Extraction tank and equipment group for producing enzymolysis bone meal rich in low-molecular sodium chondroitin sulfate
By combining equipment for cyclic processing and continuous countercurrent extraction, the problem of unsatisfactory yield of sodium chondroitin sulfate in bovine cartilage has been solved, achieving efficient and clean production and improving the yield of sodium chondroitin sulfate and the output of co-products.
Patent Information
- Application Number
- CN202422914579.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-27
- Publication Date
- 2025-11-21
- Estimated Expiration
- 2034-11-27
AI Technical Summary
In existing technologies, the yield of sodium chondroitin sulfate extracted from bovine cartilage is not ideal, and a large amount of usable material is emitted, making it difficult to achieve clean production and full utilization.
The equipment group, consisting of an extraction tank, an oil removal tank, a ceramic membrane filter, and a transfer tank connected in a closed-loop pipeline, achieves the cyclical treatment of animal cartilage through stirring, crushing, enzymatic hydrolysis, continuous countercurrent extraction, and separation. It controls the degree of hydrolysis and molecular weight, thereby improving the yield of sodium chondroitin sulfate.
The yield of sodium chondroitin sulfate was significantly improved to 5-9%, of which 30-50% had a molecular weight of less than 5000. Collagen and sodium hyaluronate were also produced, reducing the discharge of waste and achieving clean production.
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Figure CN223576501U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to biological medicine raw material preparation technology, especially is used for producing the extraction tank and equipment group of the enzymatic bone powder rich in low molecule sodium chondroitin sulfate. BACKGROUND
[0002] Sodium chondroitin sulfate (abbreviation CS) is an acid mucopolysaccharide, widely exists in cow bone, pig bone, chicken bone, shark bone, squid bone, belongs to glycosaminoglycan, is a natural source biological macromolecule.Sodium chondroitin sulfate is composed of 50-70 disaccharide units, and the disaccharide unit is formed by glucuronic acid and amino galactose through beta-1, 3 glycosidic bond, and the disaccharide is polymerized into macromolecule by beta-1, 4 glycosidic bond, has the physiological functions such as lowering blood fat, anticoagulation, anti-inflammatory and antitumor.Clinically, it is mainly used as the treatment of osteoarthritis, hyperlipidemia, angina pectoris, atherosclerosis and other diseases, and its eye drops have the treatment of corneal injury, corneal ulcer or keratitis;In food, sodium chondroitin sulfate is classified as dietary supplement by FDA in the United States, and Australia uses it as a nutritional health product for improving or preventing arthrosis.
[0003] At present, sodium chondroitin sulfate is produced by enzymatic hydrolysis from animal cartilage.Animal cartilage, especially cow cartilage is very high-quality material, easy to obtain in large quantities for industrial production, and it is rich in valuable ingredients such as chondroitin sulfate, collagen, oil and calcium, in the prior art, a large amount of useful material is discharged in the process of extracting sodium chondroitin sulfate from cow cartilage, and the yield of sodium chondroitin sulfate is not ideal;How to improve the yield of sodium chondroitin sulfate, simultaneously coproduce collagen, beef tallow, amino acid powder and high-calcium powder, realize the clean production of full utilization of cow cartilage and reduction of three wastes discharge is an urgent problem to be solved and improved. Utility model content
[0004] The utility model provides an extraction tank and equipment group for efficiently producing enzymatic bone powder according to the above-mentioned field demand, and specifically as follows:
[0005] An equipment group for producing enzymatic bone powder rich in low molecule sodium chondroitin sulfate, characterized by comprising an extraction tank, an oil removal tank, a first extraction liquid transfer tank, a ceramic membrane filter and a second extraction liquid transfer tank connected through pipelines in a closed loop, for cyclic treatment of raw materials.
[0006] The extraction tank is used for stirring, crushing and enzymatic hydrolysis of animal cartilage, has a cylindrical tank body, and the lower part of the tank body is conical;An electric motor is arranged at the top of the tank body, and a stirring shaft controlled by the electric motor is located at the axial center of the tank body and extends to the conical bottom;The lower part of the stirring shaft is provided with a stirring paddle with shearing function, and the middle and upper parts are provided with stirring paddles.
