Process and device for producing β-carotene with controllable color

Abstract

The present invention provides a production process and a production device for color-controllable β-carotene, which relates to the technical field of β-carotene production. In this color-controllable β-carotene production process, the crude β-carotene is dissolved using a heated solvent, and the dissolved crude β-carotene solution is sprayed and flash-crystallized under a pressure of -0.097 MPa to -0.03 MPa to obtain β-carotene products of different colors. The production process for color-controllable β-carotene provided by the present invention first heats the solvent, then redissolves the β-carotene, and then realizes the recrystallization of β-carotene through a flash evaporation process, establishing a quantitative relationship between the operating parameters and the product color, making the color of the obtained β-carotene product controllable and meeting the needs of different usage scenarios of customers. This process is continuous, highly controllable, has high processing efficiency, and the solvent is recycled, reducing the operating cost.

Description

Technical Field

[0001] The present invention relates to the technical field of β-carotene production, and in particular to a production process and a production device for β-carotene with controllable color. Background Art

[0002] β-carotene is an important edible natural pigment and is one of the carotenoids, with its molecular formula being C 40 H 56 . β-carotene exists in abundance in many natural foods, such as green vegetables, sweet potatoes, carrots, papayas, mangoes, etc. β-carotene can be obtained through organic synthesis, but due to different crystallization conditions and crystallization rates, its cis-trans isomers, crystal particle sizes, etc. are different, and thus different colors are presented through diffuse reflection, etc.

[0003] β-carotene is an important food additive, and color is its main physical and chemical property. Among them, the conjugated double bonds existing in the molecular structure of β-carotene are the main reasons for its chromogenesis. During the formulation process, various process conditions will change to varying degrees, affecting the cis-trans isomer composition, the formation of new functional groups, and the particle size distribution, etc., thus affecting the color of β-carotene. Currently, the colors at different stages during the formulation process of β-carotene products can be directly detected by a color difference meter.

[0004] However, in the current production process of β-carotene crystallization, the following deficiencies exist:

[0005] 1. The means for controlling the color of β-carotene products generally rely on the experience of technicians, and there is no quantitative relationship established between the operating parameters and the product color, and effective suggestions cannot be provided for process operations;

[0006] 2. The crystallization process is an intermittent operation, and the production efficiency is low.

[0007] In view of this, the present invention is specifically proposed. Summary of the Invention

[0008] The first object of the present invention is to provide a production process for β-carotene with controllable color, aiming to solve the technical problem that in the prior art, there is no quantitative relationship established between the operating parameters and the product color, and effective suggestions cannot be provided for process operations.

[0009] The second object of the present invention is to provide a production device for β-carotene with controllable color, aiming to solve the technical problem that in the prior art, the crystallization process cannot be carried out continuously and the production efficiency is low.

[0010] To solve the above technical problems, the present invention specifically adopts the following technical solutions:

[0011] The first aspect of the present invention provides a production process for color - controllable β - carotene. The crude β - carotene is dissolved using a heated solvent, and the dissolved crude β - carotene solution is spray - flash - crystallized at - 0.097 MPa to - 0.03 MPa to obtain β - carotene products of different colors with a particle size distribution conforming to a normal distribution.

[0012] Furthermore, the colors of the β - carotene include bright red, red, red - purple, and purple - black.

[0013] The particle size D50 of the bright red β - carotene is 1.48 μm - 1.83 μm; in the Lab color model: the L value is 35.42 - 39.42, the a value is 43.34 - 45.62, and the b value is 30.2 - 36.5.

[0014] The particle size D50 of the red β - carotene is 1.95 μm - 2.23 μm; in the Lab color model: the L value is 34.9 - 35.2, the a value is 39.56 - 42.05, and the b value is 26.88 - 29.25.

[0015] The particle size D50 of the red - purple β - carotene is 2.30 μm - 4.32 μm; in the Lab color model: the L value is 32.53 - 34.36, the a value is 35.34 - 37.34, and the b value is 15.6 - 23.22.

[0016] The particle size D50 of the purple - black β - carotene is 5.72 μm - 6.27 μm; in the Lab color model: the L value is 31.32 - 32.53, the a value is 19.89 - 23.25, and the b value is 8.78 - 9.78.

