A method and system for full-automatic online preparation of sugar crystallization process seed

Abstract

The present application relates to the field of sugar making, and provides a full-automatic online seed preparation method and system for a sugar making crystallization process, comprising: raw material bins, a dissolving reaction tank, a filter washer, a storage bin, a seed waiting bin and a crystallization tank connected in sequence according to a process sequence; further comprising an anhydrous ethanol storage tank, a water tank and a gas-water separation tank, the dissolving reaction tank, the filter washer and the storage bin being connected with the anhydrous ethanol storage tank, the dissolving reaction tank being connected with the water tank, and the filter washer and the crystallization tank being connected with the gas-water separation tank. The present application can realize precise quality control, efficient crystallization, safety and sterility, intelligent adaptation, high-quality seed preparation and stability and controllability.

Description

Technical Field

[0001] This invention relates to the field of sugar production technology, specifically to a fully automated online method and system for preparing seed crystals in the sugar crystallization process. Background Technology

[0002] Crystallization is the core purification and shaping process in sugar refining. The timing, amount, particle size, and dispersion uniformity of seed crystals directly determine the product's crystal particle size distribution, product purity, and production efficiency. Currently, in the sugar industry, seed crystal addition and powder feeding are mostly done manually, and some simple devices can only achieve a single addition function, which cannot meet the needs of continuous and precise production.

[0003] The existing technologies for preparing and adding sugar crystal seeds have the following key shortcomings: Manual addition has large errors: the amount, timing and speed of seed crystal addition cannot be precisely controlled, which can easily lead to an imbalance of supersaturation in the crystallization system, causing secondary nucleation (waste sand), resulting in uneven crystal particle size and high CV value, which directly affects product quality.

[0004] Poor seed dispersibility: During the seeding process, the seed crystals tend to agglomerate and clump together, resulting in insufficient contact with the mother liquor and reduced crystallization efficiency.

[0005] High risk of contamination and poor adaptability: There are many manual intervention steps, high labor intensity, low production efficiency, and it is easy to introduce foreign objects and microbial contamination. It cannot meet the sterility requirements of pharmaceutical-grade sugar products and is difficult to match with continuous production lines.

[0006] The existing seed crystal addition devices are mostly single-function designs and are not linked with the crystallization tank, making it impossible to accurately control the timing of addition based on the supersaturation of the crystallization system; at the same time, they lack online cleaning and sterilization structures, making cleaning and maintenance difficult.

[0007] Traditional seed production processes are outdated: Traditional mechanical grinding methods are time-consuming, energy-intensive, and result in low crystal nucleus uniformity. The grinding process can easily damage the crystal form and may leave behind foreign matter such as metal, which cannot meet the sterility and foreign matter-free requirements of injectable pharmaceutical sugars, thus limiting high-end applications. Summary of the Invention

[0008] To address the aforementioned technical problems, this invention aims to provide a fully automated online method and system for preparing seed crystals in the sugar crystallization process. To solve these problems, this invention employs the following technical solution: A fully automated online seed crystal preparation system for sugar crystallization includes: a raw material silo, a dissolution reaction tank, a filter and washer, a storage silo, a seed crystal waiting silo, and a crystallization tank connected in sequence according to the process order; It also includes an anhydrous ethanol storage tank, a water tank and a gas-liquid separator, a dissolution reaction tank, a filter and scrubber and a storage silo are respectively connected to the anhydrous ethanol storage tank, the dissolution reaction tank is connected to the water tank, and the scrubbing filter and crystallization tank are respectively connected to the gas-liquid separator.

