CN115385776A - Erythritol crystal and preparation method and application thereof - Google Patents
Erythritol crystal and preparation method and application thereof Download PDFInfo
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- CN115385776A CN115385776A CN202210948104.XA CN202210948104A CN115385776A CN 115385776 A CN115385776 A CN 115385776A CN 202210948104 A CN202210948104 A CN 202210948104A CN 115385776 A CN115385776 A CN 115385776A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/78—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by condensation or crystallisation
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/52—Adding ingredients
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/30—Foods or foodstuffs containing additives; Preparation or treatment thereof containing carbohydrate syrups; containing sugars; containing sugar alcohols, e.g. xylitol; containing starch hydrolysates, e.g. dextrin
- A23L29/37—Sugar alcohols
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Nutrition Science (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Molecular Biology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides an erythritol crystal and a preparation method and application thereof, wherein the erythritol crystal is subjected to controllable coalescence by regulating and controlling dispersion work among crystals in a wet agglomeration process in a system aiming at agglomeration phenomenon caused by adhesion work of the erythritol crystal in an aqueous solution during cooling crystallization, so that a highly uniform crystal product is prepared by utilizing a trace crystal seed. The erythritol crystals are highly uniform in particle size, more than 89.2wt% is 20-40 meshes, more than 97.0wt% is 20-60 meshes, high in dissolution rate and good in fluidity. The preparation method is simple, easy to implement, free of any organic solvent, green and environment-friendly, and capable of realizing industrialization and low in economic investment.
Description
Technical Field
The invention belongs to the technical field of chemical engineering industrial crystallization, particularly relates to an erythritol crystal and a preparation method and application thereof, and particularly relates to a method for regulating and controlling production of the erythritol crystal with uniform particle size and high dissolution rate by utilizing wet agglomeration.
Background
High-sugar diets are considered to be an important cause of obesity and various diseases. With the increasing pursuit of health, more and more consumers use novel sugar substitutes as a source for obtaining sweet taste in foods, which promotes the vigorous development of the sugar alcohol industry. Erythritol (CAS: 149-32-6) English name erythrothritol, molecular formula C 4 H 10 O 4 Molecular weight 122.12. Usually white crystalline powder, with a refreshing sweetness of 60-80% of sucrose. According to European food additive guidelines (2008/100/EC), erythritol has a caloric value of 0kcal kg -1 Therefore, in recent years, food formulations containing erythritol have been more and more emphasized, which has led to the development of erythritolThe yield rises sharply, and the production scale is expected to reach 35 ten thousand tons in the market scale in the next five years according to the prediction of Shalivin. At present, erythritol is mainly produced by adopting a biological fermentation process. The metabolic behavior is different from that of other polyols, and the polyols are mainly discharged through urine without causing any digestive dysfunction. The tolerance in the human body is 2-3 times that of xylitol, so that the composition has almost no diarrheal property compared with other sugar alcohols. The erythritol has strong heat absorption when dissolved in water, the dissolution heat absorption is 97.4kJ/kg, and the particle compound food can create a cool mouthfeel in the oral cavity. Because of its many unique advantages, erythritol is widely used in the formulation of sugar-free beverages and other low-sugar foods.
CN103709007A mentions a method for refining erythritol crystals by using cooling crystallization coupled with elution crystallization, but this method requires the use of organic solvent for auxiliary production, which is not environment-friendly. CN113912475A proposes a method for preparing large erythritol particle crystals with high yield of more than 50 meshes by using temperature reduction crystallization, and in order to further confirm the technical advantages of the method, the erythritol particles are prepared by the method, and the obtained erythritol particles are large in size, good in flowability and low in dissolution rate. CN112479820A proposes a continuous oscillation flow membrane crystallization device of erythritol, but the device operation is complicated, and the industrialization is difficult to realize.
Therefore, the technical problem which cannot be solved by the prior art is to find a preparation method of erythritol crystal products which does not use any organic solvent, has highly uniform product particle size and good solubility, and can realize industrialization.
