CH663908A5 - PROCESS FOR PRODUCING A DRY GRANULAR EXTRACT. - Google Patents

Description

DESCRIPTION

The present invention relates to a method for manufacturing a dry granular extract, for example an extract of tea leaves, roasted beans and beans, toasted cereals, fruit juices, vegetables or honeys, this method comprising drying by spraying with an aqueous solution containing this extract. The method according to the invention makes it possible to conveniently dry an extract having poor drying characteristics, and to carry out the drying and granulation operations simultaneously, in a very short period of time, which makes it possible to obtain very efficiently. a dry granular extract having excellent properties of solubility, flowability and resistance to agglomeration, without causing deterioration of the aroma.

In accordance with the prior art, preparations for instant drinks, such as instant black tea, instant coffee, instant barley tea, as well as instant juices, have been obtained, in the usual manner, by methods allowing transforming into an dry powder, for example by spray drying, an extract in aqueous solution obtained by extraction with water of each of the materials, or by pressing. During the spray drying operation, the hygroscopicity and thermofusibility characteristics of these extracts would result in obtaining poor drying characteristics, as well as in the deterioration of the taste. In addition, the dry powders thus obtained are in the form of particles having the dimensions of dust with a diameter of the order of 100 (i, so that undissolved agglomerates would frequently be formed during the dissolution of these powders in l These powdery products have other drawbacks, such as their property of easily forming dust and poor flowability, which makes packaging difficult and makes them susceptible to solidification. .

In order to eliminate these drawbacks, attempts have been made to granulate these particles having the dimensions of dust, as obtained by spray drying, using granulating devices, such as a fluidized bed granulating device or an extrusion granulator. However, the hygroscopicity and hot-melt characteristics of these extracts make the granulation operation very difficult and, on the other hand, prolonged heating during the granulation operation is liable to cause a deterioration in the taste of the products. . In addition, the products thus obtained are in the form of hard granules which are not very soluble in water. It is therefore extremely difficult to obtain, by these methods, a granular product having an excellent taste and a high solubility.

The process according to the present invention allows an extract having poor drying characteristics to be dried properly and drying and granulation to be carried out simultaneously in a very short period of time, which makes it possible to obtain the abovementioned extracts very efficiently. in the form of an instant product having excellent properties, in particular a high solubility, • a good flowability and a great resistance to agglomeration, without causing a deterioration of the taste.

The method according to the invention has the characteristics specified in claim 1.

Thus, the process according to the invention comprises the operation of dissolving an appropriate quantity of carbon dioxide in a thick aqueous solution of an extract containing a suitable starch hydrolyzate, in suitable quantity, under pressure and / or at low temperature, the introduction of the mixture thus obtained in a sprayer provided with a nozzle under pressure, and the spraying of the mixture, from the nozzle, in a drying chamber, in order to cause its dehydration.

The aqueous solutions of extracts used during the implementation of the invention can be placed, roughly speaking, in the following groups: tea leaf extract, roasted bean extract, toasted cereal extract, fruit juice, vegetable juice and honey juice.

As examples of aqueous solutions of tea leaf extracts, there may be mentioned tea-based beverages, such as green tea, roasted tea, so-called "oolong" tea and black tea, extracts aqueous herbs such as Chinese wedding vine, geranium, hydrangea, bamboo leaves and persimmon leaves, and their concentrates.

40 As examples of aqueous solutions of extracts of roasted beans, mention may be made of those obtained by extraction of roasted beans such as coffee beans and cocoa beans, under pressure equal to or greater than atmospheric pressure, as well as their concentrates.

45 As examples of aqueous solutions of toasted cereal extracts, mention may be made of those obtained by extraction of roasted cereals such as barley, rye, the so-called "teardrop" ("adlay") cereal. ”), Unglazed rice or rice bran, in the presence of at least one enzyme such as amylase, under atmospheric pressure or 50 under high pressure, as well as their concentrates.

Examples of fruit juices include orange, lemon, apple, pineapple, grape, pear, peach, strawberry and plum juices, as well as their concentrates.

Examples of vegetable juices include the tomato, Chinese cabbage, cabbage, carrot, horseradish, and so-called "shiitake" mushroom juices, and their concentrates.

Examples of honey juice include those obtained from Chinese astragalus, orange or buckwheat honey, and their concentrates.

60 When implementing the method according to the invention, an aqueous solution of an extract containing an appropriate amount of at least one starch hydrolyzate, suitable for obtaining an appropriate dry matter content, containing a suitable quantity of carbon dioxide in the dissolved state is sprayed under pressure 65 in a drying chamber, the drops of liquid thus sprayed not being broken, but expanding instantaneously, so as to produce hollow spheres having each an increased surface, which are intended to be dried. We can thus obtain a

3

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dried product formed from hollow granules, which exhibits considerably improved drying characteristics, as well as high and uniform particle sizes. The granular dried extract prepared by the process according to the invention has a specific density by mass of the order of 0.1 to 0.4, and average particle sizes of the order of 200 to 1000 (i. particles have very uniform dimensions, and the number of those that are broken is small. The product has excellent drying characteristics. Furthermore, it can be dried and granulated simultaneously in an extremely short period of time ( for example, approximately 10 seconds), it is not very subject to a deterioration in taste. Consequently, the method according to the invention allows a dried instant extract having a better taste and a higher solubility to be obtained, as well as better flow characteristics and resistance to solidification than the granular products of the prior art prepared by drying and granulation according to the usual methods.