[0009] A fully automated online method for preparing seed crystals in a sugar crystallization process, based on the aforementioned fully automated online seed crystal preparation system for a sugar crystallization process, includes the following steps: S1: Obtain syrup raw materials; S2: Ethanol crystallization: Add the syrup raw materials into the dissolving reaction tank, start the stirring device on the dissolving reaction tank, and use the anhydrous ethanol storage tank to quickly add 3-6 times the volume of the syrup to form a uniform sugar-water-ethanol seed mixture. S3: Filtration and washing: The seed crystal mixture is sent into a filter and washer with negative pressure function. The vacuum system is turned on, and the seed crystal mixture is filtered through a 10–20μm filter screen to separate the mother liquor from the seed crystals. The seed crystals are washed 2-3 times with anhydrous ethanol in the anhydrous ethanol storage tank to remove moisture and uncrystallized sugar from the surface of the seed crystals. The sugar-water-ethanol mixture generated during washing is then vacuum-inhaled into the crystallization tank, mixed with the syrup raw material, and recycled. S3: Seed preparation: Use the online weighing module of the filter washer to read the weight of the seed crystals, add anhydrous ethanol to the anhydrous ethanol storage tank at a ratio of 30%–50% solid content of the seed crystals, and start the stirring device 2 on the filter washer to stir so that the seed crystals and anhydrous ethanol are fully mixed. S4: Low temperature storage: The prepared seed crystal mixture is sent into the storage chamber, and the temperature of the storage chamber is controlled at 0℃–10℃. At the same time, the stirring device in the storage chamber is started to stir to prevent the seed crystals from settling and clumping, and to maintain the uniformity and fluidity of the seed crystals. S5: Linked seeding: When the concentrated base material in the crystallization tank reaches the preset seeding concentration, a seeding preparation signal is sent to the preparation system; The preparation system automatically calculates the required amount of seeding based on the amount of sugar paste in the crystallizer, the particle size of the target product, and the particle size of the seed crystals. The corresponding amount of seed crystal mixture is then delivered to the seed crystal waiting chamber via a metering pump. When the seed crystal waiting chamber receives the seeding signal from the crystallization tank, it automatically opens the seeding valve and draws the seed crystal mixture into the crystallization tank under vacuum, thus completing the fully automatic addition of seed crystals. S6: CIP Cleaning: The CIP cleaning program can be started with one click through the PLC control system. The preparation system automatically completes the cleaning steps of each piece of equipment and pipeline in sequence according to the process. After cleaning, the waste liquid is automatically discharged without manual intervention. Optionally, S1 includes: When preparing injectable pharmaceutical excipient sugars, the finished sugar is mixed with hot water at 70-85℃ or purified water to prepare a 70-90 Brix sugar solution as raw material.

[0010] Optionally, it also includes S7, which includes: SIP sterilization: After CIP cleaning is completed, the SIP sterilization program is started, and anhydrous ethanol is used for closed-loop sterilization to ensure the system is sterile and meets GMP sterility requirements.

[0011] Optionally, S1 includes: when it is necessary to prepare food-grade, oral pharmaceutical excipient sugar, extracting the concentrated base material from crystallization tank 70–90 Brix as raw material.

[0012] Optionally, the stirring speed of the stirring device is 60–80 r / min.

[0013] Optionally, the continuous stirring time of the stirring device is 5–30 min.

[0014] Optionally, the vacuum level of the vacuum system is controlled at -0.07 to -0.08 MPa.

[0015] Optionally, the stirring speed of the second stirring device is 30–50 r / min.

[0016] Optionally, the cycle time for the cyclic sterilization is 30 minutes.

[0017] The present invention has the following beneficial effects: Precise quality control: Fully automated and precise dosing eliminates human error, stably controls the supersaturation of the crystallization system, avoids secondary nucleation, reduces the crystal CV value, and improves product quality; High-efficiency crystallization: The seed crystals are uniformly dispersed throughout the process, without agglomeration or clumping, and have sufficient contact with the mother liquor, significantly improving crystallization efficiency; Safe and sterile: The entire process is closed and unmanned, reducing labor intensity, eliminating foreign matter and microbial contamination, meeting pharmaceutical-grade sterility requirements, and suitable for continuous production; Intelligent Adaptation: The integrated design can be linked with the crystallization tank to accurately match the timing of dosing; integrated CIP / SIP online cleaning and sterilization for convenient maintenance; High-quality seed production: Online ethanol crystallization seed production replaces mechanical grinding, which is highly efficient and low-consumption, produces uniform crystal nuclei, and eliminates crystal form damage and foreign matter residue, which is conducive to crystal growth; Stable and controllable: Fully automated and data traceable, adaptable to the production of multiple grades of sugar, including food-grade, oral-grade, and injectable-grade, with high production stability. Attached Figure Description

[0018] The present invention will be further described with reference to the accompanying drawings, but the embodiments in the drawings do not constitute any limitation on the present invention. For those skilled in the art, other drawings can be obtained based on the following drawings without creative effort.

[0019] Figure 1 This is a schematic diagram of the structure of a fully automated online seed crystal preparation system for sugar crystallization process according to the present invention; Detailed Implementation

[0020] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0021] In the description of this invention, it should be noted that the terms "vertical," "upper," "lower," and "horizontal," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing the invention and for simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on the invention. Furthermore, "first," "second," "third," and "fourth" are used for descriptive purposes only and should not be construed as indicating or implying relative importance.