Disclosure of Invention
The food industry has strict requirements on the dissolution rate, the fluidity and the anti-caking performance of the properties of the sugar granule powder, so that the particle size control of the sugar alcohol crystals is always a research difficulty and a hotspot in the field of functional sugar, and the fluidity and the anti-caking performance of the sugar alcohol crystals can be obviously improved by narrow particle size distribution. At present, erythritol is mainly applied to the field of sugar-free beverages, and has high requirements on the particle size distribution of erythritol, and erythritol crystals with different particle size distribution ranges also show different physical properties in consideration of the requirements on dissolution rate, fluidity and anti-caking performance. For example: under the condition of constant-temperature water bath at 25 ℃,30g of erythritol crystals with different grain size intervals are dissolved in water, the time for dissolving the erythritol crystals with the grain size distribution of 16-40 meshes is approximately 180-240 s, the time for dissolving the erythritol crystals with the grain size distribution of 20-60 meshes is approximately 140-200 s, and the time for dissolving the erythritol crystals with the grain size distribution of 30-80 meshes is 100-150 s. The dissolution rate is directly related to the sugar alcohol dissolution time of the sugarless beverage and the cooling feeling degree of the erythritol in the oral cavity when the erythritol is used as a compound granular product. Flowability is another important measure of the dissolution of a particulate product in a beverage and the properties of the particulate product, usually measured as angle of repose, and is significantly improved when the particle size is larger or uniform, and conversely, reduced. Balancing the factors of the various aspects, the crystal size is usually required not to be too large or too small, and in the market, 20-60 mesh crystals are more popular when the beverage is produced and the granular food is compounded. However, in industrial production, wet agglomeration and scaling can occur in the solution crystallization process of erythritol crystals, and the design of a cooling curve is not reasonable, so that the particle size distribution of products is out of control, wherein the mass ratio of large particles above 20 meshes to crushed crystals below 60 meshes is high. Currently, grinding is generally used for processing large particles, which increases energy consumption and destroys crystal morphology, and the large amount of fine powder generated in the grinding process significantly increases the agglomeration risk. In order to overcome the defects of the existing product preparation method and utilize the characteristic that agglomeration occurs due to large adhesion work of erythritol crystals in a solution, the invention provides a method for preparing the erythritol crystals with high dissolution rate and uniform granularity (20-60 meshes) by using micro crystal seeds to influence dispersion force in wet agglomeration by using a regulation flow field and further regulating and controlling the number of agglomeration layers by changing dispersion work to resist the adhesion work so that the crystals can be subjected to controllable wet agglomeration. The process does not use any organic solvent, and is green and environment-friendly.
One of the purposes of the invention is to provide a preparation method of erythritol crystals, which comprises the following steps:
adding erythritol seed crystals into the erythritol concentrated solution with the temperature of 60-70 ℃, and cooling and crystallizing in four sections under the action of a flow field and stirring to obtain erythritol crystals;
preferably, the method for preparing the erythritol concentrated solution with the temperature of 60-70 ℃ comprises the following steps: evaporating and concentrating 10-20wt% erythritol solution at constant temperature of 60-70 deg.C to 50-70wt%;
preferably, the method for preparing the erythritol concentrated solution with the temperature of 60-70 ℃ comprises the following steps: evaporating and concentrating 10-20wt% erythritol solution at constant temperature of 60-70 deg.C to 61-68wt%;
preferably, the preparation of the erythritol concentrated solution is realized in a sugar boiling tank or a vacuum evaporation crystallizer;
preferably, the erythritol seed crystal has a particle size of 250-325 mesh.
