CN114586874A - Method for realizing multi-structure low-fat chocolate two-channel 4D printing by inducing deformation - Google Patents
Method for realizing multi-structure low-fat chocolate two-channel 4D printing by inducing deformation Download PDFInfo
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- CN114586874A CN114586874A CN202210229759.1A CN202210229759A CN114586874A CN 114586874 A CN114586874 A CN 114586874A CN 202210229759 A CN202210229759 A CN 202210229759A CN 114586874 A CN114586874 A CN 114586874A
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- chocolate
- cocoa butter
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Images
Classifications
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A23G1/00—Cocoa; Cocoa products, e.g. chocolate; Substitutes therefor
- A23G1/30—Cocoa products, e.g. chocolate; Substitutes therefor
- A23G1/32—Cocoa products, e.g. chocolate; Substitutes therefor characterised by the composition containing organic or inorganic compounds
- A23G1/36—Cocoa products, e.g. chocolate; Substitutes therefor characterised by the composition containing organic or inorganic compounds characterised by the fats used
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G1/00—Cocoa; Cocoa products, e.g. chocolate; Substitutes therefor
- A23G1/0003—Processes of manufacture not relating to composition or compounding ingredients
- A23G1/0046—Processes for conditioning chocolate masses for moulding
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G1/00—Cocoa; Cocoa products, e.g. chocolate; Substitutes therefor
- A23G1/0003—Processes of manufacture not relating to composition or compounding ingredients
- A23G1/005—Moulding, shaping, cutting, or dispensing chocolate
- A23G1/0053—Processes of shaping not covered elsewhere
- A23G1/0056—Processes in which the material is shaped at least partially by a die; Extrusion of cross-sections or plates, optionally with the associated cutting
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23G—COCOA; COCOA PRODUCTS, e.g. CHOCOLATE; SUBSTITUTES FOR COCOA OR COCOA PRODUCTS; CONFECTIONERY; CHEWING GUM; ICE-CREAM; PREPARATION THEREOF
- A23G1/00—Cocoa; Cocoa products, e.g. chocolate; Substitutes therefor
- A23G1/30—Cocoa products, e.g. chocolate; Substitutes therefor
- A23G1/32—Cocoa products, e.g. chocolate; Substitutes therefor characterised by the composition containing organic or inorganic compounds
- A23G1/36—Cocoa products, e.g. chocolate; Substitutes therefor characterised by the composition containing organic or inorganic compounds characterised by the fats used
- A23G1/38—Cocoa butter substitutes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Abstract
The invention discloses a method for realizing multi-structure low-fat chocolate two-channel 4D printing by inducing deformation, and belongs to the technical field of healthy fat products and chocolate 4D printing application thereof. The method comprises the following steps: (1) mixing W/O/W fat and cocoa butter, cocoa butter equivalent or cocoa butter substitute according to the mass ratio of 1: (1.1-10), and uniformly mixing; then adding auxiliary materials, and grinding to obtain a first type of slurry system; (2) mixing W/O/W fat and cocoa butter, cocoa butter equivalent or cocoa butter substitute according to the mass ratio of 1: (0.1-1), and uniformly mixing; then adding auxiliary materials, and grinding to obtain a second type slurry system; (3) and carrying out double-channel printing to obtain a chocolate model, and then carrying out thermal induction deformation to realize 4D printing. The method can be applied to the development of 4D printed food.
Description
Technical Field
The invention relates to a method for realizing multi-structure low-fat chocolate two-channel 4D printing by inducing deformation, and belongs to the technical field of healthy fat products and chocolate 4D printing application thereof.
Background
The method is characterized in that macromolecular substances such as vegetable protein and polysaccharide are utilized to structure liquid vegetable oil, and nano-particles are adsorbed on an oil-water interface by means of micro-gelation and the like, so that the traditional solid grease is replaced. The system can ensure the stability of the liquid vegetable oil for a long time, and realizes the substitution of the traditional solid grease.
The 3D printing technology is also called Additive Manufacturing (AM), which integrates computer aided design, material processing and molding technology, designs a 3D model by using digital model software, generates a plurality of corresponding layers of three-dimensional slices by slice software, calculates a path of each layer of slices by using a programming G code and finally inputs the path into printing equipment. The equipment moves according to a preset path and extrudes printing materials according to a specified speed through recognizing the codes, and a product with a three-dimensional structure is built through layer-by-layer stacking of the materials according to the principle of layered manufacturing and layer-by-layer stacking. Food 3D printing technique compares with traditional means of making, and 3D prints and can realize that the precision is higher, the product production that the structure is more stable to the accuracy and the quality of improvement product that can be very big. In the process of small-range production, materials can be saved to the maximum extent, the design mode is simpler and more flexible, and meanwhile, personalized customization is also considered. The method can meet the demand of real-time orders and fast customized production, and compared with the traditional food industry supply chain, the method can greatly shorten the reaction time and cost of the supply chain and simplify the customized food service.
The 4D printing is a structure printed by 3D (such 3D printed products are generally made of different raw materials and are printed by two channels to form a multi-structure product), and can change its physical and chemical properties under a certain stimulus (temperature, humidity, illumination, magnetic field, etc.), and the change is generally in the form of one or more of shape, color and flavor. In the food field, the appearance can be changed after thermal induction, so that the food has rich visual effect, and diversification, customization and interest of the products are realized.