[0022] In the description of this invention, it should also be noted that, unless otherwise explicitly specified and limited, the terms "set," "install," "connect," and "link" should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral connection; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or a connection through an intermediate medium; and they can refer to the internal communication between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0023] This invention is applicable to the crystallization process of various sugar products such as sucrose and xylitol, and can achieve precise addition and uniform dispersion of seed crystals, adapting to the needs of continuous sugar production.

[0024] To address the technical problems in the background art, this invention discloses a fully automated online seed crystal preparation system and method for sugar crystallization. The system is completely sealed and can operate in a vacuum / sterile environment, realizing full automation of the entire process from seed crystal preparation to storage, metering, conveying, addition, linkage control, and cleaning and sterilization. It is suitable for the crystallization production of sugars such as food-grade, oral pharmaceutical-grade, and injectable pharmaceutical-grade sucrose and xylitol.

[0025] like Figure 1 As shown, a fully automated online seed preparation system for sugar crystallization includes: a raw material silo, a dissolution reaction tank, a filter and washer, a storage silo, a seed waiting silo, and a crystallization tank, which are connected in sequence according to the process order. It also includes an anhydrous ethanol storage tank, a water tank and a gas-liquid separator, a dissolution reaction tank, a filter and scrubber and a storage silo are respectively connected to the anhydrous ethanol storage tank, the dissolution reaction tank is connected to the water tank, and the scrubbing filter and crystallization tank are respectively connected to the gas-liquid separator.

[0026] A fully automated online method for preparing seed crystals in a sugar crystallization process, based on the aforementioned fully automated online seed crystal preparation system for a sugar crystallization process, includes the following steps: S1: Obtain syrup raw materials; S2: Ethanol crystallization: Add the syrup raw materials into the dissolving reaction tank, start the stirring device on the dissolving reaction tank, and use the anhydrous ethanol storage tank to quickly add 3-6 times the volume of the syrup to form a uniform sugar-water-ethanol seed mixture. S3: Filtration and washing: The seed crystal mixture is sent into a filter and washer with negative pressure function. The vacuum system is turned on, and the seed crystal mixture is filtered through a 10–20μm filter screen to separate the mother liquor from the seed crystals. The seed crystals are washed 2-3 times with anhydrous ethanol in the anhydrous ethanol storage tank to remove moisture and uncrystallized sugar from the surface of the seed crystals. The sugar-water-ethanol mixture generated during washing is then vacuum-inhaled into the crystallization tank, mixed with the syrup raw material, and recycled. S3: Seed preparation: Use the online weighing module of the filter washer to read the weight of the seed crystals, add anhydrous ethanol to the anhydrous ethanol storage tank at a ratio of 30%–50% solid content of the seed crystals, and start the stirring device 2 on the filter washer to stir so that the seed crystals and anhydrous ethanol are fully mixed. S4: Low temperature storage: The prepared seed crystal mixture is sent into the storage chamber, and the temperature of the storage chamber is controlled at 0℃–10℃. At the same time, the stirring device in the storage chamber is started to stir to prevent the seed crystals from settling and clumping, and to maintain the uniformity and fluidity of the seed crystals. S5: Linked seeding: When the concentrated base material in the crystallization tank reaches the preset seeding concentration, a seeding preparation signal is sent to the preparation system; The preparation system automatically calculates the required amount of seeding based on the amount of sugar paste in the crystallizer, the particle size of the target product, and the particle size of the seed crystals. The corresponding amount of seed crystal mixture is then delivered to the seed crystal waiting chamber via a metering pump. When the seed waiting chamber receives the seeding signal from the crystallization tank, it automatically opens the seeding valve and draws the seed mixture into the crystallization tank under vacuum, thus completing the fully automatic addition of seed crystals. S6: CIP Cleaning: The CIP cleaning program can be started with one click through the PLC control system. The preparation system automatically completes the cleaning steps of each piece of equipment and pipeline in sequence according to the process. After cleaning, the waste liquid is automatically discharged without manual intervention. According to an optional embodiment of the present invention, S1 includes: When preparing injectable pharmaceutical excipient sugars, the finished sugar is mixed with hot water at 70-85℃ or purified water to prepare a 70-90 Brix sugar solution as raw material.

[0027] In an optional embodiment of the present invention, S7 is further included, which includes: SIP sterilization: after CIP cleaning is completed, the SIP sterilization program is started, and anhydrous ethanol is used for closed-loop sterilization to ensure the system is sterile and meets the GMP sterility requirements.

