Toulten flavored concentrate as well as preparation method and application thereof

Abstract

The preparation method comprises the following steps: putting tallow into a reactor, heating to 330-370 DEG C in a low-oxygen environment, keeping for 80-140 minutes, carrying out thermal cracking reaction, controlling the heating voltage to be 150V and the stirring speed to be 300r / min during the period, condensing gas generated in the reaction process, and collecting thermal cracking liquid fraction, so as to obtain the tallow-flavor concentrate. And cooling after the reaction is completed, and carrying out purification treatment to obtain the tallow-flavor concentrate. According to the method, key parameters (including the reaction temperature, the pressure condition, the heating rate and the retention time) of the thermal cracking reaction are accurately regulated and controlled, so that the yield of the organic liquid product is remarkably improved, the composition of the components is optimized, and the production efficiency is high. According to the process improvement, the selectivity of the target product is improved, and a quality foundation is laid for subsequent application.

Description

Technical Field

[0001] The invention belongs to the technical field of food processing, and particularly relates to a beef tallow flavor concentrate and a preparation method and application thereof. Background Art

[0002] Hot pot is a popular dining experience in the restaurant industry, particularly in China. Beef tallow, a core ingredient in hot pot base, is a defining element of hot pot flavor in the Sichuan and Chongqing regions due to its unique aroma and taste.

[0003] Currently, thermal cracking technology is being applied in the oil conversion field. It can crack animal fats such as beef tallow under high-temperature, oxygen-free conditions to produce organic liquid products with distinctive flavor characteristics. By controlling parameters such as temperature, pressure, and residence time, this technology can produce products with different compositions, providing a feasible solution for extracting beef tallow flavor compounds.

[0004] However, existing pyrolysis technology produces low concentrations of beef tallow flavoring compounds, requiring large amounts to be added to achieve the desired flavor effect. This not only fails to address the inherent high saturated fatty acid and cholesterol content of beef tallow, but also exacerbates carbon emissions from livestock farming due to high demand, contradicting both healthy eating and environmental concerns. Furthermore, pyrolysis processes still face technical bottlenecks in product purification and large-scale production, further limiting their practical application. Summary of the Invention

[0005] To address the shortcomings of the prior art, the present invention provides a beef tallow flavor concentrate, its preparation method, and its application. This invention utilizes an optimized thermal cracking process to produce a high-purity flavor concentrate. This addresses the problem of low beef tallow flavor concentrations in existing methods, which necessitates the addition of large amounts of tallow flavoring to achieve the desired flavor effect in practical applications.

[0006] To achieve the above object, the technical solution adopted by the present invention is as follows:

[0007] In one aspect, the present invention provides a method for preparing a beef fat flavor concentrate by thermal cracking, comprising the following steps:

[0008] Beef tallow is placed in a reactor and heated to 330-370°C in a low-oxygen environment for 80-140 minutes for thermal cracking reaction. During this period, the heating voltage is controlled at 150V and the stirring speed is 300r / min. The gas generated during the reaction is condensed and the thermal cracking liquid fraction is collected until no gas is released. After the reaction is completed, it is cooled and purified to obtain beef tallow flavor concentrate.

[0009] In the present invention, the reactor is a batch tubular reactor.

[0010] As a further aspect of the present invention: The treatment method for the low-oxygen environment is as follows: The reactor is flushed with ultra-high purity nitrogen to remove the air in the reactor.

[0011] Specifically, the ultra-high purity nitrogen is nitrogen with a purity higher than 99.999%.

[0012] As a further aspect of the present invention: The purification treatment method is the distillation method.

[0013] Specifically, simple distillation is as follows: The light fraction is <100 °C (atmospheric pressure), and the target products such as short-chain hydrocarbons and acrolein are collected; the medium fraction: 100 - 200 °C (under reduced pressure), and the target products such as low-carbon carboxylic acids and esters are collected; the heavy fraction is >200 °C (requiring reduced pressure), and the target products such as macromolecular alkanes, alkenes, and fatty acids are collected.

[0014] On the other hand, the present invention provides a beef tallow flavor concentrate, which is prepared by the above-mentioned thermal cracking preparation method of the beef tallow flavor concentrate.