In the present invention, the seed crystal should have a uniform particle size (mesh size of not more than 0.02mm, for example, 250 to 300 mesh, 300 to 325 mesh). The addition amount of the seed crystal needs to be controlled properly, and the grain diameter of a crystal product is not out of control due to over-large or over-small crystal seeds;
preferably, the erythritol seed crystal is added in an amount of 0.2 to 1wt%, preferably 0.3 to 0.6wt%, based on the dry matter content of erythritol in the erythritol concentrate;
preferably, the flow field is a flow field existing in both the z-axis direction and the tangential direction;
preferably, the z-axis flow field is applied through a flow guide cylinder;
preferably, the flow field tangential direction is applied by a single layer of three-bladed propeller;
preferably, the stirring power during the temperature reduction crystallization is 0.37-2.64kW/m 3 。
Preferably, the cooling crystallization comprises four steps, wherein the temperature is reduced from 70-60 ℃ to 64-54 ℃ in the first step at a rate of 0.5-1.5 ℃/h, the temperature is reduced from 64-54 ℃ to 54-39 ℃ in the second step at a rate of 1-2.5 ℃/h, the temperature is reduced from 54-39 ℃ to 39-25 ℃ in the third step at a rate of 2-4 ℃/h, and the temperature is reduced from 39-25 ℃ to 25-20 ℃ in the third step at a rate of 4.5-5.5 ℃/h;
preferably, the cooling crystallization is realized in a vertical cooling crystallizer with a guide shell, a cooling crystallization tank with a guide shell or a cooling crystallizer with a guide shell.
In the invention, a cooling crystallizer with a guide cylinder is required to be used, and a z-axis flow field is required to be provided to avoid excessive coalescence of crystals. And avoids the influence on the particle size distribution of the product caused by different crystal growth rates caused by huge linear velocity difference of each point of the fluid when a tangential flow field exists only;
preferably, the preparation method further comprises the steps of sequentially carrying out solid-liquid separation, cleaning and drying on the mixed liquid obtained by cooling and crystallizing.
Preferably, the solid-liquid separation mode is centrifugation;
preferably, the drying mode is normal pressure drying, the drying temperature is 45-55 ℃, and the drying time is 6-12h.
The second object of the present invention is to prepare erythritol crystals according to the preparation method described in the first object;
preferably, the erythritol crystals are uniform in particle size, wherein more than 89.2wt% of the erythritol crystals have a size of 20-40 meshes, and more than 97wt% of the erythritol crystals have a size of 20-60 meshes;
preferably, the angle of repose of the erythritol crystals is 21.3 to 22.6 °;
preferably, the dissolution rate of 30g of the erythritol crystals in 100g of water under a constant-temperature water bath at 25 ℃ is 96-105s, which is obviously faster than that of the erythritol crystals prepared in the same field.
The method for distinguishing the particle size particles is a vibrating screening method;
preferably, 100g of the same batch of products are taken and put into the uppermost layer of screens with different meshes, the screens are laminated in a vibrating screen bed, the vibrating time is adjusted for 5min, and the amplitude is 1mm/g for screening the erythritol particle size.
A third object of the present invention is the use of the erythritol crystals according to second object in the preparation of sugarless beverages and to enhance the cooling mouthfeel of granular products.
The invention has the technical characteristics and beneficial effects that:
1. the invention adopts the cooling crystallization technology to prepare the erythritol crystals, does not need to be heated for many times, and has simple process; no organic solvent is needed, the cost is low, and the environment is protected; the obtained product has high uniformity of grain diameter.
2. The invention obviously reduces the addition amount of the crystal seeds by utilizing the crystal homogenization coalescence caused by the flow field, ensures that less crystal seeds can complete the homogenization of the particle size, adjusts the crystal seed addition and stirring speed to regulate the crystal particle size distribution range, and realizes the accurate control of the particle size distribution of the product.
3. According to the invention, different cooling rates are designed in different temperature intervals according to the parameters of molecular thermodynamics and crystal growth kinetics of erythritol. In a higher temperature range (above 55 ℃), the nucleation of erythritol is obviously inhibited, and the growth is improved. Under reasonable cooling rate, add the trace seed crystal and can restrain the secondary nucleation, and below 55 ℃, though the nucleation promotes, under the same supersaturation, the system is more easy to nucleate, but the seed crystal that adds in earlier stage has obviously grown up, has more crystal faces to accept the supersaturation and consumes, consequently can accelerate cooling rate gradually. By reasonably designing the cooling curve, the wide particle size distribution caused by secondary nucleation can be remarkably inhibited.
4. After the crystallization is finished according to the preparation method, the obtained erythritol crystals have uniform grain size, more than 89.2wt% of the erythritol crystals can be 20-40 meshes, and more than 97.0wt% of the erythritol crystals can be 20-60 meshes. The dissolving time of 30g of product in 100g of water at 25 ℃ in a constant-temperature water bath is 96-105s, and the dissolving speed is obviously faster than that of the product prepared by the erythritol crystals in the same field. And has an angle of repose of 21.3 to 22.6 DEG and good fluidity. Has wide application in the food chemical industry fields of sugar-free beverage production, granular food compounding and the like.