The current 4D printing is mainly applied to materials taking starch as a main component, and the causes of induced deformation are basically structural curling and the like caused by a high-temperature dehydration effect. The chocolate system is a lipid product constructed by protein-based stable liquid oil, the components are more complex, and 4D printing requires certain melting point difference between two materials and better printing strength; the difficulty of preparing chocolate by 4D printing is higher.
Disclosure of Invention
[ problem ] to
Because 4D printing requires that a certain melting point difference exists between two materials and excellent printing strength is realized, no document discloses that liquid oil replaces cocoa butter to construct a chocolate system by using a 4D printing technology.
[ solution ]
In order to solve the above problems, the present invention stabilizes liquid vegetable oils of different internal phases with vegetable-based proteins to obtain solid fats with excellent physical properties, and obtains aqueous chocolate products having similar properties to conventional chocolate by adjusting different cocoa butter substitution ratios.
According to the invention, a double-channel 3D printing technology is adopted to obtain multi-structure low-fat water-containing chocolate, and then the multi-layer and multi-system structure constructed by printing is printed by utilizing different thermodynamic properties of the water-containing chocolate, so that the form change under the stable condition of an external environment, namely the 4D printing effect is realized.
The invention provides a method for realizing multi-structure low-fat chocolate two-channel 4D printing by inducing deformation, which comprises the following steps of:
(1) preparation of chocolate paste of the first type
Uniformly mixing the W/O/W fat and the cocoa butter equivalent or cocoa butter substitute according to the mass ratio of 1: 1.1-10; then adding auxiliary materials, and grinding to obtain a first type of slurry system;
(2) preparation of chocolate mass of the second type
Uniformly mixing the W/O/W fat and the cocoa butter equivalent or cocoa butter substitute according to the mass ratio of 1: 0.1-1; then adding auxiliary materials, and grinding to obtain a second type slurry system;
(3)4D printing:
filling the first type of chocolate paste into one printing tube, filling the second type of chocolate paste into the other printing tube, and performing double-channel printing to obtain a chocolate model; the chocolate model is placed in an environment with the temperature of 30-36 ℃ for thermal induction deformation for 30-120 s, so that the outer layer of chocolate is melted, and 4D printing is realized.
The preparation method of the W/O/W fat comprises the following steps:
preparing a protein isolate solution with the mass concentration of 5-20%, and hydrating to obtain a hydrated protein isolate solution; wherein the protein isolate comprises one or more of peanut, pea, mung bean and soybean protein isolate;
secondly, shearing the hydrated protein isolate solution obtained in the first step at a high speed, and homogenizing at a high pressure to obtain a nano-scale protein isolate dispersion liquid;
thirdly, heating the nanoscale protein isolate dispersion liquid obtained in the second step to obtain modified protein isolate dispersion liquid;
fourthly, adding transglutaminase TGase into the separated protein dispersion liquid obtained in the third step for reaction to obtain separated protein glue;
fifthly, adding diluent into the separated protein gel obtained in the step IV, and carrying out micro-jet and high-pressure homogenization to obtain a nano microgel solution;
sixthly, adding the nano gel dispersion liquid after the gelation treatment obtained in the fifth step into liquid edible vegetable oil, and performing high-speed shearing treatment to obtain W/O system emulsion, wherein the liquid edible vegetable oil is a continuous phase, and the nano gel dispersion liquid after the gelation treatment is a dispersed phase;
seventhly, using the whole W/O emulsion obtained in the step (c) as a dispersed phase, using the gelatinized nano microgel dispersion liquid obtained in the step (c) as a continuous phase, and performing secondary emulsification and high-speed shearing treatment to obtain the double-emulsified W/O/W fat.
In one embodiment of the invention, the first type of chocolate mass in step (1) is a low-melting point chocolate mass, and the melting point is in the range of 26-32 ℃.
In one embodiment of the invention, the second type of chocolate mass in step (2) is a high melting point chocolate mass, the melting point range is 33-38 ℃.
In one embodiment of the invention, the auxiliary materials in step (1) comprise cocoa powder/milk powder, powdered sugar, soybean lecithin; the mass ratio of the cocoa butter, the cocoa butter equivalent or the cocoa butter substitute to the cocoa powder/milk powder, the powdered sugar and the soybean lecithin in the first chocolate slurry is 1: 0.05-0.2: 0.1-0.5: 0.001-0.01.
In one embodiment of the invention, the auxiliary materials in the step (2) comprise cocoa powder, powdered sugar, soybean lecithin; the mass ratio of the cocoa butter, the cocoa butter equivalent or the cocoa butter substitute to the cocoa powder, the sugar powder and the soybean lecithin in the second chocolate paste is 1: 0.4-2: 0.5-3: 0.001-0.1.
In one embodiment of the invention, the cocoa butter equivalents in steps (2) and (1) comprise one or more of shea butter, sal fat, mango kernel oil, kokum butter, palm oil melting point fraction, and illipe butter; the cocoa butter substitute comprises one or more of lauric acid type cocoa butter substitute and non-lauric acid type cocoa butter substitute.
