DE2439233A1 - METHOD OF REMOVING SOLVENTS FROM PROTEIN MATERIAL - Google Patents

Description

The invention relates to a method for removing solvent made of protein material.

The aim of the invention is to obtain a way of removing residual solvents from a protein material that has been extracted with a solvent or contains a solvent, optionally after mechanical separation of excess Solvent to remove very small residues without heating the protein material in such a way that that a thermal denaturation and thus a loss is more important

509815/1241

functional properties of the protein material, such as coagulability, Swellability, water and oil binding capacity will.

Another object of the invention is to provide a coagulable and swellable desolventized protein such as animal protein from fish or vegetable protein from soybeans and rapeseed.

Yet another object of the invention is to provide a way to solvent on a protein material can be removed even if it has already been denatured by heat after previous treatment, without influencing the color of the end product too much.

It is known that by direct treatment with steam and thus heating the protein material to temperatures can remove the solvent very largely near 100 ° C, but because the protein is above its denaturation point has been heated, the disadvantage arises that the protein retains its functional properties such as coagulability and water-binding ability, completely loses.

Protein material treated in this way, after drying, gives a sandy feel when it is eaten, so it is suitable for the in most cases it becomes unsuitable as an additive to water-containing foods such as fish and meat products.

By treating the protein material with direct hydrogen a change in color was obtained on evaporation which was complete when the protein material was added to light-colored foods was obviously at a great disadvantage.

509815/1241

ORIGINAL INSPECTED

It has now surprisingly become possible with the aid of the present invention to eliminate these disadvantages and at the same time to obtain extensive solvent evaporation. \

The invention is characterized in that the protein. '■ material treated with water-containing air, the temperature and the relative humidity of the air being adjusted in this way that enough energy is supplied for the evaporation of the solvent, and at the same time water is condensed from the air and replaces the amount of solvent that has evaporated.

According to one embodiment of the invention, the treatment takes place using water-containing air at a temperature of 40 to 90 ° C.

According to a further preferred embodiment of the invention the treatment of undenatured protein is carried out using water-containing air which has a temperature from 40 to 70 ° C., expediently from 45 to 65 ° C., preferred from 45 to 55 C.

According to yet another preferred embodiment of the invention the protein material is treated with water containing air in an amount of 1.0 to 5.0 m / kg of treated protein material,

3 treated preferably in an amount of 2.0 to 3.0 m / kg Treated protein material.

According to a further advantageous embodiment of the invention the water-containing air is saturated up to at least 50%, preferably 70%, preferably 100%.

According to yet another advantageous embodiment of the invention the treatment of the protein material is continuous

509815/12 * 1

borrowed in a vertical column with the help of water-containing air carried out in countercurrent to the stream of material, the column being heated indirectly to a temperature which is below the temperature of the air introduced is, specifically expediently at 10 to 30, preferably 10 to 15 c, with the water-containing Air is conveniently distributed to some different heights in the column.

According to another advantageous embodiment of the invention, the temperature exceeds that introduced into the upper part of the column, water-containing air is the temperature of the water-containing air introduced into the lower part of the column, the air introduced into the upper part is introduced in such an amount and at such a temperature that the temperature of the material in this part of the column by solvent evaporation essentially the same as the temperature of the material is in the lower part of the column.

Solvent-containing protein material is such protein material to which solvents have been added for reasons of shelf life or which contains solvents after an extraction. Solvents used for extraction are usually isopropanol, n-butanol, sec-butanol, isobutanol, ethanol, ethyl acetate, Acetone, chlorinated hydrocarbons and hexane. These solvents are used individually or in combination with each other used.

The protein material can be of animal or vegetable origin, such as protein from slaughterhouse waste, fish, crustaceans or aquatic mammals or protein from soybean

509815/1241

beans and rapeseed or protein from a culture of microorganisms on hydrocarbons.

Protein material that is at a temperature above the denaturation point of the protein has been heated, usually 60 to 70 C, quickly loses its functional properties, i. among other things its ability to absorb and bind water. This property is very valuable and necessary when The protein can be added as a substitute protein to products of animal origin, such as meat fillings, sausages and fish is supposed to preserve the structure and the cohesiveness of these foods. When using larger amounts of Denatured protein does not bind you, but the products fall apart.