During the implementation of the process according to the invention, a thick aqueous solution of an extract is prepared containing a suitable quantity of a starch hydrolyzate having an average degree of polymerization of the order of 4 to 20. add another starch hydrolyzate (that is to say cyclic dextrin) having a degree of polymerization of 6, 7 or 8. These starch hydrolysates are very effective in allowing good drying of the aqueous solution extract, without deteriorating its properties, in particular the taste, as well as to accelerate the dissolution of carbon dioxide, and to preserve the quality of the granular dried product thus obtained by the process according to the invention.

When starch hydrolysates each having an average degree of polymerization greater than 21, the viscosity of the aqueous solution thus prepared is too high to allow adequate dissolution of the carbon dioxide, as well as the drying of the solution by spraying. Consequently, a granular dried product cannot be obtained having high and uniform particle sizes. On the other hand, when starch hydrolysates each having an average degree of polymerization less than 3, the viscosity of the aqueous solution thus prepared is too low, while its hygroscopicity is too high. As a result, the dried product thus obtained has base particles which are difficult to dry. In addition, the product has a bad taste, as well as too high a hygroscopicity.

The content of starch hydrolysates is approximately 20 to 70% by weight relative to the total content of dry matter contained in the aqueous solution comprising an extract essence and the starch hydrolysates according to the properties of the starch hydrolysates. having an average degree of polymerization from 4 to 20, and the extract contained in the solution. A content outside the limits indicated above is likely to interfere with the subsequent steps by making it impossible to obtain the results targeted by the invention.

When a fruit or honey juice containing a large amount of highly hygroscopic sugars and / or organic acids and having very poor drying characteristics is dried by the process according to the invention, a hydrolyzate can be used highly moisture resistant starch having a high degree of polymerization (i.e. 20 to 60), as well as a relatively low viscosity, prepared by low hydrolysis of waxy starch comprising amylopectin . In this case, this starch hydrolyzate can be added so as to obtain a concentration of 10 to 50% by weight, relative to the total dry matter content contained in the aqueous solution, depending on the dry matter content and the properties. aqueous solution comprising the extract and the starch hydrolysates. A content of these hydrolysates greater than 50% by weight is capable of excessively increasing the viscosity by making it impossible to obtain the result targeted by the invention.

The average degree of polymerization of the starch hydrolyzate, indicated in the present description, signifies the average degree of polymerization calculated from its DE value, in the case of an acyclic dextrin, or obtained from each of the degrees polymerization, in the case of a cyclic dextrin.

The thick aqueous solution comprising an extract and starch hydrolysates should be prepared so as to obtain a dry matter content of the order of 20 to 55% by weight. A content outside the limits defined above is likely to interfere with the subsequent steps, making it impossible to obtain the results targeted by the invention.

Starch hydrolysates can be added beforehand to the water used to extract a raw material such as tea leaves or roasted beans. Alternatively, they can be added to the aqueous extraction solution. The dry matter content of the aqueous solution containing the extract and the starch hydrolysates is then adjusted to an appropriate value, for example about 20 to 55% by weight (i.e. the solution contains 80 55% by weight of water) depending on the properties of the extract, the quantity of carbon dioxide to dissolve during the subsequent operation and the dimensions of the drops of liquid to be formed by spray drying. When the dry matter content in the aqueous solution is less than 20% by weight, the dried product obtained is in the form of broken particles having the dimensions of dust, whereas, when this content is greater than 55% by weight, the gas carbon dioxide is practically not dissolved, which makes it impossible to obtain the result targeted by the invention.

During the implementation of the process according to the invention, the aqueous solution comprising an extract and hydrolysates of starch is cooled to a suitable temperature, and carbon dioxide is dissolved therein under a sufficiently high pressure. In order to obtain the result targeted by the invention, the carbon dioxide is dissolved in an amount corresponding to 0.2 to 2.4% by weight, relative to the amount of water in the solution, depending on the concentration of the aqueous solution, the properties of the extract and the particle sizes desired for the granular dried product which it is desired to form. The carbon dioxide dissolved in an amount less than 0.2% by weight does not allow any improvement in the drying characteristics, which results in a small particle size and a high specific gravity of mass. On the other hand, when the content of dissolved carbon dioxide is greater than 2.4% by weight, the particles are broken, which does not make it possible to obtain the result targeted by the invention. The carbon dioxide is dissolved in the aqueous solution by cooling the thick aqueous solution containing the extract and the starch hydrolysates, to a temperature of 0 to 30 ° C., and bringing the carbon dioxide into contact with this solution, by proceeding in the usual way, using an appropriate device, under a carbon dioxide pressure of 1 to 15 kg / cm2g. The content of carbon dioxide dissolved in the aqueous solution is calculated from the temperature of the aqueous solution and the pressure of the gas during dissolution.