[0007] The bottom cover of the tank body is provided with a bottom water inlet pipe, a valve and an air inlet pipe; the top of the tank body is provided with a discharge outlet for discharging the enzymatic liquid into the oil removal tank.
[0008] The liquid inlet of the oil removal tank is connected with the discharge outlet arranged on the upper portion of the extraction tank through a pipeline, so that the enzymatic liquid in the extraction tank can be discharged into the oil removal tank for oil removal.
[0009] The first extraction liquid transfer tank is used for collecting the oil-removed liquid from the oil removal tank,
[0010] The ceramic membrane filter is used for filtering the liquid material from the first extraction liquid transfer tank,
[0011] The second extraction liquid transfer tank is used for collecting the filtered liquid generated by the ceramic membrane filter, and the bottom water inlet pipe of the extraction tank is connected with the liquid inlet of the oil removal tank through a pipeline, so that the filtered liquid can be returned to the extraction tank through the bottom water inlet pipe by the backflow pump, thereby realizing the cyclic treatment of the liquid material.
[0012] Preferably, the equipment set further comprises an ultrafiltration transfer tank and an ultrafiltration device, the ultrafiltration transfer tank is used for collecting the liquid material which has completed the cyclic treatment in the extraction tank, and the ultrafiltration device is used for ultrafiltrating the liquid material which has completed the cyclic treatment, and the filtered liquid generated by the ultrafiltration is subjected to post-treatment to obtain the enzymatic bone powder.
[0013] Preferably, the equipment set is characterized in that the top of the extraction tank is further provided with a feeding hole, an alkali pipe and an acid pipe.
[0014] Preferably, the equipment set is characterized in that the side wall of the extraction tank is sequentially provided with a lower temperature detection pipe, a middle temperature detection pipe and an upper temperature detection pipe from bottom to top.
[0015] Preferably, the equipment set is characterized in that the side wall of the extraction tank is further provided with a sampling and analysis pipe and a disinfectant pipe.
[0016] The filter membrane parameter of the ceramic membrane filter in any of the above equipment sets is 3000 daltons.
[0017] In another aspect of the utility model, an extraction tank for producing the enzymatic bone powder rich in low-molecular sodium chondroitin sulfate is provided, and the extraction tank is characterized in that it has a cylindrical tank body, and the lower portion of the tank body is conical; a motor is arranged at the top of the tank body, a stirring shaft controlled by the motor is located at the axial center position in the tank body and extends to the conical bottom, a stirring paddle with a shearing function is arranged at the lower portion of the stirring shaft, and stirring paddles are arranged at the middle portion and the upper portion.
[0018] The bottom cover of the tank body is provided with a bottom water inlet pipe, a valve and an air inlet pipe; the top of the tank body is provided with a discharge outlet for discharging the enzymatic liquid into the oil removal tank.
[0019] The extraction tank, preferably, is characterized in that a feeding hole, an alkali pipe, and an acid pipe are also provided on the top of the extraction tank.
[0020] Preferably, the extraction tank is characterized in that a lower temperature detection tube, a middle temperature detection tube, and an upper temperature detection tube are arranged sequentially from bottom to top on the side wall of the extraction tank.
[0021] Preferably, the extraction tank is characterized in that a sampling and analysis tube and a disinfectant tube are further provided on the side wall of the extraction tank.
[0022] The beneficial effects of this utility model are:
[0023] The extraction tank for producing enzymatically hydrolyzed bone powder based on animal cartilage provided by this utility model can realize shearing, grinding, fluid flushing dissolution, and solid-liquid separation. It can continuously pulverize cartilage and release water-soluble substances such as collagen and glycoproteins. The concentration of dissolved substances is controllable, and the production capacity of a single tank can be increased.