Denatured protein also has a sand-like character, which makes the products rough to the touch in the mouth, when you eat them. If the functional properties are left in the protein, the sand-like character does not appear but the products feel natural.

example 1

In a column for evaporation of solvent, which is interrupted by a stirrer in the shape of a spiral the circumference of which was 10 mm in diameter and 200 mm in height was extracted with solvent Fish material introduced in the amount of 200 g. The protein material consisted of 61.5% dry matter, 25.5% Isopropanol and 13.0% water.

509815/1241

At the bottom of the evaporator, water-containing air was drawn in at a rate of 2.0 m / h. introduced with effective stirring.

The air saturated with water was obtained by adding air to the Bottom of a water-containing closed boiler of a certain temperature was introduced, whereupon the air directly into the Bottom of the evaporator was introduced.

The test was carried out using air saturated with water at four different temperatures. The evaporation capacity is directly dependent on the amount of energy supplied and is therefore in a certain volume of equipment adjusted by the amount and temperature of the air saturated with water. According to a table about the properties of moist air is the heat content of air saturated with water, calculated per kilogram of air at 40 ° C 39.6 kcal / kg, while the energy content of air at 50 ° C, 60 ° C, 70 ° C, 80 ° C and 90 ° C is 65.3, 109, 190, 363 and 912 kcal / kg, respectively.

In Table I below, the dry matter (TS) and the isopropanol (IPA) remaining in the material are different Time indicated. The evaporator column, which was surrounded by a jacket, had a temperature of 10 ° C was below that of air saturated with water.

509815/1241

Table I.

Air 40 ° C Air 50 ° C Air 60 ° C Air 70 ° C Time (min.) TS% IPA% TS% IPA% TS% IPA% TS% IPA%

10 68.8 11.9 69.0 0.062 68.5 0.044 68.2 0.047

15 71.2 2.95 67.5 0.049 66.7 0.032 64.2 0.017

30 69.0 0.064 63.9 0.025 61.1 0.014 54.7 0.004

45 67.6 0.048 58.4 0.005 56.2 0.003

60 6.4.2 0.027 55.2 0.003 46.0 0.002

As can be seen from the above results, substantial solvent evaporation is obtained very quickly, which after 60 minutes or earlier has progressed so far that only up to 270 ppm remained in the moistened material. In the subsequent drying this residue is further reduced and is only 10 to 30 ppm in the dry material. For this reason, this evaporation can be interrupted after 15 minutes if air at 50, 60 or 70 C used, or it can be interrupted after about 30 minutes if air at 40 ° C is used, since the then obtained After drying, material contains only 20 to 40 ppm isopropanol, which is an extremely low value. The drying takes place at 35 ° C with inflation of dry air. 15-minute blowing with water-saturated air according to The above statements correspond to an air volume of 2.5 m / kg protein material.

Example 2

A solvent evaporation according to Example 1 was carried out with unground or ground products, with water

509815/1241

this saturated air with a temperature of 50 ° C was used. The shell temperature was 40 ° C. The unground product had a particle size corresponding to the following distribution: 18% <5 to 3 mm, 13% <3 to> 2mm and 69% £ 2mm. The ground material had a particle size of <^ 2 mm. The results are summarized in Table II below. The amount of protein material introduced was 400 g with a content of 68.7% dry matter, 15.8% isopropanol and 15.5% water.

Table II IPA% Ground product Ungrinded product 2.83 TS% IPA% Time TS% 0.898 76.4 2.66 10 75.5 0.084 76.4 1.03 15th 75.6 0.027 74.6 0.053 30th 74.1 0.018 72.0 0.008 45 71.1 68.4 0.002 60 68.4

As can be seen from Table II, a satisfactory one is obtained Result also with the unground product, showing that extracted fish material was not prior to evaporation must be redistributed. The differences shown with regard to the remaining amounts of solvent are such that a further equalization is obtained when the material is finally dried.