During the implementation of the process according to the invention, the aqueous solution containing the extract and the starch hydrolysates is then introduced and containing carbon dioxide in the dissolved state in a sprayer provided with a nozzle under pressure, this introduction being carried out by means of a high pressure pump, and the solution is sprayed into a drying chamber of a spray drying apparatus, in a dry atmosphere. The bore of the nozzle under pressure is chosen, as well as the pressure and the spraying temperature, as appropriate, according to various factors, such as the particle sizes and the specific mass density which it is desired to impart to the product. to obtain.

The process according to the invention is expected to have a great impact, because it makes it possible to carry out drying and granulation simultaneously and that it can be used for the treatment of a wide range of aqueous solutions containing extracts . In addition to starch hydrolysates, the aqueous solution of the extract may also contain one or more high molecular weight substances, such as gelatin, gum arabic, starch treated with one or more acids, or derivatives of 'starch.

We will now give a certain number of examples in order to illustrate the invention in more detail, without implied limitation.

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65

1

520 kg of a starch hydrolyzate (CELDEX CH-20, produced by the company NIHON SHO-KUHIN KAKO Co., Ltd), which comprises 60% dextrin, are dissolved in 9400 l of water at 60 ° C. acyclic having an average degree of polymerization of 5.15% of cyclic dextrin and 25% of water, and 80 kg of ß-cyclodextrin (CELDEX N, produced by the company NIHON SHOKUHIN KAKO Co., Ltd), and there is added 2000 kg of roasted tea leaves, and extraction is carried out at 60 ° C for 30 minutes, shaking occasionally. After draining and filtering, about 9000 kg of an aqueous extract solution are obtained having a dry matter content of 8.9%. The extract is concentrated using a vacuum concentrator, keeping the temperature of the material at 45 ° C., which makes it possible to obtain approximately 2400 kg of a concentrated aqueous solution having a dry matter content of 33%. by weight, containing 48% by weight of starch hydrolyzate relative to the total dry matter content.

The concentrated aqueous solution thus obtained is divided into five aliquots, which are respectively subjected to tests A to E, 5 during which each aliquot portion is injected into a device for dissolving carbon dioxide, by means of a pump, while cooling to 12.5 ° C., by means of a continuous cooling device, so as to completely dissolve the carbon dioxide under the conditions indicated in Table 1, and it is dried by spraying, under a pressure of spraying 30 kg / cm2, with a spraying enclosure temperature of 95 ° C, the concentrated aqueous solution containing carbon dioxide in corresponding concentration. The results are shown in Table 1.

Table 1

-

Test A

Trial B

Test C

Test D

Test E

Temp. from the ground. aq. conc. on dissolution of C02 (° C)

12.5 ° C

12.5eC

12.5 ° C

12.5 ° C

12.5 ° C

C02 gas pressure. on dissolution of C02 (kg / cm2g)

0.1 kg / cm2g

4.0 kg / cm2g

7.0 kg / cm2g

10.0 kg / cm2g

13.0 kg / cm2g

Proportion of C02 gas. dissolved relative to the water in the soil. aq. conc. (% in weight)

0.23 w / w%

0.86 w / w%

1.41 w / w%

1.96 w / w%

2.60 w / w%

Drying state

Some non-dried parts adhering to the walls of the chamber

Well

Well

Well

Well

Specific mass density of the dried product (weight / volume)

0.38

0.23

0.18

0.15

0.18

Particle dimensions of the dried product

<105 p.

26.1%

8.1%

1.8%

7.4%

29.6%

105 ~ 210 p.

41.9%

15.0%

4.2%

11.8%

40.9%

210-297 n

22.0%

16.3%

5.8%

12.5%

20.1%

297 - 420 (x

8.5%

20.1%

15.4%

20.4%

8.2%

420-710 n

1.5%

38.2%

62.0%

43.5%

1.2%

> 710 dd.

-

2.3%

18.8%

4.4%

-

Form of the dried product

The particles are less expanded and have an average particle size of about 190 n

Particles less dilated than those of test C and having an average particle size of approximately 450 n.

Hollow and spherical granular particles having an average particle size of approximately 610 µi.

Hollow and spherical granular particles and a small amount of broken particles. The average particle size is approximately 450 n.

Most of the particles are broken and have an average particle size of about 170 n, and they do not flow well.