[0017] Furthermore, the dissolved crude β - carotene solution is pressurized by a high - pressure spray pump and then enters a high - pressure nozzle.

[0018] Preferably, the color of the β - carotene is bright red, and the aperture of the high - pressure nozzle is 0.1 mm - 0.5 mm.

[0019] Preferably, the color of the β - carotene is red, and the aperture of the high - pressure nozzle is 0.5 mm - 0.7 mm.

[0020] Preferably, the color of the β - carotene is red - purple, and the aperture of the high - pressure nozzle is 0.5 mm - 0.8 mm.

[0021] Preferably, the color of the β - carotene is purple - black, and the aperture of the high - pressure nozzle is 1.0 mm - 1.2 mm.

[0022] The second aspect of the present invention provides a production device for the production process described in the first aspect, including a heating kettle, a dissolving kettle, a flash tank, a condenser, and a recovery tank that are connected in sequence;

[0023] The recovery tank is used to collect the solvent condensed by the condenser.

[0024] Furthermore, a high-pressure nozzle is arranged inside the flash tank for atomizing and spraying the liquid in the dissolving kettle for recrystallization.

[0025] Furthermore, a spray pump is also included, which is arranged between the dissolving kettle and the flash tank and is used to increase the pressure of the liquid in the dissolving kettle and then send it into the high-pressure nozzle arranged in the flash tank.

[0026] Furthermore, the upper parts of the heating kettle and the dissolving kettle are each independently provided with a feed inlet, an air inlet and an exhaust outlet, and the lower parts of the heating kettle and the dissolving kettle are each independently provided with a discharge outlet.

[0027] The heating kettle and the dissolving kettle are each independently provided with a jacket outside, and a heating medium is passed through the jacket for heating the kettle body.

[0028] Furthermore, the discharge outlet of the heating kettle is communicated with the feed inlet of the dissolving kettle;

[0029] The discharge outlet of the dissolving kettle is communicated with the feed inlet of the flash tank.

[0030] Compared with the prior art, the present invention has at least the following beneficial effects:

[0031] The production process of color-controllable β-carotene provided by the present invention first heats the solvent, then redissolves β-carotene, and then realizes the recrystallization of β-carotene through the flash evaporation process, establishing a quantitative relationship between the operating parameters and the product color, making the color of the obtained β-carotene product controllable and meeting the requirements of different usage scenarios of customers. This process is continuous, highly controllable, has high processing efficiency, the solvent is recycled, and the operating cost is reduced.

[0032] The color-controllable β-carotene production device provided by the present invention, according to the characteristics of β-carotene crystallization, by arranging a heating kettle, a dissolving kettle, a flash tank, a condenser and a recovery tank that are connected in sequence, enables the β-carotene crystals to meet the requirements. The device is also provided with a recovery tank for recycling the solvent used in the process, enabling the solvent to be recycled and reducing the production cost. Heating, dissolving, flash evaporation, condensation and recovery are each carried out in separate equipment, without affecting each other, with a high degree of controllability, continuous operation, and improved production efficiency. Description of the Drawings

[0033] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the following will briefly introduce the drawings required for the description of the specific embodiments or the prior art. Obviously, the drawings in the following description are some embodiments of the present invention. For those of ordinary skill in the art, without creative efforts, other drawings can also be obtained based on these drawings.

[0034] Figure 1 It is a schematic structural diagram of a production device for color - controllable β - carotene provided by the present invention;

[0035] Figure 2 It is a schematic structural diagram of another production device for color - controllable β - carotene provided by the present invention;

[0036] Figure 3 It is a schematic structural diagram of the production device for color - controllable β - carotene provided in Example 1.

[0037] Icon: 10 - heating kettle; 11 - first feed inlet; 12 - first air inlet; 13 - first exhaust outlet; 14 - first discharge outlet; 15 - first jacket; 16 - first hot water outlet; 17 - first low - pressure steam inlet; 19 - hot water inlet; 20 - dissolution kettle; 21 - second feed inlet; 22 - second low - pressure steam inlet; 23 - second hot water outlet; 24 - second air inlet; 25 - second exhaust outlet; 26 - third feed inlet; 27 - second jacket; 28 - second discharge outlet; 30 - flash tank; 31 - high - pressure nozzle; 32 - product outlet; 33 - solvent outlet; 34 - solvent inlet; 40 - condenser; 41 - low - temperature cooling water inlet; 42 - low - temperature cooling water outlet; 43 - gas - phase inlet; 44 - liquid - phase outlet; 50 - recovery tank; 51 - vacuum tube; 60 - spray pump. Specific Embodiments

[0038] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are some, but not all, of the embodiments of the present invention. Usually, the components of the embodiments of the present invention described and illustrated in the drawings here can be arranged and designed in various different configurations.