The products obtained according to Examples 1 and 2 had retained their functional properties and showed good swelling

509815/1241

in water, with the exception of the experiment with an air temperature of 70 C, where the onset of coagulation was observed became.

Example 3

In a vertical column equipped with a stirrer in
the shape of a spiral interrupted at the periphery and
with a diameter of 300 mm, became a solvent
extracted fish protein introduced at an altitude of 3200 mm. The stirrer was rotated at a speed of 15 rpm. The column, which was provided with a jacket, had a temperature in the jacket of 40 ° C.

The protein material introduced into the column consisted of mit
Isopropanol extracted herring with a content of 55.6%
Dry substance, 38.2% isopropanol and 6.2% water. The temperature of the material at the time of introduction was 20 C. The test is carried out with continuous evaporation, with an amount of 18 kg / hour. was carried on protein material. The height of the material in the column was kept constant. The test was in
divided into two successive parts, namely 1. a treatment with water-saturated air, which had been obtained according to Example 1, at a temperature of 55 C and in one

3
Amount of 60 m / h introduced at the bottom of the column and 2. after 145 minutes of treatment using water-saturated air at a temperature of 55 ° C and in one
Amount of 30 m / h, introduced at the bottom of the column, and using air saturated with water at a temperature of 80 ° C and in an amount of 30 m / h

509815/1241

- OK -

upper part of the column was introduced. The results of the test are shown in Table III below.

* Table III

Time TS% IPA %

45 62.7 22.2

65 62.2 21.4

105 61.7 18.6

145 64.9 15.6

155 63.4 12.83

175 65.7 9.28

195 67.2 4.64

205 67.0 1.91

As can be seen from Table III, a better result is obtained with a continuous process when using water saturated air is also introduced in the upper part of the material package, this air having a temperature which higher than those introduced in the bottom of the evaporation column Is air, but the temperature of the material in the upper part is not the temperature of the water-saturated air in the exceeded the lower part of the column, as can be seen in Table IIIA below.

509815/1241

Table IIIA

Top of the upper half middle of the lower half-bottom of the

Column of column column te of column column time oc oc o _c o _c o _c

30th 40 = 41 40 39 37 65 42 42 41 41 39 85 39 41 42 42 40 145 39 41 42 42 40 155 46 44 44 43 41 175 50 47 46 44 42 205 53 50 48 46 43 235 55 52 49 47 44 265 55 53 50 48 45

When the test was continued, the following results were obtained according to the following table IHB.

Table IHB IPA% Time (min.) TS% 0.5 15th 66.2 0.2 30th 65.8 0.06 45 65.4 <O, O25 60 65.0

The capacity of the column can thus be fully used by inserting the columns at different heights water-containing air distributed, whereby the air in the upper parts of the column can get a temperature that is higher than that of the air introduced in the lower part, but with the treatment of undenatured protein the temperature denotes

509815/1241

Should not exceed the denaturation point of the material. The temperature and the amount of air should be selected so that the temperature of the material in the upper part is not the temperature of the air saturated with water in the lower part of the column exceeds. By distributing it at different heights, the supplied energy can be increased, which of course higher capacities results.

Example 4

The effect of final drying on the residual amount of solvent in a material subject to evaporation with saturated water Air according to the invention, and in a directly dried material that does not undergo such evaporation is listed in Table IV below, in which different materials with different amounts of dry matter and isopropanol before and after drying after evaporation with water-saturated air and a base material, that has not been subjected to evaporation but has been dried directly. The drying took place at 35 ° C below Use of air sweeping over it.

Tabel Evaporation H., 0% IV To Final drying H ₀ O% To IPA% 31.0 TS% IPA% 5.97 TS% 3.91 32.3 93.8 0.233 6.32 65.1 1.91 33.1 93.6 0.083 6.35 65.8 1.25 33.4 93.6 0.053 6.56 65.6 0.98 93.4 0.040 65.6

509815/1241

Before drying After drying

55.6 38.2 6.2 92, O 6.86 1.14

As can be seen from Table IV, one gets an extremely improved one Final drying result when the material is first evaporated using air saturated with water was subjected.