In one embodiment of the invention, the grinding in steps (2) and (1) is carried out by adding grinding beads into a refining cylinder, refining for 2-3 h at room temperature with a double-shaft refiner rotating speed of 1000-1500 r/min, and determining the fineness of the chocolate slurry to be less than 25 μm by using a fineness determinator.
In one embodiment of the present invention, the volume of the 3D printing syringe used in step (3) is 20-100 mL, and a PVC plastic or aluminum syringe may be used according to the temperature used.
In one embodiment of the invention, the chocolate mold in step (3) is a multi-layered, multi-structured chocolate mold with two chocolate masses interspersed.
In one embodiment of the invention, the first type (low melting point) of slurry in the chocolate mould in step (3) constitutes the outer structure; the second type (high melting point) of slurry constitutes the internal structure.
In an embodiment of the present invention, the two-pass printing in step (3) specifically includes:
adjusting the temperature in the printing chamber, selecting a 3D printing gun head for filling, and adjusting all the axes of the 3D printer X, Y, Z to be zero through program setting;
designing a 3D model by using digital model software, generating a plurality of corresponding layers of three-dimensional slices by using slice software to obtain slice models, calculating a path of each layer of slices by using a programming G code, and finally inputting the path to printing equipment;
setting various parameters in the 3D printing process according to different materials and diameters of selected needles;
3D printing is carried out by the equipment by adopting an extrusion method according to the imported slice model to form a customized model with certain self-supporting property, namely a chocolate model;
wherein, the internal temperature of the printing chamber is adjusted according to different liquid vegetable oil, cocoa butter or cocoa butter equivalent or cocoa butter substitute and mass percentage ratio, the set temperature is in the range of 0-40 ℃, and the preferred temperature is 20-25 ℃;
the used data modeling software is 3ds Max 2020 version, wherein the derived 3D model is stl format, the used slicing software is replay-host version, and the sliced file format is gcode format;
the printing parameters are as follows: the printing layer is 0.2-1.2 mm thick, the wall thickness is 0.4-1.2 mm, the filling density is 10-60%, the bottom layer and the top layer are 0.2-1.2 mm thick, the printing speed is 40-120 mm/s, the printing temperature is 0-40 ℃, the initial layer thickness is 0.2-0.8 mm, the line width of the initial layer is 10-80%, the bottom layer is cut off to be 0mm, the moving speed is 20-200 mm/s, the bottom layer speed is 20-120 mm/s, the filling speed is 20-120 mm/s, the bottom layer speed and the top layer speed are 20-100 mm/s, the shell speed is 20-120 mm/s, and the inner wall speed is 10-80 mm/s;
the offset value of the two printing head intervals of the dual-channel printer needs to be set to be 64mm, the upper solid layer is 0-3 layers, and the lower solid layer is 0-3 layers.
In one embodiment of the invention, the solvent adopted by the protein separation solution in the step (r) in the preparation method of the W/O/W fat-like substance comprises one or two of phosphate buffer solution and water; the hydration is to put the protein isolate solution at low temperature for hydration; the low temperature is 1-10 ℃ for refrigeration for 10-18 hours, preferably 1-4 ℃ for refrigeration for 12-16 hours;
secondly, the high-speed shearing is carried out for 1-3 minutes at 5000-15000 rpm; the high-pressure homogenization is carried out at 20-100 Mpa for 1-4 minutes;
heating for 30-60 minutes at 80-90 ℃ to obtain a protein solution with a stretched structure and better hydrophobic property;
before the reaction, the pH value needs to be adjusted to be 6.2-7.3, preferably 6.7-7.1, and in the range, the dispersion of protein is facilitated, and a gel network is formed more easily through the cross-linking of amino acid residues; the addition amount of transglutaminase TGase in the step (iv) is 2-10U/g, and the reaction conditions are as follows: crosslinking for 2-4 hours at a low temperature of 30-45 ℃, and then heating in a water bath at a temperature of 85-100 ℃ for 5-20 minutes to obtain protein gel, so that an isopeptide bond is formed between Lys and Gln and the protein gel is constructed to form the protein gel;
the diluent in the fifth step comprises one or two of phosphate buffer solution and water, and the mass ratio of the diluent to the protein gel is 2: 1; treating for 2-4 minutes under the condition of 20-200 Mpa of microjet; the high-pressure homogenization is carried out under the condition of 60-100 Mpa for 1-4 minutes;
in the step (sixthly), the edible vegetable oil is one or more of soybean oil, rapeseed oil, peanut oil, sunflower seed oil, rice bran oil, corn oil, linseed oil, olive oil, wheat germ oil, cottonseed oil, almond oil, tea seed oil and sesame oil, wherein the vegetable oil accounts for 70-90% of the mass percent of the nano gel dispersion liquid obtained in the step (fifth); the high-speed shearing is carried out at 5000-15000 rpm for 1-2 minutes; the mass concentration of the protein isolate in the obtained W/O system is 0.2-5%;
the volume ratio of the dispersed phase to the continuous phase is 40-70: 30, and the preferable ratio is 50-60: 30; the high-speed shearing is carried out for 1-3 minutes at 5000-15000 rpm; in the obtained double emulsified W/O/W fat, the mass concentration of the nano microgel in the continuous phase is 0.2-2%.