[0015] In the third aspect of the present invention, there is also provided a beef tallow flavor concentrate prepared by the above-mentioned thermal cracking preparation method of the beef tallow flavor concentrate, or the application of the above beef tallow flavor concentrate in food.

[0016] The positive and progressive effects of the present invention are as follows:

[0017] 1. By precisely controlling the key parameters of the thermal cracking reaction (including reaction temperature, pressure conditions, heating rate, and residence time), the present invention significantly improves the yield of the organic liquid product and optimizes its component composition. This process improvement enhances the selectivity of the target product and lays a quality foundation for subsequent applications.

[0018] 2. Through the optimized thermal cracking process, the present invention can prepare a high-purity flavor concentrate as the basic raw material for food flavorings. This product has a unique aroma and can be used in foods such as hot pot seasonings and meat products to enhance the characteristic flavor. At the same time, it can significantly reduce the intake of oil and greatly increase the added value of the product.

[0019] 3. The thermal cracking technology of the present invention is specifically strengthened for large-scale oil treatment. By improving the reaction efficiency and optimizing the energy consumption, it effectively breaks through the bottlenecks of the existing technology in terms of economy and production capacity. This innovation not only reduces the unit production cost but also improves the feasibility of industrial transformation, providing a practical technical path for the high-value utilization of oil resources.

[0020] 4. The pyrolysis process adopted by the present invention is carried out under anaerobic conditions at high temperature, which not only avoids potential safety hazards caused by the participation of oxygen, but also reduces the generation of harmful substances, having better environmental protection performance. This advantage improves the safety and environmental protection of the pyrolysis process compared with the prior art, meeting the requirements of modern industry for green and sustainable development. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 It is the infrared spectrogram of the pyrolysis liquid fraction in Example 3 of the present invention;

[0022] Figure 2 It is the GC-MS spectrograms of the pyrolysis liquid fractions of the thermal pyrolysis in Examples 1-6 of the present invention. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0023] The present invention will be specifically described below in conjunction with the embodiments. The technical solutions of the present invention are clearly and completely described to facilitate the understanding of those skilled in the art. The described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative work fall within the scope of protection of the present invention. At the same time, for the raw materials not detailedly described below, they are all commercially available products; the process steps or preparation methods not detailedly mentioned are all process steps or preparation methods known to those skilled in the art.

[0024] Example 1

[0025] A method for preparing a beef tallow flavor concentrate, comprising the following steps:

[0026] (1) Place 200 g of beef tallow in a reactor, and rinse the reactor three times with ultra-high purity nitrogen with a purity higher than 99.999% to remove the air in the reactor and ensure that the reaction proceeds in a low-oxygen environment.

[0027] (2) Set the experimental parameters. Set the final temperature to 330 °C, the residence time to 100 min, the heating voltage to 150 V, and the stirring speed to 300 r / min.

[0028] (3) Start heating. Start the heating power supply, raise the temperature in the reactor to the reaction temperature, and maintain it for the required duration of the reaction at this temperature.

[0029] (4) Thermal pyrolysis reaction. During the heating process, the beef tallow in the reactor will undergo a thermal pyrolysis reaction to produce gas and liquid products. The generated gas flows out through the top outlet of the reactor and is then condensed and collected through a condenser collection system. The liquid fraction of the condenser (i.e., the thermal pyrolysis liquid fraction) is collected in a conical flask provided on the condenser.

[0030] (5) End the reaction. When no further significant gas evolution is observed, it indicates that the reaction has ended. At this time, cool the reactor to room temperature, open the reactor, and take out the remaining solid product.

[0031] (6) Purify the pyrolysis product. Take out the pyrolysis liquid fraction in the conical flask and conduct further distillation and purification to obtain a high-purity tallow flavor concentrate.

[0032] Example 2

[0033] A method for preparing a tallow flavor concentrate, comprising the following steps:

[0034] (1) Place 200 g of tallow in a reactor and flush the reactor three times with ultra-high-purity nitrogen with a purity higher than 99.999% to remove the air in the reactor and ensure that the reaction proceeds in a low-oxygen environment.