Drawings
FIG. 1: the solubility and metastable zone curve of erythritol;
FIG. 2: an optical microscope picture of erythritol crystals of example 1;
FIG. 3: an optical microscope picture of erythritol crystals of example 2;
FIG. 4 is a schematic view of: an optical microscope picture of erythritol crystals of example 3;
FIG. 5: an optical microscope picture of erythritol crystals of comparative example 1;
FIG. 6: the optical microscope picture of erythritol crystals of comparative example 2;
FIG. 7: the optical microscope picture of erythritol crystals of comparative example 3;
FIG. 8: the optical microscope picture of erythritol crystals of comparative example 4;
FIG. 9: the optical microscope picture of erythritol crystals of comparative example 5;
FIG. 10: the optical microscope picture of erythritol crystals of comparative example 6;
FIG. 11: a graphical representation of a method for measuring dissolution rate;
FIG. 12: a graphical representation of a method of measuring angle of repose;
FIG. 13: a method for measuring the angle of repose.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitation of the present invention.
In order to make the technical solutions of the present application more clearly understood by those skilled in the art, the technical solutions of the present application will be described in detail below with reference to specific embodiments. If the experimental conditions not specified in the examples are specified, the conditions are generally conventional or recommended by the reagent company; the erythritol raw material used in the following examples was purchased from fuyo biotechnology, shandong, having a purity of 99.6wt% or more in dry matter, and other reagents, consumables, etc. used therein were commercially available, unless otherwise specified.
Example 1:
(1) And (3) evaporation and concentration: taking a certain amount of erythritol sugar solution (10 wt%), evaporating and concentrating to 65wt% under the vacuum degree of 0.04MPa, maintaining the temperature at 65 ℃, and stirring at the power of 0.1kW/m 3 ；
(2) Adding seed crystals: injecting the solution into a crystallizer with a guide cylinder, cooling to 65 ℃ and keeping the temperature stableAdding 3.36g300-325 mesh crystal seed (solute mass fraction 0.2 wt%) for 1h, stirring power is 1.16kW/m 3 ；
(3) Cooling and crystallizing: the cooling rate is within the range of 65-60 ℃, the temperature is reduced by 1.0 ℃ per hour, the temperature is reduced by 2 ℃ per hour within the range of 60.0-54.0 ℃, the temperature is reduced by 3.0 ℃ per hour within the range of 54-39 ℃, the temperature is reduced by 5 ℃ per hour within the range of 39-25 ℃, and the crystallization is stopped when the temperature is reduced to 25 ℃.
(4) Product treatment: the centrifugation speeds of 1000rpm,2000rpm and 3000rpm respectively last for 1min, and drying for 9h at the temperature of 50 ℃.
The solubility and supersaturated solution concentration of erythritol are shown in FIG. 1, and the bulk optical microscope picture of the product is shown in FIG. 2, wherein the crystal size is highly uniform, and each crystal is formed by stacking 2-3 layers of small crystals. The yield of erythritol crystals was detected to be 71.07wt%, and the resulting crystal particle size distribution is shown in the following table (table 1), in which 90wt% of the crystals had a size of 20-40 mesh and 97.8wt% had a size of 20-60 mesh.
TABLE 1 Crystal size distribution of example 1
Example 2:
(1) And (3) evaporation and concentration: taking a certain amount of erythritol sugar solution (15 wt%), the vacuum degree is 0.01MPa, the erythritol sugar solution is evaporated and concentrated to 68wt%, the maintaining temperature is 70 ℃, and the stirring power is 0.05kW/m 3 ；
(2) Adding seed crystals: injecting the solution into a crystallizer with a guide cylinder, cooling to 70 deg.C, maintaining the temperature, adding 6.72g of 250-325 mesh crystal seed (solute mass fraction is 0.6 wt%), maintaining for 1 hr, and stirring at 0.37kW/m 3 ；
(3) Cooling and crystallizing: the cooling rate is in the range of 70-60 ℃, the temperature is reduced by 1.5 ℃ per hour, the temperature is reduced by 2.5 ℃ per hour in the range of 60-54 ℃, the temperature is reduced by 4 ℃ per hour in the range of 54.0-39.0 ℃, the temperature is reduced by 5.5 ℃ per hour in the range of 39-25 ℃, and the crystallization is stopped when the temperature is reduced to 25 ℃.