Solubility in water of the dried product

Poorly soluble and forming undissolved agglomerates

Good

Good

<3

Good

Poorly soluble and forming undissolved agglomerates

Table 1 indicates that the dried product of test C is the best instant product based on roasted tea, because of its excellent drying characteristics, its good taste, its high and uniform particle sizes, its specific density by mass. suitable, its excellent flowability and its high solubility in water, the products of tests B and D coming next. On the other hand, the dried product of test A, containing 0.23% by weight of dissolved carbon dioxide, relative to the amount of water contained in the solution.

60 tion concentrated aqueous, was in the form of particles having the dimensions of dust and had poor drying characteristics, which resulted in poor solubility, while the product of test E, containing 2.60% by weight of carbon dioxide dissolved, in relation to the amount of water, consisted of overly dilated particles and crushed particles having dimensions of dust, which was accompanied by poor solubility, as well as poor flow and resistance to agglomeration.

5

Example 2:

600 kg of a starch hydrolyzate (CELDEX CH-20, produced by the company NIHON SHO-KUHIN KAKO Co., Ltd), comprising 60% of acyclic dextrin having an average degree of polymerization of 5.15% cyclic dextrin and 25% water. 1000 kg of black tea leaves (produced by the company Japan Black Tea Co., Ltd) are added thereto, and extraction is carried out at 55 ° C. for 30 minutes, with occasional stirring. After wringing, an additional 1000 kg of the same black tea leaves as indicated above are added to the extract solution obtained and extracted under the same conditions as indicated above. After wringing by pressure and filtering, about 4000 kg of a black tea extract solution having a dry matter content of 17% by weight, containing approximately 8.5% by weight of starch hydrolyzate, are obtained. which corresponds to 50% of the total amount of dry matter.

Subsequently, the extract thus obtained is divided into six parts,

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quotes. One of the parts, as it is (sample I), is subjected to the operations described below. The other parts are concentrated under vacuum while maintaining the product at 40 ° C, so as to obtain respective dry matter concentrations of 25.5% by weight (sample II), 34% by weight (sample III), 42.5 % by weight (sample IV), 51% by weight (sample V), and 59.5% by weight (sample VI). Each sample is injected into a device for dissolving carbon dioxide, while cooling to 15 ° C., by means of a continuous cooling device, so as to bring the carbon dioxide into intimate contact with the aqueous solution, under pressure. C02 of 6.5 kg / cm2g, the temperature of the solution being 15 ° C, which allows to dissolve 1.24% by weight of carbon dioxide relative to the amount of water contained in the aqueous solution. The solution thus obtained is then introduced into a sprayer provided with a pressure nozzle, and it is dried by spraying, under a spraying pressure of 25 kg / cm 2, with a chamber temperature of 105 ° C. The results are shown in Table 2.

Table 2

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Sample I

Sample II

Sample III

Sample IV

Sample V

Sample VI

Dry matter content of the soil. aq. (% in weight)

17.0%

25.5%

34.0%

42.5%

51.0%

59.5%

Proportion of starch hydro-lysates in the dry matter contained in the soil. aq. (%)

. 50%

50%

50%

50%

50%

50%

Specific mass density of the dried product (weight / volume)

0.23

0.16

0.17

0.21

0.28

0.33

Form of the dried product

Particles having the dimensions of dust, containing a large quantity of broken particles and having an average particle size of approximately 120 jx

Partially broken particles with an average particle size of about 210 n

Hollow and spherical particles, with an average particle size of about 700 n

Hollow and spherical particles with an average particle size of approximately 720 | i

Particles with an average particle size of about 480

Relatively large and dense particles, with an average particle size of about 300 | i

Solubility in water

Poorly soluble and forming undissolved agglomerates

Relatively good

Good

Good

Relatively good

Not very soluble, with sedimented granules

Table 2 indicates that the dried product prepared from sample I, which has a dry matter concentration of 17% by weight, has a low specific gravity by mass, but is found in the form of particles having dimensions of dust. , corresponding to an average size of around 120 p., which results in poor solubility. On the other hand, the dried product prepared from sample VI, which has a dry matter content of 59.5% by weight, has relatively large particle sizes, and is in the form of dense particles, having a high specific gravity, which results in poor solubility in cold water. In addition, sample VI exhibited adhesions of undried material on the walls of the chamber during the drying operation. The products prepared from samples III and IV have excellent drying properties, as well as

55 specific sites by mass and average particle size suitable, and they are very soluble in water.

Example 3:

30 kg of ß-cyclodextrin (CELDEX N, produced by the company NIHON SHOKUHIN KAKO Co., Ltd) are dissolved in 970 l of water at 50 ° C., and 200 kg of high quality green tea leaves are added thereto. , and extracted at 50 ° C for 30 minutes, stirring occasionally. After wringing by pressing, about 900 kg of extract solution are obtained. An additional quantity of 200 kg of green tea leaves of the same higher quality as that indicated above is added to the solution thus obtained, and extraction is carried out under the same conditions as those which have just been described. After wringing by pressing and filtering, 700 kg of a solution of extract of

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premium green tea leaves with a dry matter content of 15% by weight. 35 kg of starch hydrolyzate (GLISTER P, produced by the company Matsutani Chemical Co., Ltd) having an average degree of polymerization of 6.3 and a water content of 5% are dissolved in this solution. which makes it possible to obtain 735 kg of an aqueous solution consisting of green tea extract and starch hydrolyzate, having a dry matter content of 18.8% by weight, and containing approximately 39% by weight of starch hydrolyzate relative to this dry matter content.