[0028] According to an optional embodiment of the present invention, S1 includes: when it is necessary to prepare food-grade, oral pharmaceutical excipient sugar, extracting the concentrated base material from crystallization tank 70–90 Brix as raw material.

[0029] According to an optional embodiment of the present invention, the stirring speed of the stirring device is 60–80 r / min.

[0030] According to an optional embodiment of the present invention, the continuous stirring time of the stirring device is 5–30 min.

[0031] According to an optional embodiment of the present invention, the vacuum degree of the vacuum system is controlled at -0.07 to -0.08 MPa.

[0032] According to an optional embodiment of the present invention, the stirring speed of the second stirring device is 30–50 r / min.

[0033] In an optional embodiment of the present invention, the cycle time for the cyclic sterilization is 30 minutes.

[0034] The core of this system adopts online ethanol crystallization seed production technology, replacing the traditional mechanical grinding seed production method. It adapts to the production needs of different grades of sugar through a dual raw material path design. It uses a combination of sealed negative pressure, low-temperature stirring, and precise metering to achieve precise seed addition and precise particle size control. Through linkage control with the crystallizer, it accurately controls the timing and amount of seed addition. The entire process integrates CIP / SIP online cleaning and sterilization functions to meet aseptic production requirements. Ultimately, it achieves fully automated operation of seed preparation, storage, metering, addition, linkage, and sterilization, effectively solving many defects of existing technologies.

[0035] Installation and Deployment: Securely install each piece of equipment in the crystallization tank area of ​​the sugar crystallization process in the sugar workshop; The pipeline is made of sanitary stainless steel and is connected in the following order: raw material silo / water tank → dissolution reaction tank → filter and washer → seed storage silo → seed waiting silo → crystallization tank to ensure that the pipeline is sealed and leak-free. Connect the vacuum interface of the filter washer to the vacuum system, and connect the weighing module, temperature sensor, metering pump and other equipment to the PLC control cabinet to realize synchronous signal transmission and centralized control. Independently lay CIP cleaning pipelines, SIP sterilization pipelines, and ethanol supply pipelines. After the pipeline laying is completed, conduct a sealing pressure test to ensure there are no leaks or blockages and that the system operation requirements are met.

[0036] Seed addition and traceability: The PLC control system records key parameters such as temperature, vacuum degree, material metering, and solid content of the seed in real time throughout the entire process of seed preparation, storage, and addition. The data cannot be modified, enabling full traceability of the production process.

[0037] System Control: This system adopts a PLC + touch screen control method, supports preset key process parameters and one-button start / stop of the system, and can automatically complete the entire process of seed preparation, storage, metering, addition, cleaning and sterilization, realizing fully unmanned operation, reducing manual labor intensity and improving production stability.

[0038] Key process parameters: The beneficial effects of this invention are as follows: Precise quality control: Fully automated and precise dosing eliminates human error, stably controls the supersaturation of the crystallization system, avoids secondary nucleation, reduces the crystal CV value, and improves product quality; High-efficiency crystallization: The seed crystals are uniformly dispersed throughout the process, without agglomeration or clumping, and have sufficient contact with the mother liquor, significantly improving crystallization efficiency; Safe and sterile: The entire process is closed and unmanned, reducing labor intensity, eliminating foreign matter and microbial contamination, meeting pharmaceutical-grade sterility requirements, and suitable for continuous production; Intelligent Adaptation: The integrated design can be linked with the crystallization tank to accurately match the timing of dosing; integrated CIP / SIP online cleaning and sterilization for convenient maintenance; High-quality seed production: Online ethanol crystallization seed production replaces mechanical grinding, which is highly efficient and low-consumption, produces uniform crystal nuclei, and eliminates crystal form damage and foreign matter residue, which is conducive to crystal growth; Stable and controllable: Fully automated and data traceable, adaptable to the production of multiple grades of sugar, including food-grade, oral-grade, and injectable-grade, with high production stability.

[0039] The components, modules, mechanisms, and devices in this invention that are not described in detail are all general standard parts or components known to those skilled in the art. Their structures and principles can be learned by those skilled in the art through technical manuals or conventional experimental methods.

[0040] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit the scope of protection of the present invention. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the essence and scope of the technical solutions of the present invention.

Claims

1. A fully automated online seed crystal preparation system for sugar crystallization, characterized in that, include: The raw material silo, dissolution reaction tank, filter and washer, storage silo, seed crystal waiting silo and crystallization tank are connected in sequence according to the process sequence. It also includes an anhydrous ethanol storage tank, a water tank and a gas-liquid separator, a dissolution reaction tank, a filter and scrubber and a storage silo are respectively connected to the anhydrous ethanol storage tank, the dissolution reaction tank is connected to the water tank, and the scrubbing filter and crystallization tank are respectively connected to the gas-liquid separator.

