles were shredded with fast-rotating blades to form a hydrated mass of fibrous nature.

In a stainless steel container, 2.87 kg of cellulose fibers were thoroughly dispersed in 186 liters of water. To this cellulose dispersion was added 1.22 kg of 37% hydrochloric acid under complete mixing. The mass of fibrous hydrated collagen from the fast-running cutting mill and the acid-cellulose water mixture was pumped at the same flow rates through a common pipeline into a storage tank. Mixing of the collagen particles and cellulose occurs as the two solutions move through the common pipeline during acid swelling of the collagen particles. After storage for a period of 18 to 24 hours, the mixture of cellulose and acid swelling collagen was further dispersed with an appropriate homogenizer such as a Manton-Gaulin homogenizer (Model 125-K-5BS) equipped with a two-way valve and adjusted with a pressure tag of 1500 p.s.i. per. step. The homogenized mixture was pumped to a storage tank and freed from air under vacuum. The extrusion mass thus obtained had the following composition: 3.55¾ solids 0.72¾ hard wood cellulose 0.12¾ hydrochloric acid

Example 6 Extrusion

The homogenized extrusion mass prepared as described in Example V above was pumped from the storage tank through a x 2.5 orifice wire filter and extruded through a plate extruder of the type shown in FIG. 1 of U.S. Patent No. 3,122,788. The extruder was cooled by circulating fluid through the jacket at 9 ° C. The extruded collagen arm is inflated with air and anhydrous ammonia, adjusted in the interior of the intestine at a rate of about 1.6 g / min and in the outer vessel 15 surrounding the intestine at a rate of 3.4 g / min. The temperature of the extruded collagen increased as a result of the work done on the extruding mass of the rotating extruder plates and as a result of the heat of neutralization. The maximum temperature of the intestine should not rise above 34 ° C. The diameter gauge 23 was adjusted to check the diameter of the extruded intestine of 26-1 mm.

The extruded intestine flattened between the clamping rollers 20 and 22 and dropped from the end of the conveyor belt 13 into the basket 24 of the water-washing tank 40. The wet breaking strength of the intestine when leaving the conveyor belt was 382g. The intestine was transferred through a number of compartments in the tank 40 by means of the cylinders 25,26,27,28,29,30 and 31 and subjected to intimate contact with the wash water which circulated through the openings 42 in the walls of each compartment. The total residence time of the gut in the water wash tank 40 (see Fig. 5) was 35 minutes and the flow rate of fresh wash water through the tank 40 was 13 liters per minute. minute. The wet pressure of the intestine after the water wash was 703 g.

The softener in the softener tank 44 is an aqueous solution of 4.5¾ glycerine and 1.0¾ carboxymethyl cellulose which circulates through the tank 44 at a flow rate of 6 liters per minute. minute. The total residence time of the intestine in the softening tank 44 was 7.5 minutes. Openings in the vertical walls of compartments 46, 48 and 50 interact with the softening solution in tank 44 and ensure intimate contact between the intestine and the soaking bath. The wet strength of the gut when leaving the soaking bath was 750 g. The gut from the soaking bath was dried and wrinkled as described in Example I above. The temperature of the first section was kept at 81 ° C and the temperature of the second and third sections was kept at 72 ° C.

The wrinkled intestine was heat cured by gradually increasing the temperature from 25 to 75 ° C over a period of 12 hours and leaving the intestine at 75 ° C for an additional 3 hours. The cured intestine was then wetted in a room of constant humidity to a moisture content of approx. 12 to 14¾, which is satisfactory when using the intestine for fresh pork sausages.

An improved strength intestine sufficient to withstand the stresses, high speed frankfurter and knotting apparatus can be obtained by heat curing the wrinkled bowel at a higher temperature. For example, the intestine can be heated in an oven from room temperature to 90 ° C over a period of 12 hours and kept at 90 ° C for an additional 12 hours before wetting.

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Example 7

To 8.3 kg of ground, decalcified skin particles (2.7 kg of dry matter) prepared as described in Example IV was added 29.7 l of water. The mixture was treated as described in Example V in a fast-running cutting mill (micro-cutter molds) to produce an aqueous slurry of collagen fibers. This mixture contained a total of 2.7 kg of leather skin on a dry basis.

A cellulose dispersion was prepared using 0.57 kg of cellulose, 36.8 l of water and 0.60 kg of 88¾ lactic acid. The mixture of this cellulose-lactic acid-water dispersion with fibrous collagen slurry was made as described in Example V, and the mixture was homogenized using a total pressure of 205 atm. through a two-stage homogenization valve. The extrusion mass thus obtained was extruded as described in Example VI, with the flow of anhydrous ammonia gas to the interior of the extruded intestine being 3.4 g / ml. The flow of ammonia gas to the gut surrounding the gut was 6.8 g per minute. minute.

The extruded intestine was treated as described in Example VI, keeping the diameter of the intestine at 26 ~ 1 mm throughout the extrusion. The flow rate of water through the wash tank was 13 L per liter. The total residence time in the water wash tank was 50 minutes.

The plasticizer in container 44 was identical to that of Example VI. The flow rate of fresh softening solution through the tank was 6.5 liters per liter. minute. The total residence time in the soaking tank 44 was 7.5 minutes.

The softened intestine thus obtained was dried as described in Example I, holding the first section of the dryer at 82 ° C and the second and third sections of the dryer at 72 ° C. The wrinkled intestine was heat cured by gradually increasing the temperature from 25 to 75 ° C over 12 hours, and the intestine was then kept at 75 ° C for an additional 3 hours. Next, the intestine was wetted to a moisture content of 12-141 and was acceptable for use in fresh pork sausages.