[0035] (2) Set the experimental parameters. Set the final temperature to 350 °C, the residence time to 100 min, the heating voltage to 150 V, and the stirring speed to 300 r / min.

[0036] (3) Start heating. Start the heating power supply, raise the temperature in the reactor to the reaction temperature, and maintain it for the duration required for the reaction at this temperature.

[0037] (4) Pyrolysis reaction. During the heating process, the tallow in the reactor undergoes a pyrolysis reaction to produce gas and liquid products. The generated gas flows out through the top outlet of the reactor and is then condensed and collected through a condenser collection system. The liquid fraction of the condenser (i.e., the pyrolysis liquid fraction) is collected in a conical flask set on the condenser.

[0038] (5) End the reaction. When no further significant gas evolution is observed, it indicates that the reaction has ended. At this time, cool the reactor to room temperature, open the reactor, and take out the remaining solid product.

[0039] (6) Purify the pyrolysis product. Take out the pyrolysis liquid fraction in the conical flask and conduct further distillation and purification to obtain a high-purity tallow flavor concentrate.

[0040] Example 3

[0041] A method for preparing a tallow flavor concentrate, comprising the following steps:

[0042] (1) Place 200 g of tallow in a reactor and flush the reactor three times with ultra-high-purity nitrogen with a purity higher than 99.999% to remove the air in the reactor and ensure that the reaction proceeds in a low-oxygen environment.

[0043] (2) Set the experimental parameters. Set the final temperature to 370 °C, the residence time to 100 min, the heating voltage to 150 V, and the stirring speed to 300 r / min.

[0044] (3) Start heating. Start the heating power supply, raise the temperature in the reactor to the reaction temperature, and maintain it at this temperature for the required reaction duration.

[0045] (4) Pyrolysis reaction. During the heating process, the beef tallow in the reactor will undergo a pyrolysis reaction, generating gas and liquid products. The generated gas flows out through the top outlet of the reactor and is then condensed and collected through the condenser collection system. The liquid fraction of the condenser (i.e., the pyrolysis liquid fraction) is collected in a conical flask set on the condenser.

[0046] (5) End the reaction. When no further significant gas release is observed, it indicates that the reaction has ended. At this time, cool the reactor to room temperature, open the reactor, and take out the remaining solid product.

[0047] (6) Purify the pyrolysis product. Take out the pyrolysis liquid fraction in the conical flask and perform further distillation and purification to obtain a high-purity beef tallow flavor concentrate.

[0048] Example 4

[0049] A method for preparing a beef tallow flavor concentrate, comprising the following steps:

[0050] (1) Place 200 g of beef tallow in the reactor and flush the reactor three times with ultra-high purity nitrogen with a purity higher than 99.999% to remove the air in the reactor and ensure that the reaction proceeds in a low-oxygen environment.

[0051] (2) Set the experimental parameters. Set the final temperature to 350 °C, the residence time to 80 min, the heating voltage to 150 V, and the stirring speed to 300 r / min.

[0052] (3) Start heating. Start the heating power supply, raise the temperature in the reactor to the reaction temperature, and maintain it at this temperature for the required reaction duration.

[0053] (4) Pyrolysis reaction. During the heating process, the beef tallow in the reactor will undergo a pyrolysis reaction, generating gas and liquid products. The generated gas flows out through the top outlet of the reactor and is then condensed and collected through the condenser collection system. The liquid fraction of the condenser (i.e., the pyrolysis liquid fraction) is collected in a conical flask set on the condenser.

[0054] (5) End the reaction. When no further significant gas release is observed, it indicates that the reaction has ended. At this time, cool the reactor to room temperature, open the reactor, and take out the remaining solid product.

[0055] (6) Purify the pyrolysis product. Take out the pyrolysis liquid fraction in the conical flask and conduct further distillation and purification treatment to obtain a high-purity beef tallow flavor concentrate.

[0056] Example 5

[0057] A method for preparing a beef tallow flavor concentrate, comprising the following steps:

[0058] (1) Place 200 g of beef tallow in a reactor and flush the reactor three times with ultra-high-purity nitrogen with a purity higher than 99.999% to remove the air in the reactor and ensure that the reaction proceeds in a low-oxygen environment.