Half (ie 367.5 kg) of the aqueous solution thus prepared is sprayed by drying, using a sprayer fitted with a pressure nozzle, at a chamber temperature of 95 ° C. thus approximately 70 kg of dried product in the form of particles having the size of dust with an average particle size of the order of 100 μm and having a specific density by mass of 0.41. This product was poorly soluble, even in hot water, and gave rise to the formation of undissolved agglomerates.

About 70 kg of the dried powder thus obtained is dissolved in the remaining half (i.e. 367.5 kg) of the aqueous solution prepared as described above, so as to form a concentrated aqueous solution having a content in dry matter of 31% by weight. The concentrated aqueous solution thus obtained is cooled to 8 ° C. using a cooling device, and it is introduced into a device for dissolving carbon dioxide in which it is brought into intimate contact with carbon dioxide under a CO 2 pressure of 7 kg / cm2g, maintaining the solution at the temperature of 8 ° C, so as to dissolve the carbon dioxide at a rate of 1.96% by weight, relative to the amount of water in the concentrated aqueous solution. The solution thus obtained is then introduced into a nozzle under pressure, and dried by spraying with a chamber temperature of 98 ° C., so as to produce approximately 114 kg of dried product having a water content of 2.0 %. The dried product thus obtained was in the form of hollow, spherical granular particles having a specific gravity by mass of 0.16. The dimensions of these particles were very uniform, and 85% of them were in the size range of 24 to 48 mesh (standard sieve dimensions). The average particle size of this product was around 500 µm. The granular dried green tea extract product exhibited excellent flow properties,

without any tendency to form dust, so that it could be easily packed in bottles using an automatic filling device. In addition, this product was very soluble, not only in hot water, but also in cold water. The dried product had a taste similar to that of the undried extract.

Example 4:

0.15 kg of α-amylase (CLARASE, produced by the company Kyowa-Miles Co., Ltd) is dissolved in 3000 kg of water at 50 ° C., and 500 kg of so-called “teardrop” cereal are added thereto. -Job "(" adlay ") previously roasted and ground, and extracted at 50 ° C, for 60 minutes, while stirring. After wringing by pressing, an additional 500 kg of the same "tear-of-Job" cereal as that indicated above is added to the extract solution thus obtained, and extraction is carried out under the same conditions as those which come to be described. After wringing by pressing and filtering, approximately 3200 kg of an extract solution is obtained having a dry matter content of 12.8% by weight. 320 kg of starch hydrolyzate are dissolved (CELDEX CH-20, produced by the company NIHON SHOKUHIN KAKO Co., Ltd) comprising 60% of dextrin having an average degree of polymerization of 5.15% of cyclic dextrin and 25% of water, which makes it possible to obtain approximately 3520 kg of an aqueous solution comprising the extract of "teardrop-of-Job" and the starch hydrolysates, this solution having an ED value of 19.5 and a content total dry matter of 18.5% by weight.

Subsequently, the aqueous solution containing the “tear-of-Job” extract is divided into five aliquots. One of these parts (sample I) is subjected as it is to subsequent processing. The other parts are concentrated under vacuum while maintaining the material at 45 ° C so as to produce aqueous solutions having respectively dry matter contents of 28.3% by weight (sample II), 38.0% by weight (sample III ), 48.8% by weight (sample 5 IV), and 57.5% by weight (sample V). Each sample is injected into a device for dissolving carbon dioxide, while cooling it to 15 ° C. by means of a continuous cooling device, so as to bring it into intimate contact with carbon dioxide, under a pressure of CO 2 4.5 kg / cm2g, the temperature of the solution being 15 ° C. The solution is introduced into a sprayer provided with a nozzle under pressure, by means of a high pressure pump, and it is dried by spraying at a spraying pressure of 30 kg / cm2, the temperature of the drying chamber being 103 ° C. The results thus obtained are shown in Table 3. Table 3 indicates that the dried product prepared from sample I, having a dry matter content of 18.5% by weight, has a low specific gravity by mass and average small particle sizes of about 180 | i. In addition, many particles of this product are broken, resulting in poor flow characteristics and poor solubility, with the formation of undissolved agglomerates, especially in cold water. On the other hand, the dried product prepared from sample V, having a dry matter content of 57.5% by weight, gave rise to a partial adhesion of material to the walls of the enclosure during 25 the drying operation. This product had relatively high average particle sizes, as well as a high specific gravity, and was in the form of dense particles, poorly soluble in cold water. The products prepared from samples II, III and IV had excellent drying characteristics, as well as specific mass densities and suitable average particle sizes. They were very soluble in water. In particular, the product prepared from sample III is extremely soluble in cold water and exhibits no dust formation phenomenon, while having excellent flow characteristics. Consequently, this product constitutes an instant product for the preparation of "tear-of-Job" tea, for use by dissolving in cold water, which can be conveniently packaged without solidifying.