2. A fully automated online method for preparing seed crystals in a sugar crystallization process, characterized in that, The fully automated online seed crystal preparation system for sugar crystallization as described in claim 1 includes the following steps: S1: Obtain syrup raw materials; S2: Ethanol crystallization: Add the syrup raw materials into the dissolving reaction tank, start the stirring device on the dissolving reaction tank, and use the anhydrous ethanol storage tank to quickly add 3-6 times the volume of the syrup to form a uniform sugar-water-ethanol seed mixture. S3: Filtration and washing: The seed crystal mixture is sent into a filter and washer with negative pressure function. The vacuum system is turned on, and the seed crystal mixture is filtered through a 10–20μm filter screen to separate the mother liquor from the seed crystals. The seed crystals are washed 2-3 times with anhydrous ethanol in the anhydrous ethanol storage tank to remove moisture and uncrystallized sugar from the surface of the seed crystals. The sugar-water-ethanol mixture generated during washing is then vacuum-inhaled into the crystallization tank, mixed with the syrup raw material, and recycled. S3: Seed preparation: Use the online weighing module of the filter washer to read the weight of the seed crystals, add anhydrous ethanol to the anhydrous ethanol storage tank at a ratio of 30%–50% solid content of the seed crystals, and start the stirring device 2 on the filter washer to stir so that the seed crystals and anhydrous ethanol are fully mixed. S4: Low temperature storage: The prepared seed crystal mixture is sent into the storage chamber, and the temperature of the storage chamber is controlled at 0℃–10℃. At the same time, the stirring device in the storage chamber is started to stir to prevent the seed crystals from settling and clumping, and to maintain the uniformity and fluidity of the seed crystals. S5: Linked seeding: When the concentrated base material in the crystallization tank reaches the preset seeding concentration, a seeding preparation signal is sent to the preparation system; The preparation system automatically calculates the required amount of seeding based on the amount of sugar paste in the crystallizer, the particle size of the target product, and the particle size of the seed crystals. The corresponding amount of seed crystal mixture is then delivered to the seed crystal waiting chamber via a metering pump. When the seed waiting chamber receives the seeding signal from the crystallization tank, it automatically opens the seeding valve and draws the seed mixture into the crystallization tank under vacuum, thus completing the fully automatic addition of seed crystals. S6: CIP Cleaning: The CIP cleaning program can be started with one click via the PLC control system. The preparation system automatically completes the cleaning steps of each piece of equipment and pipeline in sequence according to the process. After cleaning, the waste liquid is automatically discharged without manual intervention.

3. The fully automated online preparation method for seed crystals in a sugar crystallization process according to claim 2, characterized in that, S1 includes: When preparing injectable pharmaceutical excipient sugars, the finished sugar is mixed with hot water at 70-85℃ or purified water to prepare a 70-90 Brix sugar solution as raw material.

4. The fully automated online preparation method for seed crystals in a sugar crystallization process according to claim 3, characterized in that, It also includes S7, which includes: SIP sterilization: After CIP cleaning is completed, the SIP sterilization program is started, and anhydrous ethanol is used for closed-loop sterilization to ensure the system is sterile and meets GMP sterility requirements.

5. The fully automated online preparation method for seed crystals in a sugar crystallization process according to claim 2, characterized in that, S1 includes: when it is necessary to prepare food-grade, oral pharmaceutical excipient sugar, extracting the concentrated base material from crystallization tank 70–90brix as raw material.

6. The fully automated online preparation method for seed crystals in a sugar crystallization process according to claim 2, characterized in that, The stirring speed of the stirring device is 60–80 r / min.

7. The fully automated online preparation method for seed crystals in a sugar crystallization process according to claim 2, characterized in that, The continuous stirring time of the stirring device is 5–30 min.

8. The fully automated online preparation method for seed crystals in a sugar crystallization process according to claim 2, characterized in that, The vacuum level of the vacuum system is controlled at -0.07 to -0.08 MPa.

9. The fully automated online preparation method for seed crystals in a sugar crystallization process according to claim 2, characterized in that, The stirring speed of the second stirring device is 30–50 r / min.

10. The fully automated online preparation method for seed crystals in a sugar crystallization process according to claim 4, characterized in that, The cycle time for the cyclic sterilization is 30 minutes.

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