[0059] (2) Set the experimental parameters. Set the final temperature to 350 °C, the residence time to 120 min, the heating voltage to 150 V, and the stirring speed to 300 r / min.

[0060] (3) Start heating. Start the heating power supply, raise the temperature in the reactor to the reaction temperature, and maintain it for the duration required for the reaction at this temperature.

[0061] (4) Pyrolysis reaction. During the heating process, the beef tallow in the reactor will undergo a pyrolysis reaction to produce gas and liquid products. The generated gas flows out through the top outlet of the reactor and is then condensed and collected through a condenser collection system. The liquid fraction of the condenser (i.e., the pyrolysis liquid fraction) is collected in a conical flask set on the condenser.

[0062] (5) End the reaction. When no further significant gas release is observed, it indicates that the reaction has ended. At this time, cool the reactor to room temperature, open the reactor, and take out the remaining solid product.

[0063] (6) Purify the pyrolysis product. Take out the pyrolysis liquid fraction in the conical flask and conduct further distillation and purification treatment to obtain a high-purity beef tallow flavor concentrate.

[0064] Example 6

[0065] A method for preparing a beef tallow flavor concentrate, comprising the following steps:

[0066] (1) Place 200 g of beef tallow in a reactor and flush the reactor three times with ultra-high-purity nitrogen with a purity higher than 99.999% to remove the air in the reactor and ensure that the reaction proceeds in a low-oxygen environment.

[0067] (2) Set the experimental parameters. Set the final temperature to 350 °C, the residence time to 140 min, the heating voltage to 150 V, and the stirring speed to 300 r / min.

[0068] (3) Start heating. Turn on the heating power supply, raise the temperature inside the reactor to the reaction temperature, and maintain it for the duration required for the reaction.

[0069] (4) Pyrolysis reaction. During the heating process, the beef tallow inside the reactor will undergo a pyrolysis reaction, generating gas and liquid products. The generated gas flows out through the outlet at the top of the reactor and is then condensed and collected through the condenser collection system. The liquid fraction of the condenser (i.e., the pyrolysis liquid fraction) is collected in a conical flask set on the condenser.

[0070] (5) End the reaction. When no further significant gas release is observed, it indicates that the reaction has ended. At this time, cool the reactor to room temperature, open the reactor, and take out the remaining solid product.

[0071] (6) Purify the pyrolysis product. Take out the pyrolysis liquid fraction in the conical flask and conduct further distillation and purification treatment to obtain a high-purity beef tallow flavor concentrate.

[0072] Comparative Example 1

[0073] The difference from Example 3 is that the reaction temperature is 390 °C.

[0074] Comparative Example 2

[0075] The difference from Example 3 is that the reaction temperature is 320 °C. At this temperature, the pyrolysis reaction rarely occurs. At the same time, due to equipment limitations, when the reaction temperature is low, the heat in the pyrolyzer is not sufficient to push the pyrolysis components generated by the reaction to the condenser, and no liquid fraction can be condensed.

[0076] Comparative Example 3

[0077] The difference from Example 3 is that the residence time is 60 min.

[0078] Comparative Example 4

[0079] The difference from Example 3 is that the heating voltage is 100 V.

[0080]

Product Performance Test

[0081] Conduct an application performance test on the products prepared in the examples and comparative examples. The test method is as follows:

[0082] I. Yield: The liquid fraction in the condenser (i.e., the pyrolysis liquid fraction) is collected in a pre-weighed conical flask installed on the condenser, and then weighed, which is the yield.

[0083] II. Yield rate: Calculate through the following formula

[0084] Yield rate = pyrolysis liquid / total amount of initial raw materials × 100%

[0085] The test data of the pyrolysis liquid fractions prepared in the above examples and comparative examples are shown in Table 1.

[0086] Table 1

[0087] Sample Output (g) Yield (%) Example 1 78 39 Example 2 94 47.25 Example 3 105 52.75 Example 4 80 40 Example 5 90 45 Example 6 90 45 Comparative Example 1 52 26 Comparative Example 2 0 0 Comparative Example 3 60 30 Comparative Example 4 80 40

[0088] By precisely regulating the key parameters of the thermal pyrolysis reaction, including reaction temperature, pressure conditions, heating rate, and residence time, the present invention significantly improves the yield of organic liquid products and has high production efficiency.