(Table at the top of the next page)

40

Example 5:

200 kg of starch hydrolyzate are dissolved (CELDEX CH-20, produced by the company NIHON SHOKUHIN KAKO Co., Ltd) comprising 60% of acyclic dextrin having an average degree of polymerization of 5.15% of cyclic dextrin and 25% water, in 1300 kg of water at 80 ° C, and 200 kg of roasted barley, not ground, are added thereto and extraction is carried out at 80 ° C for 30 minutes, with stirring. After wringing by pressing and filtration, 1410 kg of an extract solution are obtained having a dry matter content of 14.0% by weight, which is designated below by the term "extract A" . Subsequently, 0.5 kg of α-amylase (CLARASE, produced by the company Kyowa-Miles Co., Ltd) is dissolved in 4000 kg of water at 50 ° C., and 800 kg of barley are added thereto. roasted, ground, and extracted at 50 ° C for 60 minutes, while stirring, in the presence of the enzyme. 55 After wringing by pressing and filtration, 4080 kg of an extract solution is obtained having a dry matter content of 11.5% by weight, which is designated below by the term "extract B" . Extract B is spray dried using a spray dryer with a chamber temperature of 102 ° C, which provides 470 kg of dried powder, which is subsequently dissolved in the extract A, so as to produce 1880 kg of concentrated aqueous solution comprising the extract of roasted barley and the starch hydrolysates and having a dry matter content of 34.3% by weight. The dried powder obtained by spray drying of extract B was sparingly soluble in water, and gave rise to the formation of undissolved agglomerates. Another attempt was made to granulate the same powder using a fluidized bed granulator. This test showed that the powder obtained was practically not granulated, and that the

7

Table 3

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Sample I

Sample II

Sample III

Sample IV

Sample V

Dry matter content of the soil. aq. (% in weight)

18.5 w / w%

28.3 w / w%

38.0 w / w%

48.8 w / w%

57.5 w / w%

Proportion of C02 gas. dissolved relative to the amount of water in the soil. aq. (% in weight)

0.92 w / w%

0.92 w / w%

0.92 w / w%

0.92 w / w%

0.92 w / w%

Specific mass density of the dried product (weight / volume)

0.23

0.14

0.18

0.24

0.34

Particle dimensions of the dried product

<105 n

29.2%

9.2%

1.2%

8.2%

9.2%

105-210 n

41.4%

14.8%

4.4%

10.4%

15.8%

210 ~ 297 n

20.6%

18.3%

7.1%

11.0%

41.0%

297 ~ 420 n

7.6%

19.3%

10.7%

28.7%

20.2%

420 ~ 710 n

1.2%

35.4%

65.2%

38.1%

12.4%

> 710 n

-

3.1%

11.4%

3.6%

1.4%

Form of the dried product

Particles having the dimensions of dust, having an average particle size of about 180 | i, comprising many broken particles

Hollow and spherical particles, having an average particle size of 390 (d. Approximately, including some broken particles

Hollow and spherical particles, having an average particle size of about 600 | i

Hollow and spherical particles, having an average particle size of about 430 | i, with a relatively high specific gravity by mass

Relatively high number of particles with an average particle size of about 310 n, with a relatively high specific gravity by mass

Solubility of the dried product in cold water (10 ° C)

Poorly soluble and forming undissolved blocks

Relatively soluble

Very soluble

Relatively soluble

Poorly soluble, with sedimented granules granules thus prepared were practically not soluble in water.

The concentrated aqueous solution containing the roasted barley extract was divided into five aliquots, which were then subjected, respectively, to tests A to E described below, in which each of the parts was injected into an apparatus. of dissolution of carbon dioxide, by means of a pump, while cooling to 15 ° C. by means of a continuous cooling apparatus, and bringing into intimate contact with carbon dioxide under the conditions indicated in table 4, the solution thus prepared being spray-dried under a spraying pressure of 30 kg / cm 2, with a chamber temperature of 98 ° C. The results obtained are shown in Table 4.