[0039] Therefore, the following detailed description of the embodiments of the present invention provided in the drawings is not intended to limit the scope of the claimed present invention, but merely represents the selected embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts belong to the scope of protection of the present invention.

[0040] It should be noted that like reference numerals and letters refer to like items in the following figures. Therefore, once an item is defined in one figure, it does not need to be further defined and explained in subsequent figures. The terms "first", "second", "third", etc. are only used for descriptive distinction and should not be construed as indicating or implying relative importance.

[0041] The first aspect of the present invention provides a production process of color-controllable β-carotene. The crude β-carotene is dissolved using a heated solvent, and the dissolved crude β-carotene solution is spray flash-crystallized at -0.097 MPa to -0.03 MPa to obtain β-carotene products of different colors.

[0042] The production process of color-controllable β-carotene provided by the present invention first heats the solvent, then redissolves β-carotene, and then realizes the recrystallization of β-carotene through a flash process, establishing a quantitative relationship between the operating parameters and the product color, making the obtained β-carotene products color-controllable and meeting the needs of different customer usage scenarios. This process is continuous, highly controllable, has high processing efficiency, and the solvent is recycled, reducing the operating cost.

[0043] Flash crystallization reduces the pressure of the hot crude β-carotene solution to below the saturation pressure at this temperature, then part of the solvent will boil and vaporize instantaneously when the pressure decreases, obtaining β-carotene crystals. The advantage of flash evaporation is to avoid the formation of scale on the heat transfer surface. Flash evaporation does not require heating, and the heat comes from the sensible heat released by itself. In some embodiments of the present invention, the pressure of flash crystallization is typically but not limited to -0.097 MPa, -0.08 MPa, -0.07 MPa, -0.06 MPa, -0.05 MPa, -0.04 MPa or -0.03 MPa.

[0044] The present invention does not specifically limit the solvent for dissolving β-carotene, and any solvent that can dissolve β-carotene can be used, typically but not limited to dichloromethane.

[0045] Furthermore, the colors of the β-carotene include bright red, red, red-violet and purple-black.

[0046] The particle size D50 of the bright red is 1.48 μm - 1.83 μm; in the Lab color model: the L value is 35.42 - 39.42, the a value is 43.34 - 45.62, and the b value is 30.2 - 36.5.

[0047] The particle size D50 of the red is 1.95 μm - 2.23 μm; in the Lab color model: the L value is 34.9 - 35.2, the a value is 39.56 - 42.05, and the b value is 26.88 - 29.25.

[0048] The particle size D50 of the red-violet color is 2.30 μm - 4.32 μm; in the Lab color model: the L value is 32.53 - 34.36, the a value is 35.34 - 37.34, and the b value is 15.6 - 23.22.

[0049] The particle size D50 of the purple-black color is 5.72 μm - 6.27 μm; in the Lab color model: the L value is 31.32 - 32.53, the a value is 19.89 - 23.25, and the b value is 8.78 - 9.78.

[0050] Furthermore, the crude β-carotene solution after dissolution is pressurized by a high-pressure spray pump and then enters a high-pressure nozzle.

[0051] Preferably, the color of the β-carotene is bright red, and the aperture of the high-pressure nozzle is 0.1 mm - 0.5 mm.

[0052] Preferably, the color of the β-carotene is red, and the aperture of the high-pressure nozzle is 0.5 mm - 0.7 mm.

[0053] Preferably, the color of the β-carotene is red-violet, and the aperture of the high-pressure nozzle is 0.5 mm - 0.8 mm.

[0054] Preferably, the color of the β-carotene is purple-black, and the aperture of the high-pressure nozzle is 1.0 mm - 1.2 mm.

[0055] Furthermore, the heating, the dissolution, and the flash crystallization are all carried out under the protection of an inert gas. This can prevent reactions with the components in the air, resulting in a decrease in the yield and quality of the target product.