[0089] In Comparative Example 1, the reaction temperature was 390 °C. At this temperature, the triglyceride component in beef tallow was also vaporized and condensed into the liquid fraction together with the pyrolysis components, resulting in raw material loss. At the same time, the triglyceride in beef tallow became solid after condensation, causing blockage of the condensation pipeline, a significant reduction in yield, and large raw material loss.

[0090] In Comparative Example 2, when the reaction temperature was 320 °C, the pyrolysis reaction rarely occurred and was not sufficient to produce fractions.

[0091] In Comparative Example 3, the reaction temperature was 370 °C and the reaction time was 60 min, with a low yield.

[0092] In Comparative Example 4, the low heating voltage led to a long heating-up time, which was up to twice as long as the time from the start of heating to the set reaction temperature, resulting in too low production efficiency.

[0093] Infrared spectrum analysis

[0094] According to the above experiments, in Example 3, when the final reaction temperature was 370 °C and the residence time was 100 min, it was the optimal condition for obtaining the pyrolysis liquid fraction with the maximum yield by thermal pyrolysis. The functional groups of the pyrolysis liquid fraction obtained under this condition were analyzed using a Thermo Nicolet Nexus 4700 infrared spectrometer in the United States. The KBr tablet pressing technique was used to prepare the FT-IR test sample with 2% oil sample. The scanning wavenumber of the infrared spectrum was in the range of 400 - 4000 cm -1 The resolution of the spectrometer was 0.1 cm -1 . Under the above conditions, attenuated total reflection (ATR) was used to identify the functional groups present in the thermal pyrolysis liquid fraction.

[0095] The obtained FTIR spectrum is as Figure 1 shown. The presented spectrum shows several absorption bands attributed to many functional groups. The O-H stretching vibration band between 3200 - 3600 cm -1 indicates the presence of carboxylic acids, alcohols, and water. Strong bands are present near 2920 cm -1 and 2850 cm -1 , and at 2960 cm -1and 2870 cm -1 There are two shoulders near -1 , which are due to the symmetric and asymmetric stretching of C-H in the CH2 and CH3 groups respectively. The high intensity of these bands indicates that saturated aliphatic hydrocarbons dominate in the pyrolysis liquid fraction. The presence of other aliphatics (the C-H bending vibration band at 1384 cm -1 and the asymmetric deformation of C-H between 1475 - 1430 cm -1 ) with moderate intensity confirms the aliphatic characteristics. In the frequency range of 1770 - 1700 cm -1 , there is a C=O stretching vibration band, indicating the presence of ketones, carboxylic acids, aldehydes or esters. The bands at 950 and 1300 cm -1 belong to the C-O stretching vibration, indicating the presence of alcohols or esters. Several signals appear in the range of 700 and 900 cm -1 , which are due to aromatic stretching vibrations, indicating the presence of aromatic compounds in the pyrolysis liquid fraction.

[0096] The FTIR results show the complexity of the chemical composition of the pyrolysis liquid fraction and the diversity of the organic compounds that make up this liquid fraction.

[0097] GC-MS analysis

[0098] For a detailed molecular characterization, the pyrolysis liquid fractions of Examples 1 - 6 were further analyzed by GC-MS. This GC-MS spectrum was obtained by performing gas chromatography - mass spectrometry (GC-MS) analysis of the chemical composition of the pyrolysis liquid fraction using an Agilent 7890A gas chromatograph equipped with an Agilent 5975 mass selective detector. The GC-MS chromatogram is as shown in Figure 2 . It can be seen from the chromatogram that the components produced under different reaction conditions have great similarities. The GC-MS analysis results show that these compounds are mainly: carboxylic acid compounds (acetic acid, heptanoic acid, octanoic acid, nonanoic acid, decanoic acid, etc.); alkanes (hexane, heptane, octane, nonane, decane, undecane, dodecane, tridecane, tetradecane, pentadecane, hexadecane, heptadecane, etc.); alkenes (hexene, heptene, octene, nonene, decene, undecene, 1-dodecene, 1-tridecene, 2-tetradecene, 1-pentadecene, 1-hexadecene, 8-heptadecene, etc.) and cycloalkanes (cyclopentene, cyclohexene, methylcyclohexane, 1-methyl-2-pentylcyclopropane, 1-butylcyclopentene, 1-propylcyclohexene, cyclopentadecane, nonylcyclohexane, etc.). A variety of other oxygen-containing compounds (aromatic compounds, phenols, ketones, aldehydes, alcohols, etc.) were also found. The contents of 1-pentadecene and pentadecane in the pyrolysis liquid fraction are relatively large, reaching up to 5.0995% and 15.0064% respectively. The high contents of these two components are due to the relatively high content of saturated palmitic acid, which is one of the main fatty components of beef tallow. Table 2 shows the fatty acid composition of beef tallow.