Table 4 indicates that the dried product of test C has uniform and high particle sizes, a suitable specific gravity by mass and excellent flow properties, as well as a high solubility in cold water, products of tests B and D coming next. On the other hand, the product of test A, containing 0.18% by weight of dissolved carbon dioxide, relative to the amount of water, was in the form of particles having the dimension of dust, whose solubility is extremely weak, while the product of test E, containing 2.41% by weight of dissolved carbon dioxide, is in the form of particles having the dimensions of dust, comprising a large quantity of particles which are excessively magnified and broken, so that this product is practically not soluble in water. A spoonful (approximately 1 g) of the instant barley tea product obtained in test C, B or D is introduced into a cup, and about 110 ml of iced water are poured over it without stirring. The product dissolves completely in 30 minutes, giving a drink that can be consumed as it is. Its taste 40 is similar to the usual product prepared by extracting roasted barley by heating to boiling and cooling the extract in the refrigerator.

(Table at the top of the next page)

45 Example 6:

50 kg of an enzymatic starch hydrolyzate (GLISTER P, produced by the company Matsu-tani Chemical Co., Ltd) having an average degree of polymerization of 6 is dissolved in 1600 kg of water at 80 ° C. 7 and containing 5% water, and 30 kg of ß-cyclodextrin (CELDEX so N, produced by the company NIHON SHOKUHIN KAKO Co., Ltd) containing 10% water. 200 kg of ground roasted coffee beans are added thereto, and extraction is carried out at 80 ° C. for 20 minutes, while stirring. After wringing by pressing and filtration, 1580 kg of an extract solution is obtained having a dry matter content 55 of 9.0% by weight. The solution thus obtained is concentrated by the concentration process by reverse osmosis, which makes it possible to obtain 400 kg of a concentrated solution having a dry matter content of 35.2% by weight. The concentrated solution thus obtained is cooled to 10 ° C., using a plate cooler, and it is introduced into a device for dissolving carbon dioxide, in which it is brought into intimate contact with carbon dioxide under a pressure of gas of 8 kg / cm2g, at 10 ° C, which gives a solution containing 1.81% by weight of carbon dioxide relative to the water of the concentrated solution. The solution thus obtained is introduced into a nozzle 65 under pressure, at a spraying pressure of 20 kg / cm 2, and dried by spraying at a chamber temperature of 92 ° C. This gives approximately 140 kg of dried product containing 4.6% water.

663,908

8

Table 4

- —_______

Test A

Trial B

Test C

Test D

Test E

Temp. from the ground. aq. on dissolution of C02 gas. (° C)

15 ° C

15 ° C

15 ° C

15 ° C

15 ° C

C02 gas pressure. on dissolution of C02 (kg / cm2g)

0.1 kg / cm2g

3.5 kg / cm2g

6.5 kg / cm2g

9.5 kg / cm2g

12.5 kg / cm2g

Proportion of C02 gas. dissolved relative to the water in the soil. aq. (% in weight)

0.18 w / w%

0.76 w / w%

1.24 w / w%

1.87 w / w%

2.41 w / w%

Specific mass density of the dried product (weight / volume)

0.40

0.25

0.19

0.22

0.28

Granulometry of the dried product

> 105 n

37.8%

8.7%

0.5%

17.8%

35.6%

105-210 n

30.9%

15.4%

3.1%

13.3%

28.2%

210 - 297 n

23.3%

18.6%

4.4%

13.2%

26.7%

• 297 - 420 n

6.5%

18.5%

18.2%

21.9%

5.7%

420 - 710 n

1.5%

33.3%

59.3%

28.4%

3.0%

<710 (X

-

5.5%

14.5%

5.4%

0.8%

Form of the dried product

Particles less dilated, having the dimensions of dust, with an average particle size of 170 | i approximately

Particles less dilated than those of test C and having an average particle size of approximately 410 n.

Hollow and spherical particles, comprising 60% of particles of average particle size from 420 | i to 710 (x and having an average particle size of approximately 610 n

Hollow and spherical particles, some of which are broken, having an average particle size of approximately 380 n

Dried, poorly flowing powder with an average particle size of about 180 n, most of the particles of which are broken

Solubility of the dried product in cold water (15 ° C)

Poorly soluble and forming undissolved blocks

Good

Excellent

Good

Poorly soluble and forming undissolved blocks

The dried product thus obtained was in the form of easily flowing spherical granules having an average particle size of 460 n, as well as a specific gravity by mass of 0.13. No deterioration in taste was observed during drying, the product obtained being very soluble not only in hot water, but also in cold water. Consequently, the product thus obtained is very suitable for use as a preparation for instant coffee.

Example 7;

Dissolve in 500 kg of concentrated orange juice, consisting of 20% dry matter and 80% water, prepared by concentration by freezing, 50 kg of waxy starch hydrolyzate (Pinedex # 100, produced by company Matsutani Chemical Co., Ltd) having an average degree of polymerization of 30, and containing 5.0% of water, which makes it possible to obtain 550 kg of an aqueous solution having a dry matter content of 26.8 % in weight.