(4) Product treatment: the centrifugation rotation speed is 1000rpm,2000rpm and 3000rpm, and the drying is carried out for 12 hours at the temperature of 45 ℃ respectively.
The picture of the product of the integral optical microscope is shown in figure 3, the size of the crystal is highly uniform, and each crystal is polymerized by 2-3 layers of small crystals. The yield of erythritol crystals was detected to be 72.46wt%, and the resulting crystal size distribution is shown in the following table (table 2), in which 89.8wt% of the crystals had a size between 20 and 40 mesh, and 98.2wt% was between 20 and 60 mesh.
TABLE 2 Crystal size distribution of example 2
Example 3:
(1) And (3) evaporation and concentration: taking a certain amount of erythritol sugar solution (20 wt%), vacuum degree of 0.08MPa, evaporating and concentrating to 61wt%, maintaining temperature at 60 deg.C, and stirring power at 5kW/m 3 ；
(2) Adding seed crystals: injecting the solution into a crystallizer with a guide flow cylinder, cooling the solution to 60 ℃, adding 4.48g of 250-325 mesh crystal seeds (solute mass fraction is 0.4 wt%) and maintaining for 1h, wherein the stirring power is 2.64kW/m 3 ；
(3) Cooling and crystallizing: the cooling rate is within the range of 60-54 ℃, the temperature is reduced by 0.5 ℃ per hour, within the range of 60-54 ℃, the temperature is reduced by 1 ℃ per hour, within the range of 54-39 ℃, the temperature is reduced by 2 ℃ per hour, within the range of 39-25 ℃, the temperature is reduced by 4.5 ℃ per hour, and the crystallization is stopped when the temperature is reduced to 25 ℃.
(4) Product treatment: the centrifugation speeds are 1000rpm,2000rpm and 3000rpm, and the drying is carried out for 1min respectively, and the drying is carried out for 6h at the temperature of 55 ℃.
The picture of the product by a bulk optical microscope is shown in figure 4, the size of the crystal is highly uniform, and each crystal is polymerized by 2-3 layers of small crystals. The yield of erythritol crystals was detected to be 65.78wt%, and the resulting crystal particle size distribution is shown in the following table (table 3), in which 89.8wt% of the crystals had a size of 20-40 mesh and 97.4wt% had a size of 20-60 mesh.
TABLE 3 Crystal size distribution of example 3
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention and are intended to be equivalent substitutions are included in the scope of the present invention.
Comparative example 1:
erythritol crystals were produced by the method of example 1, except that erythritol seed crystals were added in an amount of 6g of 150-180 mesh crystals (solute mass fraction 0.54 wt%) in comparison with example 1, and the other steps and operations were the same as in example 1.
After crystallization, the stereomicroscope photo of the obtained crystal is shown in fig. 5, the crystal is still relatively uniform, but the crystal face number of the seed crystal is not enough, secondary nucleation occurs to a certain extent, and along with the increase of the size of the seed crystal, the particle size distribution is shown in the following table (table 4), 27.5wt% of the product is larger than 20 meshes, the particle size is mainly distributed between 4-20 meshes and 20-30 meshes, and 27.7wt% of the product exceeds the effective particle size range of the erythritol crystal.
TABLE 4 distribution of crystal grain size of comparative example 1
Comparative example 2:
erythritol crystals were prepared according to the method of example 1, except that the z-axis flow field was applied without using a draft tube, and the back-mixing was promoted with a double-layer propeller, and the other steps and operations were the same as in example 1.
After crystallization is finished, the stereogram of the obtained crystal is shown in fig. 6, and as a z-axis flow field is not applied, wet agglomeration of erythritol cannot be effectively controlled, so that 1-4 layers of unequal small crystal coalescence are generated, a large amount of scaling substances are generated, and the particle size distribution is widened. The particle size distribution is shown in the following table (table 5), with 18.3wt% product larger than 20 mesh and 23.5wt% outside the effective particle size range of the erythritol crystals.