[0024] In this application, the retentate from the ceramic membrane filtration is recycled, employing continuous countercurrent extraction and separation to continuously separate oils, low-molecular-weight peptides, and mucopolysaccharides from the hydrolysate. This reduces the concentration of hydrolysate products, increases the enzymatic hydrolysis rate, and allows for control over the degree of hydrolysis, thereby improving the product yield within the controlled molecular weight range of the hydrolysate. Simultaneously, it prevents oil accumulation from adhering to bone particles and affecting the release of soluble substances from the bone particles, and increases the adsorption of proteases to bone particles, further enhancing the hydrolysis rate and increasing the yield of enzymatically hydrolyzed bone powder. No chemical extraction agents are used in this process. Experimental data show that the yield of enzymatically hydrolyzed bone powder is 6%-10%, of which sodium chondroitin sulfate (of which 30-50% has a molecular weight less than 5000) accounts for 90-95%, protein 2-4%, and sodium hyaluronate 0.5-1%. Attached Figure Description
[0025] Figure 1 A schematic diagram of the extraction tank structure for producing enzymatically hydrolyzed bone powder rich in low-molecular-weight chondroitin sulfate sodium according to this utility model: Figure 2 The schematic diagram of the equipment assembly for producing enzymatically hydrolyzed bone powder rich in low-molecular-weight chondroitin sulfate sodium according to this utility model is as follows: 1-tank body 1, 2-motor 2, 3-stirring shaft, 4-stirring paddle with shearing function 4, 5-stirring paddle; 6-bottom water inlet pipe, 7-valve, 8-air inlet pipe, 9-outlet, 10-feeding hole, 11-alkali pipe, 12-acid pipe, 13-lower temperature detection pipe, 14-middle temperature detection pipe, 15-upper temperature detection pipe; 16-sampling and analysis pipe, 17 and disinfectant pipe;
[0026] 21-Oil removal tank, 22-First extract transfer tank, 23-Ceramic membrane filter, 24-Second extract transfer tank. Detailed Implementation
[0027] The specific implementation process of the utility model is described below in combination with the drawings, and the following description is only used for exemplary illustration of the utility model and does not serve to limit the protection scope of the utility model. Unless otherwise defined, the professional terms used in the utility model have the same meaning as generally understood by those skilled in the art.
[0028] As shown in Figure 1 The extraction tank provided by the utility model has a cylindrical tank body 1, and the lower part of the tank body 1 is conical. A motor 2 is arranged at the top of the tank body, and a stirring shaft 3 controlled by the motor 2 is located at the shaft center position in the tank body and extends to the conical bottom. A stirring paddle 4 with shearing function is arranged at the lower part of the stirring shaft 2, and a stirring paddle 5 is arranged at the middle and upper parts.
[0029] The bottom cover of the tank body is provided with a bottom water inlet pipe 6, a valve 7 and an air inlet pipe 8. The top of the tank body is provided with a discharge port 9 for discharging the enzymatic material liquid into an oil removal tank. A charging hole 10, an alkali pipe 11 and an acid pipe 12 are also arranged.
[0030] In some preferred embodiments, a lower temperature detection pipe 13, a middle temperature detection pipe 14 and an upper temperature detection pipe 15 are sequentially arranged on the side wall of the tank body 1 from bottom to top.
[0031] In some preferred embodiments, a sampling and analysis pipe 16 and a disinfectant pipe 17 are also arranged on the side wall of the tank body 1.
[0032] In the use process, the stirring paddle 4 with shearing function cuts and extrudes the animal cartilage into fine particles in the stirring process, and the material liquid as a whole is in a slurry state.
[0033] As shown in Figure 2 The utility model provides an example of a device group for producing enzymatic bone powder, which comprises any of the above-mentioned extraction tanks, an oil removal tank 21, a first extraction liquid transfer tank 22, a ceramic membrane filter 23 and a second extraction liquid transfer tank 24 connected through pipelines in a closed loop, and is used for cyclically processing animal cartilage.
[0034] The extraction tank is used for stirring, crushing and enzymatic hydrolysis of animal cartilage.
[0035] The discharge port 9 arranged at the upper part of the extraction tank is connected with the oil removal tank 21 through a pipeline, so that the enzymatic material liquid in the extraction tank can be discharged into the oil removal tank 21 for oil removal.
[0036] The first extraction liquid transfer tank 22 is used for collecting the material liquid after oil removal from the oil removal tank 21,
[0037] The ceramic membrane filter 23 is used for filtering the liquid material from the first extraction liquid transfer tank.