The aqueous solution thus obtained is injected into a device for dissolving carbon dioxide, by means of a pump, while cooling to 12.5 ° C., by means of a continuous cooler, so as to dissolve the carbon dioxide therein. under a gas pressure of 6 kg / cm2g, at 12.5 ° C. The aqueous solution thus obtained, containing 1.23% by weight of carbon dioxide dissolved relative to the amount of, is dried by spraying, under a spraying pressure of 50 kg / cm 2 and at a chamber temperature of 86 ° C. water. The drying operation takes place in excellent conditions, without the slightest adhesion of material to the walls of the enclosure, and makes it possible to obtain approximately 147 kg of dried product.

The dried product, which is in the form of hollow spherical granules having average particle sizes of the order of 300 | i, as well as a specific density by mass of 0.24, is very soluble in cold water, and has excellent flow properties and resistance to agglomeration, without any deterioration in taste. As a result, this product is of great interest as an instant juice preparation.

Example 8:

Dissolve in 500 kg of onion juice concentrate prepared by pressing and filtering onion, and vacuum concentration of the onion juice so obtained, 50 kg of starch hydrolyzate (Pinedex # 1, produced by Matsutani Chemical Co., Ltd) having an average degree of polymerization of 12.5 and a water content of 5.0%, so as to produce 550 kg of an aqueous solution having a dry matter content of 31, 4% by weight.

65 The aqueous solution thus obtained is injected into a device for dissolving carbon dioxide, by means of a pump, while re-cooling to 15 ° C. by means of a continuous cooling device, so as to dissolve the gas therein. carbon dioxide under a pressure of

45

9

663,908

10 kg / cm2g, at 15 ° C. The aqueous solution thus obtained, which contains 1.92% by weight, is spray-dried under a spraying pressure of 40 kg / cm2 and at a chamber temperature of 95 ° C. carbon dioxide dissolved relative to the amount of water. The drying operation takes place in excellent conditions, without any adhesion of material to the walls of the chamber, which makes it possible to obtain approximately 172 kg of dried product having a specific density by mass of 0.18.

The dehydrated onion juice thus obtained was very soluble, and exhibited excellent flow properties as well as resistance to agglomeration, and a very good taste. As a result, this product is useful as an additive for various instant preparations, such as an instant soup.

15

Example 9:

Dissolve, in 900 kg of water, 250 kg of honey concentrate, from astragalus from China, and comprising 80% dry matter and 20% water, 180 kg of waxy starch hydrolyzate (Pinedex # 100, produced by Matsutani Chemical Co., Ltd.) com- 20

taking 5.0% water and having an average degree of polymerization of 30, as well as 30 kg of starch hydrolyzate (Pinedex # 1, produced by the company Matsutani Chemical Co., Ltd) comprising 5.0% d water and having an average degree of polymerization of 12.5, so as to produce 1350 kg of aqueous solution having a dry matter content of 28.9% by weight.

The aqueous solution thus obtained is injected into a device for dissolving carbon dioxide, by means of a pump, while cooling to 15 ° C., so as to dissolve 1.34% by weight of carbon dioxide relative to the amount of water contained in the aqueous solution, under a gas pressure of 7 kg / cm2g at 15 ° C. The solution thus obtained is introduced into a nozzle under pressure, at a spraying pressure of 100 kg / cm 2, at a chamber temperature of 86 ° C, and dried by spraying. The drying operation takes place in excellent conditions, and makes it possible to obtain 390 kg of a dried honey product having a specific density by mass of 0.35, average particle sizes of 210 | i and a content 3.2% water. This dried honey product has excellent taste, solubility, flow and agglomeration resistance properties.

R

Claims (6)

663,908 CLAIMS 1. A method of manufacturing a dry granular extract, comprising drying an aqueous solution containing an extract and at least one starch hydrolyzate, characterized in that the dry matter content of this aqueous solution is adjusted to a value of 20 to 55% by weight, that there is dissolved therein an amount of carbon dioxide corresponding to 0.2 to 2.4%, by weight, relative to the water contained in this aqueous solution, and that l the solution thus obtained is spray dried using a sprayer fitted with a pressure nozzle, so as to form a dried product. 2. Method according to claim 1, characterized in that said aqueous solution containing an extract is an aqueous extract solution of tea leaves, roasted beans, roasted cereals, fruit juice, vegetables or honeys. 3. Method according to claim 1 or 2, characterized in that said starch hydrolyzate contains acyclic dextrin having a degree of polymerization from 4 to 20, or alternatively acyclic dextrin having a degree of polymerization from 4 to 20 and cyclic dextrin. 4. Method according to claim 1, 2 or 3, characterized in that said aqueous solution of an extract and of starch hydrolyzate (s) contains the starch hydrolyzate (s) in an amount corresponding to 20 to 70% by weight relative to its total dry matter content. 5. Method according to claim 1 or 2, characterized in that said aqueous solution contains at least one starch hydrolyzate prepared by hydrolysis of waxy starch and having an average degree of polymerization from 20 to 60, in an amount corresponding to 10 to 50% by weight relative to its total dry matter content. 6. Granular process resulting from the drying of an extract, obtained by the process according to one of claims 1 to 5.