TABLE 5 Crystal grain size distribution of comparative example 2
Comparative example 3:
erythritol crystals were prepared by the method of example 2, differing from example 1 in that the stirring power was 4.98kW/m 3 The other steps and operations were the same as in example 1.
After the crystallization, the bulk optical microscope photograph of the obtained crystal is shown in fig. 7, and the crystal has non-uniform particle size, both agglomeration and non-agglomeration, and more fine crystals. The particle size distribution is shown in the following table (table 6), 11wt% of the product is smaller than 60 mesh, and 11.8wt% is out of the erythritol effective particle size range.
TABLE 6 Crystal grain size distribution of comparative example 3
Comparative example 4:
erythritol crystals were prepared according to the method of example 2, except that the cooling rate was 2.5 ℃ per hour at a constant rate, and the other steps and operations were the same as those of example 1.
As shown in FIG. 8, the crystal size of the obtained crystal was not uniform but much fine-grained, and the photograph of the crystal by a bulk optical microscope was taken after the crystallization. The partial agglomeration phenomenon tends to be fine-grained adhesion. The particle size distribution is shown in the following table (table 7), with 13.2wt% of the product having a particle size greater than 20 mesh and 22.4wt% outside the effective particle size range of erythritol.
TABLE 7 distribution of crystal grain size of comparative example 4
Comparative example 5:
erythritol crystals were prepared according to the method of example 3, which is different from example 3 in that the cooling rate was divided into two stages, that is, 3 ℃ per hour at a temperature in the range of 60 to 45 ℃ and 5 ℃ per hour at a temperature in the range of 45 to 25 ℃ to stop crystallization when the temperature is reduced to 25 ℃. The other steps and operations were the same as in example 3.
After the crystallization, the stereomicroscope photograph of the obtained crystal is shown in fig. 9, the crystal grain size is not uniform, more fine crystals exist, and the partial agglomeration phenomenon tends to be fine crystal adhesion. The particle size distribution is shown in the following table (table 8), 8.4wt% of the product has a particle size greater than 20 mesh, and 19.0wt% is outside the range of the effective particle size of erythritol.
TABLE 8 Crystal grain size distribution of comparative example 5
Comparative example 6:
the erythritol crystals are prepared according to the method of patent CN113912475A, and after crystallization is finished, the bulk optical microscope photograph of the obtained crystals is shown in fig. 10, and the obtained product is consistent with the crystal morphology obtained in patent CN113912475A, and mostly exists in a single crystal form. The particle size distribution is as follows (Table 9), with 85.9wt% product having a particle size between 20 and 40 mesh. 98.6wt% of the crystals are larger than 40 mesh, which meets the standard that most of the grain diameter is above 50 mesh.
TABLE 9 Crystal grain size distribution of comparative example 6
The crystal form refers to an arrangement mode of crystal molecules in the crystal, and is important physicochemical properties of the crystal, and for a polymorphic substance, certain physicochemical properties (such as melting point, solubility and stability) may be different due to different crystal forms; under different conditions, mutual transformation and crystal transformation may occur among the crystal forms. In order to verify whether the crystal form difference exists between the erythritol agglomerated crystal and an erythritol common crystal, XRD characterization is carried out on the erythritol agglomerated crystal in the example 1 and the erythritol large-particle crystal in the comparative example 6, the diffraction peak position is shown in figure 11, and according to the specification of the year 2015 version P372 of Chinese pharmacopoeia, if the crystal form substances of two crystalline samples are judged to be the same, the error range of the diffraction peak positions of the two crystalline samples is within +/-0.2 degrees. In fig. 11, it can be seen that the corresponding diffraction angles of the peak positions of the erythritol crystals with two different morphologies are the same, and therefore, it can be considered that the erythritol agglomerated crystal in the patent has a consistent crystal form compared with a common product, and a crystal transformation phenomenon does not occur in the crystallization process.