Example 5

The importance of the water in the evaporation air is from the The following test can be seen in which 200 g of test material with 65.1% dry matter, 25.8% isopropanol and 9.1% water e on the one hand with water-saturated air and on the other hand with non-water-saturated air (maximum 35% relative humidity) in an amount of 2 m / h. during 45 minutes and at an evaporation temperature of the air of 30, 40, 50 and 60 C were treated. In each experiment, the jacket temperature was kept 10 ° C. below the temperature of the water-containing air. The result after 45 minutes is shown in Table V below.

Tabel V IPA% H ₀ O% Air type Evaporation
temperature TS% 0.91 18.7 With water 30th 80.4 0.21 21,, 8 saturated 40 78.0 0.053 23.5 air 50 76.4 0.036 . 25.5 60 74.5

509815/1241

Not with 30th 87.7 5.06 7th , 2 Water ge 40 90.7 5.10 4th , 2 satiated 50 • 93.9 6.09 + 0 air 60 94.2 6.44 + 0

The results show a noticeable difference between the two different evaporation methods, the second being Method must be viewed more or less as a drying method.

Example 6

A number of experiments were carried out to determine the applicability of the method with different solvents and materials to show. In Table VIA is an evaporation test with Press cake flour from Sardinella, extracted with isropanol and with a content of 65.1% dry matter, 25.8% isopropanol and 9.1% water. 350 g of test material were with water-saturated air with an inlet temperature of 50 C and in an amount of 2 m / h. treated in a column that was provided with a jacket, the jacket temperature being 40 ° C.

Table VIA TS% IPA% H ₀ O% Evaporation
time (min.) Outlet gas temperature
temperature (° C) 64.1 24.4 9.5 2.5 32 68.3 19.1 12.6 5 35 71.8 7.6 20.6 10 36 73.7 1.81 24.5 15th 39

509815/1241

20 42 72.0 0.389 27.6

25 43 70.8 0.162 29.0

30 44 69.0 0.082 30.9

45 44 64.0 0.030 36.0

60 44 57.8 0.013 42.2

The same experiment was carried out using press cake flour which had been extracted with sec-butanol, the extracted material containing 56.8% dry matter, 18.7% sec-butanol and 24.5% water. The result is in Table VIB listed.

Table VIB

Evaporation outlet gas temperature (min.) Temperature (° C) TS% IPA% H ₀ O%

2.5 35 56.9 18.2 24.9

5 38 58.1 14.5 27.4

10 39 60.6 6.56 32.8

15 40 60.7 1.81 37.5

20 41 60.4 0.77 38.8

25 44 59.2 0.24 40.6

30 44 57.3 0.075 42.6

45 44 52.3 0.022 47.7

60 44 47.1 0.007 52.9

The same experiment was carried out with press cake flour which had been extracted with hexane, which extracted Material contained 70.4% dry matter, 21.5% hexane and 8.1% water. The result is in the following table VIC listed.

509815/1241

Table VIC

Evaporation
time (min.) Outlet gas temperature
temperature (° C) TS% Hexane% H ₀ O% 2.5 23 80.4 10.7 8.9 5 24 88.1 0.85 11.0 10 41 84.8 0.095 15.1 15th 43 83.0 O, O6O 16.9 20th 44 81, 4 0.025 18.6 25th 44 79.1 0.021 2O, 9 30th 44 77.7 0.015 22.3 45 44 72.8 0.013 27.2 60 44 67.4 0.010 32.6

The same experiment was also carried out on soybeans extracted with hexane, which extracted Material 79.5% dry matter, 11.4% hexane and 9.1% water contained. The results are shown in Table VID.

Table VID

Evaporation
time (min.) Outlet gas tempe
temperature (° C) TS% Hexane% H ₀ O% 2.5 28 88.6 0.515 10.9 5 32 87.0 0.178 12.8 10 40 85.3 0.120 14.6 15th 42 83.8 0.095 16.1 20th 43 82.2 0.075 17.7 25th 44 80.3 0.050 19.6 30th 44 78.5 030 21, 5 45 44 71.6 0.018 28.4 60 44 64.5 0.011 35.5

509815/1241

The results show that the choice of solution or the The choice of material has no influence on the evaporation effect, but you get a satisfactory result different types of solvent and material.