The second object of the invention is the 4D printed chocolate produced by the process of the invention.
[ advantageous effects ]
(1) The W/O/W structured fat prepared by the invention effectively reduces the fat content and the saturated fatty acid content in the traditional chocolate by replacing the traditional cocoa butter, cocoa butter equivalent or cocoa butter substitute in the chocolate, and simultaneously realizes the construction of multilayer multi-structure low-fat chocolate by combining a two-channel food 4D printing technology, thereby enhancing the practical value of the structured fat product in the food field.
(2) The invention adjusts the internal phase proportion of different liquid vegetable oils to obtain the most stable structured grease, and simultaneously makes different gradient contrasts on the replacement proportion of the structured grease to cocoa butter, cocoa butter equivalent or cocoa butter substitute in a chocolate system, selects products with similar physical properties but different thermodynamic properties with the traditional chocolate, and can be applied to the development of 4D printing of foods.
(3) The invention utilizes two different materials, combines the advantages of a dual-channel printer, constructs a printing product with a plurality of layers and structures, can realize the effect of mutually staggering the two materials on the same layer, and utilizes the difference of thermodynamic properties to realize spontaneous structural change under certain thermal induction conditions, namely 4D printing.
Drawings
Fig. 1 shows a low-fat black chocolate 3D printing product constructed by using structured fat instead of cocoa fat, which is constructed by using different liquid vegetable oil proportions in example 2, wherein the oil phase proportions are 36%, 45%, 54% and 63% from left to right.
FIG. 2 is a representation of the multilayer multi-structured Taiji pattern obtained using a two-pass printer and a low fat chocolate model of school badge of south of the Yangtze university in example 2 with an oil phase ratio of 54%.
Fig. 3 shows a low fat black chocolate 3D printed product constructed using a structured fat, i.e. a fat-containing substitute for cocoa butter at various ratios in example 3, with the substitution ratios of cocoa butter being 0%, 25%, 50%, 75%, 100% from left to right.
Figure 4 is a DSC thermodynamic analysis of different 3D printed chocolates constructed in example 3 at different cocoa butter substitution ratios.
FIG. 5 is a printed mechanical diagram (A) and a rheological property change (B) at the cocoa butter substitution ratios of 0% and 100% in example 3.
FIG. 6 is a scanning microscope photomicrograph of the surface atomic force at the cocoa butter substitution ratios of 0%, 50% and 100% in example 3, in which Ra is the surface average roughness of chocolate, and higher values indicate that the surface is rougher.
FIG. 7 is a variation of the modeling, slicing, printing and 4D printing of two different types of melting point chocolate made in example 4, wherein the inner high melting point dark chocolate is heart shaped and the outer low melting point dark (white) chocolate is a cuboid.
Fig. 8 is a 4D print of a low fat dark chocolate with a cocoa butter substitution ratio of 50% in example 4, showing a spontaneous structural change within 60s at 35 ℃.
FIG. 9 is a low fat chocolate model of the multilayer multi-structured Taiji graphic and school badge of south of the Yangtze university obtained using the two-channel printer of comparative example 1.
Fig. 10 is a model of the structure of the pentagram and the square frame printed at 35 c in comparative example 2.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of better illustrating the invention and is not intended to limit the invention thereto.
The test method comprises the following steps:
determination of the melting crystallization Curve: firstly, correcting an instrument by using indium and n-octadecane, then weighing 5-8 mg of a sample in an aluminum box, and measuring the temperature program of the sample: cooling from room temperature to-10 deg.C at 10 deg.C/min, maintaining for 5min to crystallize completely, heating to 50 deg.C at 10 deg.C/min, and maintaining for 5min to obtain melting curve. The onset, maximum, end and enthalpy (Δ H) of the melting peak are then obtained by the DSC software.
Rheological Property testing: the Linear Viscoelastic Region (LVR) is determined by strain scanning with a strain amplitude in the range of 0.1-100 Pa. In the measurement of the strain restoring force, the strain force is 0.1pa when 0-120s, 100pa when 120-240s and 0.1pa when 240-360 s. In addition, an aluminum plate (diameter 40mm) was used for all the tests, and the gap value was set to 1000 μm.
Hardness test of chocolate: the chocolate was stabilized at 20 ℃ and 32 ℃ for 12 hours, and the hardness was measured by cutting with a blade probe. The conditions were such that the blade height was 15mm from the upper surface of the sample, the pre-measurement rate was 10mm/s, the test rate was 0.5mm/s, the return rate was 10mm/s, and the compression distance was 50%.