[0056] Preferably, the temperature of the solvent after heating is 40°C to 120°C. Heating the solvent first and then mixing it with β-carotene can reduce the heating time of β-carotene and decrease the conversion of β-carotene from all-trans to cis. In some embodiments of the present invention, the temperature of the solvent after heating is typically but not limited to 40°C, 50°C, 60°C, 70°C, 80°C, 90°C, 100°C, 110°C, or 120°C. In some preferred embodiments of the present invention, the temperature of the solvent after heating is 80°C to 120°C, with better solubility and the ability to handle more crude β-carotene.

[0057] Preferably, the temperature for dissolving the crude β-carotene is 40°C to 120°C, the pressure for dissolving is 0 MPa to 1.0 MPa, and the time for dissolving is 8 min - 15 min. Corresponding to the temperature of the heated solvent, the temperature for dissolving the crude β-carotene is also 40°C to 120°C, and it can be carried out under normal pressure or pressurized conditions. The pressure for dissolving is typically but not limited to 0 MPa, 0.2 MPa, 0.4 MPa, 0.6 MPa, 0.8 MPa or 1.0 MPa.

[0058] It should be noted that in the present invention, unless otherwise specified, the pressure mentioned refers to gauge pressure.

[0059] Preferably, the mass ratio of the crude β-carotene to the solvent is 1:8 to 50; preferably 1:8 to 15. Typically but not restrictively, the mass ratio of the crude β-carotene to the solvent is, for example, 1:8, 1:10, 1:15, 1:20, 1:30, 1:40 or 1:50.

[0060] Furthermore, the spray pressure of the high-pressure spray pump is 1.0 MPa to 15.0 MPa, preferably 8.0 MPa to 12.0 MPa. In some embodiments of the present invention, the spray pressure of the high-pressure spray pump is typically but not limited to 1.0 MPa, 2.0 MPa, 3.0 MPa, 4.0 MPa, 5.0 MPa, 6.0 MPa, 7.0 MPa, 8.0 MPa, 9.0 MPa, 10.0 MPa, 11.0 MPa, 12.0 MPa, 13.0 MPa, 14.0 MPa or 15.0 MPa.

[0061] The second aspect of the present invention provides a device for producing β-carotene with controllable color, comprising a heating kettle, a dissolving kettle, a flash tank, a condenser and a recovery tank connected in sequence;

[0062] The recovery tank is used to collect the solvent condensed by the condenser.

[0063] The device for producing β-carotene with controllable color provided by the present invention, according to the characteristics of β-carotene crystallization, by setting a heating kettle, a dissolving kettle, a flash tank, a condenser and a recovery tank connected in sequence, enables the β-carotene crystals to meet the requirements. The device is also provided with a recovery tank for recovering the solvent used in the process, enabling the solvent to be recycled, reducing the production cost. Heating, dissolving, flashing, condensing and recovering, each process unit is carried out in a separate device, without mutual influence, with a high degree of controllability, continuous operation, and improved production efficiency.

[0064] Figure 1 It is a schematic structural diagram of a device for producing β-carotene with controllable color provided by the present invention. As Figure 1As shown in the figure, the production device of color-controllable β-carotene provided by the present invention comprises a heating kettle 10, a dissolving kettle 20, a flash tank 30, a condenser 40 and a recovery tank 50 which are connected in sequence. The flash tank 30 provides a space for the rapid gasification and gas-solid separation of the solvent in the β-carotene solution. When the β-carotene solution reaches the flash tank 30, the pressure suddenly drops, the solution becomes supersaturated, β-carotene recrystallizes and precipitates, and the solvent gasifies and separates from the β-carotene crystals. A high-pressure nozzle 31 is arranged inside the flash tank 30 to atomize the β-carotene solution by utilizing the pressure energy of the high-pressure solution. The specific structure of the high-pressure nozzle 31 is not limited in the present invention, and any nozzle structure that can achieve the atomization of the solution can be used. Typically but not limited to, it can be a fan-shaped atomizing nozzle, a conical atomizing nozzle or a spiral atomizing nozzle.

[0065] In some embodiments of the present invention, a spray pump 60 is arranged between the dissolving kettle 20 and the flash tank 30 for raising the pressure of the liquid in the dissolving kettle 20 and then feeding it into the high-pressure nozzle 31 arranged in the flash tank 30.