Example 7

An experiment was carried out to determine the effect of the amount of water to show in the water-containing air. Evaporation of isopropanol was carried out in accordance with that listed in Table VIA Procedure, but carried out with the difference that the air is saturated to 50 ° C and 100% before the introduction in the evaporation column was heated to 60 C, the degree of saturation was lowered to 57%. The result of evaporation can be seen from Table VII below.

Table VII TS% IPA% H _n O% Evaporation
time (min.) Outlet gas temperature
temperature (° C) 65.1 22.1 12.8 2.5 35 67, 7 16.3 16.0 5 37 73.0 3.60 23.4 10 40 73.1 0.471 26.4 15th 44 72.6 0.153 27.2 20th 45 71.3 0.097 28.6 25th 45 69.8 0.049 30.2 30th 45 67.1 0.031 32.9 45 45 63.3 0.016 . 36.7 60 45

509815/1241

Since the outlet temperature had just risen 1 C (cf. Table VIA, above) compared to evaporation using of water-saturated air at 50 ° C, this shows that the excess heat in the air that is not saturated with water is consumed during the passage through the packing material. This can also be done by means of a somewhat faster evaporation of residual isopropanol at the start of evaporation and based on a slightly lower water condensation in the product. The requirement for efficient evaporation is that enough energy be supplied to evaporate the solvent, while at the same time a certain amount of water condenses in the material in exchange with the evaporated solvent will. If these requirements are met, the low-temperature evaporation can be used within wide limits in terms of relative humidity of the air, but it can be seen that one is dealing with a maximum upper temperature limit Has the highest evaporation capacity with 100% relative humidity, i.e. when the air is saturated with water.

Those subjected to evaporation according to the present invention Materials which have been treated in such a way that they have not been denatured prior to this treatment have theirs retain functional properties after evaporation, such as water swellability.

509815/1241

Claims (10)

Claims 1. method for evaporation of solvent from protein material, such as with solvent extracted fish protein, characterized in that the protein material with water-containing air treated while adjusting the temperature and relative humidity of the air so that there is enough energy for evaporation of the solvent is supplied, while at the same time water is condensed from the air and the evaporated Replaced the amount of solvent. 2. The method according to claim 1, characterized in that the protein material with water-containing air at a temperature between 40 and 90 ° C treated. 3. The method according to claim 1 and 2, characterized in that one Undenatured protein material with water-containing air at a temperature of 40 to 70, preferably 45 to 65, especially 45 to 55 ° C treated. 4. The method according to claim 1 to 3, characterized in that one treating the protein material with air in an amount of 1.0 to 5.0, preferably 2.0 to 3.0 m / kg of treated protein material. 5. The method according to claim 1 to 4, characterized in that water-containing air is used, which is preferably saturated at least 50% at least 70%, particularly 100% with water. 509815/1241 6. The method according to claim 1 to 5, characterized in that the treatment of the protein material is carried out continuously in one vertical column with the aid of water-containing air in countercurrent to the flow of material, the column being carried out indirectly a temperature is heated which is below the temperature of the introduced air. 7. The method according to claim 6, characterized in that the column to a temperature 10 to 30 ° C, preferably 10 to Heated 15 C below the temperature of the introduced air. 8. The method according to claim 1 to 7, characterized in that one the protein material is continuously treated in a vertical column with the aid of water-containing air in countercurrent to the flow of material, the water-containing air being introduced into the column at several different levels. 9. The method according to claim 8, characterized in that the temperature of the water-containing air in the upper part of the column is introduced above the temperature of the hydrous air introduced in the lower part of the column. 10. The method according to claim 9, characterized in that the water-containing air, which is introduced in the upper part of the column, introduces in such an amount and at such a temperature that the Temperature of the material in this part of the column due to solvent evaporation is essentially the same as the temperature of the material in the lower part of the column. 50981 5/1241