Example 1
A method for preparing W/O/W fat based on nano-scale pea protein comprises the following steps:
(1) preparing a pea protein isolate solution with the mass concentration of 10% by taking a phosphate buffer solution as a solvent, fully stirring at 300rpm for 2 hours, adjusting the pH value to 6.7, and refrigerating in a refrigerator at 4 ℃ for 12 hours to obtain the pea protein isolate solution;
(2) carrying out high-speed shearing (10000rpm for 2 minutes) on the hydrated pea protein isolate solution obtained in the step (1), and carrying out high-pressure homogenization (100Mpa for 3 minutes) to obtain a nano-scale pea protein isolate dispersion;
(3) heating the pea protein isolate dispersion liquid in the step (2) in a water bath kettle at 80 ℃ for 20 minutes, and then cooling to 40 ℃ to obtain a modified pea protein isolate dispersion liquid;
(4) adding 15U/g transglutaminase TGase into the pea protein isolate dispersion liquid in the step (3), adjusting the pH to 7, carrying out enzyme crosslinking in a water bath kettle at 40 ℃ for 2 hours, and finally heating in the water bath kettle at 90 ℃ for 50 minutes to obtain pea protein isolate glue;
(5) adding 2 times of phosphate buffer solution by mass into the separated protein gel obtained in the step (4), and homogenizing under high pressure (processing at 100Mpa for 2 minutes) to obtain a nano-scale pea protein microgel solution;
(6) adding 10mL of the nano gel particle dispersion liquid obtained in the step (5) into 90mL of soybean oil, and performing high-speed shearing treatment (12000rpm for 2 minutes) to obtain a W/O emulsion system; wherein the soybean oil accounts for 90 percent of the mass of the nano microgel solution; the mass concentration of the pea protein in the whole system is 1 percent;
(7) and (3) mixing 40 mL, 50 mL, 60 mL and 70mL of the W/O emulsion obtained in the step (6) with 30mL of the nano microgel particle dispersion liquid obtained in the step (5), and performing high-speed shearing (processing at 10000rpm for 1 minute) to obtain the double-emulsified W/O/W fat, wherein the oil phase in the emulsion system accounts for 36, 54, 45 and 63 percent.
Example 2 optimization of the proportions of the different oil phases
A method for realizing multi-structure low-fat chocolate two-channel 4D printing by inducing deformation comprises the following steps:
(1) preparation of a first type (Low melting) chocolate mass
8.75g of W/O/W lipid and 26.25g of cocoa butter with different oil phase ratios in example 1 are placed in a water bath pot to be dissolved, and are uniformly mixed with 20g of cocoa powder, 44.5g of powdered sugar and 0.5g of soybean lecithin, and the mixture is continuously refined at 1200rpm/min for 3 hours by using a ball mill to obtain a first type (low melting point) chocolate slurry;
(2) preparation of chocolate mass of the second type (high melting point)
Placing 17.5g of W/O/W lipid and 17.5g of cocoa butter in different oil phase ratios in the example 1 into a water bath pot for dissolving, uniformly mixing with 20g of cocoa powder, 44.5g of powdered sugar and 0.5g of soybean lecithin, and continuously finely grinding for 3h at 1200rpm/min by using a ball mill to obtain a second type (high melting point) chocolate slurry;
(3)4D printing:
filling the first type of chocolate paste into a first 100mL printing tube, and filling the second type of chocolate paste into a second 100mL printing tube;
adjusting the temperature in the printing chamber to be 25 ℃, selecting a 3D printing gun head with the diameter of 1.2mm for filling, and setting and adjusting all shafts of the 3D printer X, Y, Z to be zero by a program;
designing a 3D model by using 3Dmax software, wherein the internal chocolate structure is in a heart shape, the middle of the external chocolate structure is in a heart-shaped hollowed-out square structure, namely the external structure is printed by using low-melting-point chocolate paste through a first printing pipe, the internal inlaid part is filled and printed by using high-melting-point chocolate paste through a second printing pipe, and generating corresponding 24 layers of three-dimensional slices through slicing software to obtain a slice model; calculating a path of each layer of slices by using a programming G code and finally inputting the path to the printing equipment;
various parameters in the printing process are set, and the method specifically comprises the following steps: the printing layer thickness is 1.1mm, the wall thickness is 1.2mm, the filling density is 50%, the bottom layer and the top layer thickness are 1.2mm, the printing speed is 80mm/s, the printing temperature is 30 ℃, the initial layer thickness is 1.2mm, the initial layer line width is 10%, the bottom layer cutting is 0mm, the moving speed is 60mm/s, the bottom layer speed is 60mm/s, the filling speed is 60mm/s, the bottom layer and the top layer speed is 60mm/s, the shell speed is 40mm/s, and the inner wall speed is 80 mm/s;
the equipment performs double-channel 3D printing according to the introduced slice model to form a multilayer multi-structure black chocolate model constructed by two different melting point materials;
the chocolate model is placed under the conditions of stable environment, constant temperature and 35 ℃, the induction time is controlled to be 60s, and the spontaneous change of the structure of the chocolate on the inner layer and the chocolate on the outer layer is realized, namely the 4D printing effect.