[0066] As Figure 2 shown in the figure, in some embodiments of the present invention, a first feed port 11, a first air inlet 12 and a first exhaust port 13 are arranged on the upper part of the heating kettle 10, and a first discharge port 14 is arranged on the lower part of the heating kettle 10.

[0067] A second feed port 21, a second air inlet 24 and a second exhaust port 25 are arranged on the upper part of the dissolving kettle 20, and a second discharge port 28 is arranged on the lower part of the dissolving kettle 20. The second feed port 21 is used for feeding the crude β-carotene.

[0068] The first discharge port 14 of the heating kettle 10 is communicated with the third feed port 26 of the dissolving kettle; for feeding the heated solvent into the dissolving kettle.

[0069] The heating kettle 10 and the dissolving kettle 20 are respectively and independently provided with a first jacket 15 and a second jacket 27 outside. A heating medium is passed through the first jacket 15 for heating the kettle body. In some embodiments of the present invention, low-pressure steam is passed through the first jacket 15 and / or the second jacket 27 to heat the kettle body, and low-pressure steam inlets are respectively arranged at relative positions on the diameter of the kettle body. Steam condensate outlets are respectively arranged at the bottom positions of the kettle body.

[0070] In some other embodiments of the present invention, circulating hot water is passed through the first jacket 15 and / or the second jacket 27 to heat the kettle body, and circulating hot water outlets are respectively arranged at relative positions on the diameter of the kettle body, and hot water inlets are respectively arranged at the bottom positions of the kettle body.

[0071] The upper part of the flash tank 30 is provided with a solvent outlet 33, and the lower part is provided with a β-carotene product outlet 32 for discharging the β-carotene product. The solvent outlet 33 is communicated with the gas-phase inlet 43 at the top of the condenser 40. The bottom of the condenser 40 is provided with a liquid-phase outlet 44. The gaseous solvent is condensed in the condenser 40, and the condensed liquid solvent is discharged from the liquid-phase outlet 44 and enters the recovery tank.

[0072] The outer side wall of the condenser 40 is provided with a low-temperature cooling water inlet 41 and a low-temperature cooling water outlet 42 for condensing the gaseous solvent.

[0073] The present invention will be further described below through specific examples and comparative examples. However, it should be understood that these examples are only for more detailed description and should not be construed as limiting the present invention in any form. For the raw materials used in the examples and comparative examples of the present invention, those without specific conditions are carried out according to conventional conditions or the conditions recommended by the manufacturer. For the reagents or instruments without indicating the manufacturer, they are all conventional products that can be obtained by purchasing in the market.

[0074] Example 1

[0075] This example provides a β-carotene production device with controllable color, as Figure 3 shown, including a heating kettle 10, a dissolving kettle 20, a flash tank 30, a condenser 40 and a recovery tank 50 connected in sequence. A high-pressure spray pump 60 is arranged between the dissolving kettle 20 and the flash tank 30 for feeding the β-carotene solution in the dissolving kettle 20 into the flash tank 30 for flash crystallization.

[0076] The upper part of the heating kettle 10 is provided with a first feed inlet 11, a first air inlet 12 and a first exhaust outlet 13. The lower part of the heating kettle 10 is provided with a first discharge outlet 14. The outside of the heating kettle 10 is provided with a first jacket 15, and a heating medium is passed through the first jacket 15 for heating the kettle body. The upper part of the first jacket 15 is provided with a first low-pressure steam inlet 17 and a hot water inlet 19, and the lower part of the first jacket 15 is provided with a first hot water outlet 16 for discharging the heating medium. The outside of the heating kettle 10 is also provided with a temperature display and a pressure display for measuring and outputting the temperature and pressure in the heating kettle 10.

[0077] A pressure display is arranged on the pipeline of the first hot water outlet 16 for monitoring the pressure change in the first jacket 15.

[0078] The upper part of the dissolution kettle 20 is provided with a second feed inlet 21, a second air inlet 24 and a second exhaust outlet 25, and the lower part of the dissolution kettle 20 is provided with a second discharge outlet 28. The second feed inlet 21 is used for feeding the crude β-carotene. The first discharge outlet 14 of the heating kettle 10 is communicated with the third feed inlet 26 of the dissolution kettle 20; it is used to feed the heated solvent into the dissolution kettle 20. A temperature display and a pressure display are also arranged outside the dissolution kettle 20, which are used to measure and output the temperature and pressure inside the dissolution kettle 20.