In addition, the angles of repose and dissolution rates of the different examples and comparative examples were tested to evaluate their potential for use in beverages. The dissolution rate test method adopts a laser diffraction method, and is characterized in that 30g of erythritol crystal product is poured into 100g of pure water at 25 ℃ and 300rpm, a signal receiver signal jumps, the signal receiver signal intensity gradually decreases along with the dissolution of the crystal, when the signal receiver shows that a value is lower than a certain value and is kept unchanged, the dissolution of the crystal is judged to be finished, and the required time is the dissolution time, as shown in fig. 12, the angle of repose test method is according to the angle of repose measurement method provided by patent CN113412266A, as shown in fig. 13, and the following table (table 10) shows the angle of repose and the dissolution rate of different examples and comparative examples.
TABLE 10 dissolution rate and angle of repose of the crystalline products obtained in the different examples and comparative examples.
As can be seen from a comparison between example 1 and comparative example 1, when the amount of the seed crystal added is out of the range defined in the present invention, the particle size distribution of the product is significantly large because the seed crystal having a larger particle size grows into larger crystals, and these larger crystals are further agglomerated to form larger crystals, which leads to a runaway particle size distribution, and further, the number of large particle seed crystals is smaller in the same mass, and the consumption capacity for supersaturation is insufficient, which leads to secondary nucleation of erythritol. These factors broaden the particle size distribution of erythritol crystals, a considerable portion of the crystals are out of the range of particle sizes in which erythritol is suitable for sale, the dissolution rate is low due to the larger particle size, the fluidity is also reduced due to the uneven particle size distribution, and the angle of repose is increased.
It can be known from the comparison between the embodiment 1 and the comparative example 2 that when the x-axis and y-axis flow fields are the same, when the guide cylinder and the propulsion paddle are not used to apply the integral z-axis flow field, and the double-layer stirring is used for carrying out local z-axis back mixing, the agglomeration of the erythritol can not be controlled, and a dead zone can be formed locally, so that the scaling occurs in the crystallizer, a non-agglomerated large block is formed when the scaling falls off, and the product particle size of the erythritol is larger due to the factors, so that the product requirement can not be met. The dissolution rate is low due to the large particle size, and the fluidity is reduced and the angle of repose is increased due to the uneven particle size distribution.
It can be seen from a comparison of example 2 and comparative example 3 that when the stirring rate is too high, a large shearing force and dispersion work are brought about, and that when a certain degree is reached, the dispersion work of the crystals in the solution is made smaller than the adhesion work, so that a part of the crystals does not participate in the agglomeration. In addition, a part of crystals can be broken by excessive shearing force, so that broken crystals are excessive, the particle size distribution is out of control, the crystal morphology is reduced, and the risk of agglomeration of subsequent products is increased. Thus, although the particle size is small and the dissolution rate is high, the particle size distribution is not uniform and the amount of crushed crystals is large, the fluidity is reduced, and the angle of repose is increased.
Through embodiment 2 and comparative example 4, learn, when the cooling rate adopts at the uniform velocity cooling, the seed crystal can't consume the sufficient supersaturation within the interval of partial cooling to can take place the outbreak nucleation that supersaturation accumulation triggered, cause the particle size distribution widen, the mobility is poor, angle of repose is big, because the macrocrystalline content is showing and increases, consequently whole dissolving rate is on the low side, can't satisfy the requirement of its application to the product.
Through embodiment 3 and comparative example 5 learn, when the cooling rate adopts two segmentation cooling to replace four segmentation cooling, the partial interior seed crystal of cooling interval still can't consume the degree of supersaturation of capacity to can take place the outbreak nucleation, cause the particle size distribution widen, mobility is poor, the angle of repose is big, because the macrocrystalline content is showing and is increasing, therefore whole dissolution rate is on the low side, can't satisfy the requirement of its application to the product.
It is understood from example 3 and comparative example 6 (patent CN 113912475A) that the dissolution rate of erythritol single-crystal grains is significantly lower than that of the agglomerated crystals prepared by the present method, because the surface area of the dough agglomerate is significantly larger than that of the single-crystal grains for the same volume, and on the other hand, the agglomerated flower-like structure has a significantly reduced dissolution radius compared to the single-crystal grains of the same grain size, so that the dissolution rate of the agglomerated crystals is greatly increased. On this basis, by making the grain size uniform and effectively controlling the degree of agglomeration, it is possible to maintain a similar fluidity as compared with a single crystal.