The performance test of the 4D printing chocolate prepared from the W/O/W fat with different oil phase ratios is carried out, and the test result is as follows:
TABLE 1 Property parameters of W/O/W fat-based 4D printed chocolates prepared with different oil phase ratios
| Oil phase ratio | Hardness at 20 ℃ (N) | Hardness (N) at 37 ℃ | Initial melting temperature (. degree.C.) | Maximum melting temperature (. degree. C.) |
| 36％ | 429.1±23.1 | 12.5±0.4 | 30.6±4.4 | 35.4±1.5 |
| 45％ | 431.8±57.6 | 24.7±1.5 | 31.2±0.9 | 37.3±1.2 |
| 54％ | 497.5±69.4 | 26.9±2.1 | 32.7±2.3 | 37.6±2.6 |
| 63％ | 471.5±111.8 | 30.0±4.8 | 34.1±3.8 | 38.0±1.9 |
Note: the hardness of the chocolate is 20 ℃ under the normal temperature condition, and the hardness of the chocolate is 37 ℃ under the condition of simulating the oral temperature of a human body.
As can be seen from table 1: with the increase of the oil phase ratio, the higher the oil phase W/O/W fat, the higher the hardness of the prepared 4D printing chocolate system, and the higher the melting point of the 4D printing chocolate system. This suggests that the addition of liquid vegetable oils may make chocolate more stable under high temperature conditions, but the higher oil phase is difficult to stabilize on the one hand and may also affect its lack of chocolate properties.
Fig. 1 is a real object diagram printed in embodiment 2, and it can be seen from fig. 1 that: the surface of the chocolate is smoother when the oil phase is lower, and the surface property of the 4D printed chocolate is influenced to a certain extent by the added W/O/W lipid.
Figure 2 is a taiji graphic printed with fat-built low fat chocolate having an oil phase ratio of 54% and a school badge model of south of the river university. As can be seen from fig. 2: the surface is smooth, and the texture is clear.
As can be seen by combining table 1 and fig. 1 and 2: under the premise of ensuring that the 4D printing structure forming of the chocolate can be realized by utilizing the melting point difference, the chocolate has the maximum hardness at low temperature (20 ℃) when the oil phase ratio is 54%, and has smaller hardness at 37 ℃, but can also maintain the structural change during 4D printing, and is a preferred group in an oil phase ratio system.
EXAMPLE 3 optimization of alternative ratios
The oil phase ratio of the W/O/W lipid adopted in the steps (1) and (2) of the example 2 is adjusted to 54 percent;
while adjusting the ratio of the amounts of W/O/W type fat and cocoa butter used in step (1) in Table 2, the other steps were kept the same as in example 2, to obtain 4D printed chocolate.
The obtained 4D printed chocolate was subjected to a performance test, and the test results were as follows:
TABLE 2 Property parameters for 4D printed chocolates with different cocoa butter substitution ratios
| W/O/W lipid | Cocoa butter | Hardness (N) at 20 ℃ | Hardness (N) at 37 ℃ | Initial melting temperature (. degree.C.)) | Maximum melting temperature (. degree.C.) |
| 0 | 35 | 491.5±103.4 | 1.3±0.4 | 28.6±3.3 | 34.6±4.2 |
| 8.75 | 26.25 | 497.5±69.4 | 26.9±2.1 | 32.7±2.3 | 37.6±2.6 |
| 17.5 | 17.5 | 496.7±58.8 | 66.9±10.6 | 34.0±1.1 | 38.6±2.0 |
| 26.25 | 8.75 | 501.8±94.2 | 97.1±8.9 | 34.3±0.2 | 38.3±1.2 |
| 35 | 0 | 630.1±116.5 | 486.7±30.8 | 35.6±0.9 | 40.6±2.7 |
Note: the hardness of the chocolate is 20 ℃ under the normal temperature condition, and the hardness of the chocolate is 37 ℃ under the condition of simulating the oral temperature of a human body.
As can be seen from table 2: the higher the degree of substitution of cocoa butter by W/O/W fat, the higher the hardness at 20 ℃ and 37 ℃ and the higher the melting point, because the thermodynamic stability of W/O/W fat is such that it significantly increases the melting point and hardness after cocoa butter substitution.
Fig. 3 is a real object diagram printed in embodiment 3, and it can be seen from fig. 3 that: the degree of substitution of the W/O/W fat with cocoa butter has no significant effect on the surface properties of the paste and can form a self-supporting stable structure during printing.
FIG. 4 is a DSC thermodynamic analysis of different 3D printed chocolates constructed under conditions of different cocoa butter substitution ratios; as can be seen from fig. 4: with the increase of the substitution ratio of cocoa butter, the enthalpy change during heating gradually decreases and the endothermic peak shifts to the left because the total enthalpy change decreases due to the decrease of the content of cocoa butter having crystalline property inside, and the melting point increases due to the thermal stability of adding W/O/W, that is, the leftward shift of the endothermic peak occurs.
FIG. 5 is a printed mechanical diagram (A) and a rheological property change (B) at the cocoa butter substitution ratios of 0% and 100% in example 3. Fig. 5 (a) is a schematic diagram of chocolate mass during 3D printing from barrel, where the rheological properties are shown as solid in the barrel, fluid in the needle due to shear thinning, and solid in the carrier after resting on the carrier. Fig. 5 (B) is a graph simulating deformation of chocolate paste due to the influence of shear force during printing, and it can be seen that: the loss modulus of the chocolate mass is smaller than the storage modulus at lower shear stress (0-120s) and is represented as solid, while the loss modulus is larger than the storage modulus at increased shear stress (120-240s) and is represented as fluid, and finally the chocolate system is gradually recovered to the solid state after the shear stress is recovered to the lower condition. The chocolate paste is simulated to be firstly solid from the syringe, the shearing force is applied by pressurizing and extruding so that the chocolate paste becomes fluid to pass through the needle, then the chocolate paste is static after the object carrying plate, the applied shearing force is cancelled, and the chocolate paste returns to the solid state again.