[0079] A second jacket 27 is arranged outside the dissolution kettle 20, and a heating medium is passed through the second jacket 27 for heating the kettle body. The upper part of the second jacket 27 is provided with a second low-pressure steam inlet 22 and a hot water inlet, and the lower part of the second jacket 27 is provided with a second hot water outlet 23 for discharging the heating medium. A pressure display is arranged on the pipeline of the second hot water outlet 23 for monitoring the pressure change in the second jacket 27.

[0080] A spray pump 60 is arranged between the dissolution kettle 20 and the flash evaporation tank 30, which is used to feed the liquid in the dissolution kettle 20 into the high-pressure nozzle 31 in the flash evaporation tank 30 after increasing the pressure.

[0081] The upper part of the flash evaporation tank 30 is provided with a solvent outlet 33, and the lower part is provided with a β-carotene product outlet 32 for discharging the β-carotene product. A high-pressure nozzle 31 is arranged inside the flash evaporation tank 30, and the energy of the high-pressure air flow is used to atomize the β-carotene solution. A liquid solvent inlet 34 is also arranged at the top of the flash evaporation tank 30 for the liquid solvent to enter the inside of the flash evaporation tank 30 to wash the crystals inside the flash evaporation tank 30.

[0082] The solvent outlet 33 is communicated with the gas-phase inlet 43 at the top of the condenser 40. The bottom of the condenser 40 is provided with a liquid-phase outlet 44. The gaseous solvent is condensed in the condenser 40, and the condensed liquid solvent is discharged from the liquid-phase outlet 44 and enters the recovery tank 50. The outer side wall of the condenser 40 is provided with a low-temperature cooling water inlet 41 and a low-temperature cooling water outlet 42 for condensing the gaseous solvent. A pressure display is arranged on the pipeline of the low-temperature cooling water inlet 41 for monitoring the pressure change of the cooling water in the condenser 40.

[0083] A liquid level gauge is arranged outside the recovery tank 50 for monitoring the liquid level in the recovery tank at any time and regularly discharging the solvent in the recovery tank 50. The top of the recovery tank 50 is also connected with a vacuum tube 51, and a vacuum pump is used to connect to the vacuum tube 51 to evacuate the inside of the recovery tank 50. A fourth emptying port is arranged at the top of the recovery tank 50, and a pressure gauge is arranged on the pipeline of the fourth emptying port for detecting the pressure change of the tank body.

[0084] Example 2

[0085] This embodiment provides a red β-carotene, which is produced using the production device provided in Embodiment 1. The appearance color of the crude β-carotene used is purple-black, and other information is shown in Table 1 below:

[0086] Table 1

[0087] L a b c h D10 (μm) D50 (μm) D90 (μm) 32.43 23.25 9.78 25.22 22.81 2.42 5.72 13.30

[0088] The specific process is as follows:

[0089] 1. Heating dichloromethane:

[0090] Charge 150 Kg of dichloromethane into a 200 L heating kettle, fill it with nitrogen to a pressure of 0.3 MPa, exhaust to 0.05 MPa, and repeat the replacement three times. After the replacement is completed, fill it with nitrogen to a pressure of 0.20 MPa. Start stirring and heating, and heat the dichloromethane to 80 °C for standby.

[0091] 2. Dissolution process:

[0092] Charge 15 Kg of crude β-carotene into a 200 L dissolution kettle, fill it with nitrogen to a pressure of 0.3 MPa, exhaust to 0.05 MPa, and repeat the replacement three times. After the replacement is completed, fill it with nitrogen to a pressure of 0.05 MPa. Put the dichloromethane in the heating kettle into the dissolution kettle and supplement an appropriate amount of nitrogen. Keep it at 80 °C and dissolve for 10 minutes under the condition of 0.5 MPa.