[0038] The second extraction liquid tank 24 is used for collecting the filtration interception liquid generated by the ceramic membrane filter 23, and is connected with the bottom water inlet pipe 6 of the extraction tank through a pipeline, so that the filtration interception liquid is returned to the extraction tank through the backflow pump via the bottom water inlet pipe 6, thereby realizing the cyclic treatment of the material liquid.
[0039] In some preferred embodiments, the equipment combination according to the need further comprises an ultrafiltration transfer tank used for collecting the material liquid which has completed the cyclic treatment in the extraction tank, and an ultrafiltration device used for performing ultrafiltration on the material liquid which has completed the cyclic treatment, and the interception liquid generated by the ultrafiltration is subjected to post-treatment to obtain the enzymatic bone powder.
[0040] The equipment combination of the utility model is used for producing the enzymatic bone powder rich in low-molecular sodium chondroitin sulfate, and the steps are as follows:
[0041] S1. Pre-treatment: the animal cartilage is cooked, then the floating oil is removed, and then the animal cartilage is crushed in the extraction tank; the extraction tank is provided with a stirring paddle with shearing function and a baffle in the lower part, the tank body is conical, the bottom cover is provided with a bottom water inlet pipe and a valve; the animal cartilage is crushed into fine particles by shearing and extrusion between the bone particles in the shearing and stirring process of the stirring paddle with shearing function, and the material liquid is in a slurry state as a whole;
[0042] S2. Enzymatic hydrolysis: the material liquid is cooled to 50-55 DEG C, the pH value is adjusted to 7-8, and then the proteinase is added for enzymatic hydrolysis for 0.5-2 hours,
[0043] S3. Oil removal by adsorption: the enzymatic hydrolysis liquid is discharged from the upper part of the extraction tank to the oil removal tank for oil removal by adsorption;
[0044] S4. Ceramic membrane filtration: the material liquid after oil removal by adsorption is collected into the first extraction liquid transfer tank, and then is pumped into the ceramic membrane filter for filtration;
[0045] S5. Cyclic treatment of the ceramic membrane filtration interception liquid: the ceramic membrane filtration interception liquid is backflowed into the second extraction liquid transfer tank, that is, the material liquid in the second extraction liquid transfer tank is introduced into the extraction tank through the bottom water inlet pipe of the extraction tank to perform the enzymatic hydrolysis of step S2; the enzymatic hydrolysis liquid flows into the oil removal tank after passing through the bone particle layer in the extraction tank; the material liquid after oil removal by adsorption is collected into the first extraction liquid transfer tank, and then is pumped into the ceramic membrane filter for filtration, and the generated ceramic membrane filtration interception liquid is continuously circulated and backflowed into the second extraction liquid transfer tank;
[0046] The cyclic treatment is continued until there is no obvious cartilage particle in the liquid material in the second extraction liquid transfer tank, and the material liquid is clear, and then the cyclic treatment is ended;
[0047] During the cyclic treatment, the second extraction liquid transfer tank is added with reverse water to supplement the water loss in the ceramic membrane filtration;
[0048] S6. After the end of the cycle, the second extraction liquid is pumped back to the extraction tank through the reflux pump, the stirring speed of the extraction tank is increased, and after 20-80 minutes, the liquid in the extraction tank is pumped into the self-unloading flat plate centrifuge, the filtrate is collected through the extraction transfer tank, then passes through the carbon removal filter and is added to the cation exchange resin tank, soaked for 2-5 hours, and then pumped into the ultrafiltration liquid transfer tank for subsequent ultrafiltration by the ultrafiltration unit, and the ultrafiltration retentate is the enzymatic bone meal aqueous solution.
[0049] In a preferred embodiment, the device combination further comprises an ultrafiltration transfer tank for collecting the liquid in the extraction tank after the cycle is completed, and an ultrafiltration device for ultrafiltrating the liquid after the cycle is completed, and the ultrafiltration retentate is the enzymatic bone meal after post-treatment.
[0050] The post-treatment refers to (1) concentrating the ultrafiltration retentate to a water content of 50-70%, and then spray drying to obtain the enzymatic bone meal; or (2) concentrating the ultrafiltration retentate to 10%, then adding one time of reverse osmosis water and concentrating to 10% again, then performing alcohol precipitation, dehydration, granulation, drying, and crushing and sieving to obtain the enzymatic bone meal.