The erythritol crystal disclosed and provided by the invention and the preparation method and the application thereof can be realized by appropriately changing part of links by referring to the content in the text by a person skilled in the art. While the methods of the present invention have been described in terms of preferred embodiments, it will be apparent to those of ordinary skill in the art that variations and modifications in the methods and products described herein, as well as appropriate variations and combinations, may be made to implement the techniques of the present invention without departing from the spirit and scope of the invention. It is expressly intended that all such similar substitutes and modifications apparent to those skilled in the art are deemed to be within the spirit, scope and content of the invention.
Claims (10)
1. A preparation method of erythritol crystals is characterized by comprising the following steps:
adding erythritol seed crystal into erythritol concentrated solution with the temperature of 60-70 ℃, and cooling and crystallizing in four sections under the action of a flow field and stirring to obtain erythritol crystals.
2. The method according to claim 1, wherein the erythritol concentrated solution having a temperature of 60 to 70 ℃ is prepared by a method comprising: evaporating and concentrating 10-20wt% erythritol solution at constant temperature of 60-70 deg.C to 50-70wt%;
preferably, the method for preparing the erythritol concentrated solution with the temperature of 60-70 ℃ comprises the following steps: evaporating and concentrating erythritol solution with the concentration of 10-15wt% at the constant temperature of 60-70 ℃ to 61-68wt%;
preferably, the vacuum degree of the constant-temperature evaporation is 0.01-0.08MPa.
Preferably, the stirring power of the constant-temperature evaporation is 0.05-5kW/m 3 。
3. The method according to claim 1, wherein the erythritol concentrated solution is prepared in a sugar boiling tank or a vacuum evaporation crystallizer.
4. The preparation method according to claim 1, wherein the erythritol seed crystal has a particle size of 250-325 mesh;
preferably, the erythritol seed crystal is added in an amount of 0.2-1wt%, preferably 0.3-0.6wt% based on the dry matter content of erythritol in the erythritol concentrate.
5. The production method according to claim 1, wherein the flow field is a flow field in which a z-axis direction and a tangential direction coexist;
preferably, the z-axis flow field is applied through a flow sleeve.
Preferably, the flow field tangential direction is applied by a single layer of three-bladed propeller;
preferably, the stirring power during the temperature reduction crystallization is 0.37-2.64kW/m 3 。
6. The preparation method according to claim 1, wherein the cooling crystallization comprises four steps, wherein the temperature is reduced from 70-60 ℃ to 64-54 ℃ in the first step at a rate of 0.5-1.5 ℃/h, the temperature is reduced from 64-54 ℃ to 54-39 ℃ in the second step at a rate of 1-2.5 ℃/h, the temperature is reduced from 54-39 ℃ to 39-25 ℃ in the third step at a rate of 2-4 ℃/h, and the temperature is reduced from 39-25 ℃ to 25-20 ℃ in the third step at a rate of 4.5-6 ℃/h.
7. The method for preparing the silicon nitride powder according to the claim 1, wherein the cooling crystallization is realized in a vertical cooling crystallizer with a guide cylinder, a cooling crystallizing tank with a guide cylinder or a cooling crystallizer with a guide cylinder.
8. The preparation method according to claim 1, further comprising sequentially performing solid-liquid separation, washing and drying on the mixed solution obtained by cooling and crystallizing;
preferably, the solid-liquid separation mode is centrifugation;
preferably, the drying mode is normal pressure drying, the drying temperature is 25-55 ℃, and the drying time is 6-48h.
9. Erythritol crystals prepared by the production method according to any one of claims 1 to 8;
preferably, the erythritol crystals have uniform particle size, wherein more than 89.2wt% of the erythritol crystals have a crystal size of 20-40 mesh, and more than 97wt% of the erythritol crystals have a crystal size of 20-60 mesh;
preferably, the angle of repose of the erythritol crystals is 21.3 to 22.6 °.
10. Use of erythritol crystals according to claim 9 in the preparation of a sugarless functional beverage.
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