[0093] 3. High-pressure spraying and flash evaporation crystallization:

[0094] Pre-install a high-pressure nozzle with a pore diameter of 0.5 mm in the flash evaporation tank. Open the valve on the vacuum pipe of the dichloromethane receiving tank, evacuate the flash evaporation tank through the dichloromethane receiving tank, and open the inlet and outlet valves of the condenser refrigerant. When the vacuum degree in the flash evaporation tank reaches -0.08 MPa. Transfer the dissolved solution in the high-pressure dissolution kettle into the high-pressure nozzle through a high-pressure spray pump, and control the pressure of the high-pressure spray pump at about 10.0 MPa and the flow rate at 90.0 Kg / h.

[0095] 4. Filtration and drying:

[0096] After high-pressure spraying and flash evaporation crystallization are completed, add 30 kg of dichloromethane to the dissolution kettle. Replace the high-pressure nozzle in the flash evaporation tank with a cleaning spray head with a pore diameter of 2.0 mm, and start the high-pressure spray pump to spray the dichloromethane in the dissolution kettle into the flash evaporation tank to clean the β-carotene crystals on the wall. The β-carotene crystals washed down are filtered, washed with ethanol slurry, and dried in vacuum to obtain the finished product of β-carotene crystals.

[0097] Embodiment 3

[0098] This embodiment provides a red-violet β-carotene. Different from Embodiment 2, in Step 1, dichloromethane is heated to 40°C; in Step 2, 5 Kg of crude β-carotene is put into a 200 L dissolving kettle, and the dissolving temperature is maintained at 40°C. The remaining raw materials and methods are the same as those in Embodiment 2 and will not be elaborated here.

[0099] Embodiment 4

[0100] This embodiment provides a bright red β-carotene. Different from Embodiment 2, in Step 1, dichloromethane is heated to 120°C; in Step 2, the dissolving temperature is maintained at 120°C. The remaining raw materials and methods are the same as those in Embodiment 2 and will not be elaborated here.

[0101] Embodiment 5

[0102] This embodiment provides a bright red β-carotene. Different from Embodiment 2, in Step 3, the aperture of the high-pressure nozzle is 0.1 mm. The remaining raw materials and methods are the same as those in Embodiment 2 and will not be elaborated here.

[0103] Embodiment 6

[0104] This embodiment provides a red-violet β-carotene. Different from Embodiment 2, in Step 3, the aperture of the high-pressure nozzle is 0.8 mm. The remaining raw materials and methods are the same as those in Embodiment 2 and will not be elaborated here.

[0105] Embodiment 7

[0106] This embodiment provides a bright red β-carotene. Different from Embodiment 2, in Step 3, the vacuum degree in the flash tank is -0.097 MPa. The remaining raw materials and methods are the same as those in Embodiment 2 and will not be elaborated here.

[0107] Embodiment 8

[0108] This embodiment provides a red-violet β-carotene. Different from Embodiment 2, in Step 3, the vacuum degree in the flash tank is -0.03 MPa. The remaining raw materials and methods are the same as those in Embodiment 2 and will not be elaborated here.

[0109] Embodiment 9

[0110] This embodiment provides a red β-carotene. Different from Embodiment 2, in Step 3, the pressure of the high-pressure nozzle is 10.7 MPa. The remaining raw materials and methods are the same as those in Embodiment 2 and will not be elaborated here.

[0111] Comparative Example 1

[0112] This comparative example provides a β-carotene. Different from Example 2, step 1 is omitted. In step 2, 150 Kg of dichloromethane is directly added to the dissolution kettle and dissolved for 10 minutes at 80 °C and 0.35 MPa. The remaining preparation steps are the same as those in Example 2 and will not be elaborated here.

[0113] Comparative Example 2

[0114] This comparative example provides a β-carotene. Different from Example 2, a high-pressure nozzle is not installed in the flash tank in step 3, and direct flash crystallization is carried out. The remaining preparation steps are the same as those in Example 2 and will not be elaborated here.

[0115] Comparative Example 3

[0116] This comparative example provides a β-carotene, and the crude β-carotene used is the same as that in Example 2. The specific preparation process is as follows:

[0117] Put 15 Kg of β-carotene crystals and 150 Kg of dichloromethane into a 200 L dissolution kettle, fill with nitrogen to a pressure of 0.3 MPa, exhaust to 0.05 MPa, and replace three times in total. After replacement, fill with nitrogen to a pressure of 0.20 MPa. Start stirring and heating, heat the dichloromethane to 80 °C, keep warm for 30 minutes, after keeping warm, cool down to 25 °C, filter, wash the filter cake with ethanol slurry, and dry it in vacuum. Finally, obtain the finished β-carotene crystals.