[0099] Table 2

[0100]

[0101]

[0102] The oxygen-containing compounds in the pyrolysis liquid have straight-chain short-chain fatty acids as the main products. Table 3 shows the specific compositions of the components in the pyrolysis liquid fractions of Examples 1 to 6.

[0103] Table 4 shows the yields of the target components in the pyrolysis liquid fractions. Except for Example 1 where ethyl acetate was not produced, ethyl acetate was produced in other examples. In addition, a small amount of 2-undecanone (0.4025%) was produced in Example 5, and a small amount of 2-decanone was produced in Example 6. These two components are key flavor compounds in natural tallow. In all examples, tridecane and pentadecane are the main reaction products. The pyrolysis liquid products are very complex. The components in Table 4 are the target components and also the key components in the flavor concentrate. The more components there are, the better the flavor effect.

[0104] Table 3

[0105]

[0106]

[0107]

[0108]

[0109] a All data are peak area percentages (%)

[0110] b Not detected

[0111] Table 4

[0112]

[0113]

[0114] a All data are peak area percentages (%)

[0115] b Not detected

[0116] As can be seen from the above table, through the above steps, the present application can realize the method of preparing flavor concentrate by thermal pyrolysis of tallow, thereby solving the problems of precisely controlling parameters such as reaction temperature, pressure, heating rate, and reaction residence time in the prior art, improving the yield and composition of organic liquid products, and the problems of recovering and purifying thermal pyrolysis products.

[0117] The above are only the preferred embodiments of the present invention, and do not impose any formal or substantial limitations on the present invention. It should be noted that for those of ordinary skill in the art of this technology, without departing from the premise of the present invention, several improvements and supplements can still be made, and these improvements and supplements should also be regarded as the protection scope of the present invention. Any equivalent changes in the form of minor modifications, decorations, and evolutions that can be made by those who are familiar with the technology in this field without departing from the spirit and scope of the present invention by using the technical content disclosed above are equivalent embodiments of the present invention; at the same time, any equivalent changes, modifications, and evolutions made to the above embodiments based on the essential technology of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A method for preparing a tallow flavor concentrate by thermal cracking, characterized in that, It includes the following steps: Put beef tallow in a reactor, heat it to 330 - 370 °C in a low-oxygen environment, and keep it for 80 - 140 min for thermal cracking reaction. During this period, control the heating voltage at 150 V and the stirring speed at 300 r / min. The gas generated during the reaction is condensed and the thermal cracking liquid fraction is collected until no gas is released. After the reaction is completed, cool it and obtain beef tallow flavor concentrate through purification treatment.

2. The method for preparing the thermal cracking of the tallow flavor concentrate according to claim 1, wherein The treatment method of the low-oxygen environment is: rinse the reactor with ultra-high purity nitrogen to remove the air in the reactor.

3. The method for preparing the tallow flavor concentrate by thermal cracking according to claim 1, characterized in that, The purification treatment method is the distillation method.

4. A tallow flavor concentrate, characterized in that, It is prepared by the thermal cracking preparation method of beef tallow flavor concentrate as described in claims 1 - 3.

5. A beef tallow flavor concentrate prepared by the thermal cracking preparation method of beef tallow flavor concentrate as described in claims 1 - 3, or the application of the beef tallow flavor concentrate as described in claim 4 in food.

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