Fig. 6 shows the surface roughness of printed chocolate under atomic force microscope observation. As can be seen from fig. 6: the larger the proportion of W/O/W-like fat added to the system, the greater the surface roughness, since the W/O/W-like fat system affects the surface crystallization properties of cocoa butter.
Example 4
The oil phase ratio of the W/O/W lipid adopted in the steps (1) and (2) of the example 2 is adjusted to 54 percent;
while the amounts of W/O/W fat and cocoa butter used in step (1) were adjusted to 0 and 35g, i.e., the substitution ratio in the first type (low melting point syrup) was 0%, and the amounts of W/O/W fat and cocoa butter used in step (2) were adjusted to 17.5 and 17.5g, i.e., the substitution ratio in the second type (high melting point syrup) was 50%, and otherwise the same as in example 2 was maintained, to obtain 4D printed chocolate.
The obtained 4D printed chocolate was subjected to a performance test, and the test results were as follows:
fig. 7 is a double-channel multilayer printing process in embodiment 4, which includes building a hollowed-out shell and an inner layer mosaic model from left to right in sequence, then respectively deriving a slice structure after combining the two models by adjusting slice parameters, and guiding the slice structure into a double-channel printer for structural printing, wherein an inner layer is chocolate with a high melting point of 50% cocoa butter substitution ratio, an outer layer is chocolate with a low melting point of 0% cocoa butter substitution ratio, and finally, an outer layer low melting point and inner layer high melting point mosaic structure is obtained.
Fig. 8 is a 4D print of chocolate, which is a spontaneous structural change in the low fat chocolate of example 4 with 0% cocoa butter substitution in the outer layer and 50% cocoa butter substitution in the inner layer, within 60s at 35 ℃. As can be seen from fig. 5: the outer layer has a melting point lower than that of the outer layer and is substantially completely melted in the environment of 35 ℃ for 60 seconds, and the inner layer has a melting point higher than that of the inner layer by replacing 50% of cocoa butter with W/O/W fat, so that the melting point of the inner layer is increased and the inner layer can be stably self-supporting in the environment of 35 ℃ for 60 seconds.
Example 5 selection of cocoa butter
Adjusting example 2 the cocoa butter adopted in steps (1) and (2) is replaced by kokum butter, illipe butter and mango kernel oil; the rest was kept the same as example 2, resulting in 4D printed chocolate.
The obtained 4D printed chocolate was subjected to a performance test, and the test results were as follows:
table 3 property parameters of 4D printed chocolate prepared with cocoa butter and different types of cocoa butter equivalents
| (cacao butter) | Hardness (N) at 20 ℃ | Hardness (N) at 37 ℃ | Initial melting temperature (. degree. C.) | Maximum melting temperature (. degree.C.) |
| Cocoa butter | 497.5±69.4 | 26.9±2.1 | 32.7±2.3 | 37.6±2.6 |
| Candlestand oil | 439.8±53.2 | 13.5±2.3 | 36.7±2.1 | 43.8±2.2 |
| Bingbingcao fat | 498.5±35.6 | 17.2±0.6 | 35.9±1.7 | 41.2±1.9 |
| Mango kernel oil | 416.7±23.5 | 14.6±1.8 | 33.4±0.8 | 37.5±3.1 |
Note: the hardness of the chocolate is 20 ℃ at normal temperature, and the hardness of the chocolate is 37 ℃ at simulated human mouth temperature.
As can be seen from table 3: cocoa butter equivalent has a hardness less than cocoa butter and a melting temperature comparable to cocoa butter.
Comparative example 1
The ball mill grinding in example 2 was replaced with a blade blender 1200r/min for 1h, otherwise identical to example 2, to provide a two pass printed chocolate.
The results are shown in fig. 9, and it can be seen from fig. 9 that: the resulting chocolate model had a significantly rough surface and an unclear texture as compared to example 2, which still had a large number of coarse particles in the chocolate mass obtained by blade stirring due to lack of grinding by the ball mill, which aggregated crystals on the surface to make the surface rough and lack the texture.
Comparative example 2
The temperature in the printing chamber in step (3) in example 2 was kept at 35 ℃, otherwise in agreement with example 2, to give a 4D printed chocolate.