[0118] Test Example 1

[0119] The β-carotenes obtained in Examples 2-9 and Comparative Examples 1-3 were detected. Specifically, it includes:

[0120] 1. Detection of cis content: Detected by a high-performance liquid chromatograph of model Agilent1260 produced by Agilent. The chromatographic column is: C18 250*4mm 5μm. Detection wavelength: 455 nm. The mobile phase is ethanol: petroleum ether = 30:70.

[0121] 2. Color detection: Detected by a color difference meter of model spectrophotometer CM-3500d produced by Konica Minolta.

[0122] 3. Particle size detection: The crystallization was wet-detected by a particle size analyzer of model MASTERSIZER 3000 produced by Malvern.

[0123] The results obtained are shown in Table 2 below.

[0124] Table 2

[0125]

[0126]

[0127] In Comparative Examples 1-3 of the present invention, the color of the β-carotene product was not known at the initial stage of preparation. The color of the actually produced product was taken as the standard. As can be seen from Table 2, in the operation process of Examples 2-9, the control of the β-carotene product was realized, and the color of the obtained β-carotene product met the production target.

[0128] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements on some or all of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A production process of color-controllable β-carotene, characterized in that, The crude β-carotene is dissolved using a heated solvent, and the dissolved crude β-carotene solution is subjected to spray and flash crystallization at -0.097 MPa to -0.03 MPa to obtain β-carotene products of different colors.

2. The production process according to claim 1, characterized in that, The colors of the β-carotene include bright red, red, red-violet, and purple-black; The particle size D50 of the bright red is 1.48 μm - 1.83 μm; in the Lab mode: the L value is 35.42 - 39.42, the a value is 43.34 - 45.62, and the b value is 30.2 - 36.5; The particle size D50 of the red is 1.95 μm - 2.23 μm; in the Lab mode: the L value is 34.9 - 35.2, the a value is 39.56 - 42.05, and the b value is 26.88 - 29.25; The particle size D50 of the red-violet is 2.30 μm - 4.32 μm; in the Lab mode: the L value is 32.53 - 34.36, the a value is 35.34 - 37.34, and the b value is 15.6 - 23.22; The particle size D50 of the purple-black is 5.72 μm - 6.27 μm; in the Lab mode: the L value is 31.32 - 32.53, the a value is 19.89 - 23.25, and the b value is 8.78 - 9.

78.

3. The production process according to claim 1, characterized in that, The dissolved crude β-carotene solution is pressurized by a high-pressure spray pump and then enters a high-pressure nozzle.

4. The production process according to claim 3, characterized in that, The color of the β-carotene is bright red, and the aperture of the high-pressure nozzle is 0.1 mm - 0.5 mm.

5. The production process according to claim 3, characterized in that, The color of the β-carotene is red, and the aperture of the high-pressure nozzle is 0.5 mm - 0.7 mm.

6. The production process according to claim 3, characterized in that, The color of the β-carotene is red-violet, and the aperture of the high-pressure nozzle is 0.5 mm - 0.8 mm.

7. The production process according to claim 3, characterized in that, The color of the β-carotene is purple-black, and the aperture of the high-pressure nozzle is 1.0 mm - 1.2 mm.

8. The production process according to claim 1, characterized in that, The heating, the dissolution, and the flash crystallization are all carried out under the protection of an inert gas.

9. The production process according to claim 1, characterized in that, The temperature of the heated solvent is 40°C to 120°C.

10. The production process according to claim 1, characterized in that, The temperature for dissolving the crude β-carotene is 40°C to 120°C, the pressure for the dissolution is 0 MPa to 1.0 MPa, and the time for the dissolution is 8 min - 15 min.

11. The production process according to claim 1, characterized in that, The mass ratio of the crude β-carotene to the solvent is 1:8 to 50.

12. The production process according to claim 1, wherein The mass ratio of the crude β-carotene to the solvent is 1:8 to 15.

13. The production process according to claim 3, characterized in that, The spray pressure of the high-pressure spray pump is 1.0 MPa to 15.0 MPa.

14. The production process according to claim 3, characterized in that, The spray pressure of the high-pressure spray pump is 8.0 MPa to 12.0 MPa.

Images