The results are shown in fig. 10, and it can be seen from fig. 10 that: the chocolate model structure has a certain degree of collapse, and the chocolate rheological property can be changed and the fluidity is enhanced by printing in the environment of 35 ℃, so that the structure is unstable in the printing process, and a compact self-supporting structure cannot be formed.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (10)
1. A method for realizing multi-structure low-fat chocolate two-channel 4D printing by inducing deformation is characterized by comprising the following steps:
(1) preparation of chocolate paste of the first type
Mixing W/O/W fat and cocoa butter, cocoa butter equivalent or cocoa butter substitute according to the mass ratio of 1: (1.1-10), and uniformly mixing; then adding auxiliary materials, and grinding to obtain a first type of slurry system;
(2) preparation of chocolate mass of the second type
Mixing W/O/W fat-like and cocoa butter, cocoa butter-like or cocoa butter substitute according to the mass ratio of 1: (0.1-1), and uniformly mixing; then adding auxiliary materials, and grinding to obtain a second type slurry system;
(3)4D printing:
filling the first type of chocolate paste into one printing tube, filling the second type of chocolate paste into the other printing tube, and performing double-channel printing to obtain a chocolate model; the chocolate model is placed in an environment with the temperature of 30-36 ℃ for thermal induction deformation for 30-120 s, so that the outer layer of chocolate is melted, and 4D printing is realized.
2. The method according to claim 1, wherein the preparation method of the W/O/W-like fat comprises the following steps:
preparing a protein isolate solution with the mass concentration of 5-20%, and hydrating to obtain a hydrated protein isolate solution; wherein the protein isolate comprises one or more of peanut, pea, mung bean and soybean protein isolate;
secondly, shearing the hydrated protein isolate solution obtained in the first step at a high speed, and homogenizing at a high pressure to obtain a nano-scale protein isolate dispersion liquid;
thirdly, heating the nanoscale protein isolate dispersion liquid obtained in the second step to obtain modified protein isolate dispersion liquid;
fourthly, adding transglutaminase TGase into the separated protein dispersion liquid obtained in the third step for reaction to obtain separated protein glue;
fifthly, adding diluent into the separated protein gel obtained in the step IV, and carrying out micro-jet and high-pressure homogenization to obtain a nano microgel solution;
sixthly, adding the nano gel dispersion liquid after the gelation treatment obtained in the fifth step into liquid edible vegetable oil, and performing high-speed shearing treatment to obtain W/O system emulsion, wherein the liquid edible vegetable oil is a continuous phase, and the nano gel dispersion liquid after the gelation treatment is a dispersed phase;
seventhly, using the whole W/O emulsion obtained in the step (c) as a dispersed phase, using the gelatinized nano microgel dispersion liquid obtained in the step (c) as a continuous phase, and performing secondary emulsification and high-speed shearing treatment to obtain the double-emulsified W/O/W fat.
3. The method according to claim 1, wherein the first type of chocolate mass in step (1) is a low melting point chocolate mass, the melting point being in the range of 26-32 ℃.
4. The method according to claim 1, wherein the second type of chocolate mass in step (2) is a high melting point chocolate mass having a melting point in the range of 33 to 38 ℃.
5. The method according to claim 1, wherein the auxiliary materials in step (1) comprise cocoa/milk powder, powdered sugar, soybean lecithin; the mass ratio of cocoa butter, cocoa butter equivalent or cocoa butter substitute and cocoa powder/milk powder, powdered sugar and soybean lecithin in the first chocolate paste is 1: 0.05-0.2: 0.1-0.5: 0.001 to 0.01.
6. The method according to claim 1, wherein the auxiliary materials in step (2) comprise cocoa powder, powdered sugar, soybean lecithin; the mass ratio of cocoa butter, cocoa butter equivalent or cocoa butter substitute to cocoa powder, sugar powder and soybean lecithin in the second chocolate mass is 1: 0.4-2: 0.5-3: 0.001 to 0.1.
7. The method according to claim 1, wherein the cocoa butter equivalents in steps (2) and (1) comprise one or more of shea butter, sal fat, mango kernel oil, kokum oil, palm oil medium melting point fraction, illipe butter; the cocoa butter substitute comprises one or two of lauric acid type cocoa butter substitute and non-lauric acid type cocoa butter substitute.
8. The method according to claim 2, wherein the volume ratio of the dispersed phase to the continuous phase in step (c) is 40-70: 30, the vegetable oil accounts for 70-90% of the nanogel dispersion liquid obtained in the fifth step by mass percent.
9. The method of claim 1, wherein the temperature of the printing chamber in dual pass printing is between 0 ℃ and 40 ℃.
10. A 4D printed chocolate produced by the method of any one of claims 1 to 9.
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| CN116686893A (en) * | 2023-05-31 | 2023-09-05 | 江南大学 | Method for preparing water-containing chocolate based on natural wax |
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| CN111543664A (en) * | 2020-04-21 | 2020-08-18 | 江南大学 | Method for realizing 4D printing art cold plate by utilizing microwave-induced spontaneous deformation |
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2022
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| US20200170279A1 (en) * | 2017-08-21 | 2020-06-04 | Institute of Food Science and Technology, Chinese Academy of Agricultural Sciences | Pickering emulsion prepared using peanut protein isolate and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023040374A1 (en) * | 2021-09-15 | 2023-03-23 | 江南大学 | Vegetable protein-based fat, and preparation therefor and use thereof in 3d/4d printing |
| CN116686893A (en) * | 2023-05-31 | 2023-09-05 | 江南大学 | Method for preparing water-containing chocolate based on natural wax |
| CN116686893B (en) * | 2023-05-31 | 2024-03-22 | 江南大学 | Method for preparing water-containing chocolate based on natural wax |
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