[0051] Based on the above process description of the utility model, the device combination is assembled with the conventional nanofiltration membrane concentration unit, nanofiltration device, reverse osmosis equipment, thermal concentration equipment, and various containers for transferring the liquid, etc., to obtain a device combination for co-producing collagen peptide, chondroitin sulfate sodium, and amino acid powder.
[0052] The device combination of the utility model is used for treating animal cartilage to extract enzymatic bone meal,
[0053] Protease: a mixture of 2:1 of neutral protease derived from Bacillus subtilis and alkaline protease. The collagen peptide is detected according to the national standard GB31645;
[0054] Sodium hyaluronate: detected according to QB / T4576-2013;
[0055] The number average molecular weight of chondroitin sulfate sodium is less than 10000, and more than 80%, and the detection method is referred to in the appendix of GB31645;
[0056] Chondroitin sulfate sodium and protein impurities USP (United States Pharmacopoeia): the content of chondroitin sulfate sodium is not less than 90%, and the protein is not more than 6%; the contents of chondroitin sulfate sodium, protein, and sodium hyaluronate in the enzymatic bone meal are detected.
[0057] The results are as follows:
[0058]
[0059] It can be seen that the process based on the animal cartilage produces the sodium chondroitin sulfate with the yield of 5-9%, which is significantly higher than the prior art.
Claims
1. An apparatus set for producing an enzymatic bone powder enriched with low-molecular sodium chondroitin sulfate, characterized by, The extraction tank, the oil removal tank, the first extraction liquid transfer tank, the ceramic membrane filter and the second extraction liquid transfer tank are connected in a closed loop through pipelines to recycle the raw material; The extraction tank is used for stirring, crushing and enzymatic hydrolysis of animal cartilage, has a cylindrical tank body, the lower part of the tank body is conical, a motor is arranged at the top of the tank body, a stirring shaft controlled by the motor is located at the center of the tank body and extends to the conical bottom, a stirring paddle with shearing function is arranged at the lower part of the stirring shaft, and stirring paddles are arranged at the middle and upper parts of the stirring shaft; The bottom cover of the tank body is provided with a bottom water inlet pipe, a valve and an air inlet pipe, and the top of the tank body is provided with a discharge outlet for discharging the enzymatic slurry into the oil removal tank. The liquid inlet of the oil removal tank is connected with the discharge outlet arranged at the upper part of the extraction tank through a pipeline, so that the enzymatic slurry in the extraction tank can be discharged into the oil removal tank for oil removal. The first extraction liquid transfer tank is used for collecting the material liquid after oil removal from the oil removal tank, The ceramic membrane filter is used for filtering the liquid material from the first extraction liquid transfer tank, The second extraction liquid transfer tank is used for collecting the filtered liquid generated by the ceramic membrane filter, and the bottom water inlet pipe of the extraction tank is connected with the second extraction liquid transfer tank through a pipeline, so that the filtered liquid can be returned to the extraction tank through the bottom water inlet pipe by a backflow pump, thereby realizing the recycling of the material liquid.
2. The group of devices according to claim 1, characterized in that, The ultrafiltration transfer tank is used for collecting the material liquid after recycling in the extraction tank, and the ultrafiltration device is used for ultrafiltrating the material liquid after recycling, and the filtered liquid generated by the ultrafiltration is subjected to post-treatment to obtain enzymatic bone powder.
3. The group of devices of claim 1, wherein, The top of the extraction tank is also provided with a feeding hole, an alkali pipe and an acid pipe.
4. The group of devices according to claim 1, characterized in that, From bottom to top, a lower temperature detection pipe, a middle temperature detection pipe and an upper temperature detection pipe are arranged on the side wall of the extraction tank.
5. The group of devices of claim 1, wherein A sampling and analysis pipe and a disinfectant pipe are also arranged on the side wall of the extraction tank.
6. The set of devices according to any of claims 1 to 5, characterized in that The filter membrane parameter of the ceramic membrane filter is 3000 daltons.
7. An extraction tank for producing enzymatic bone meal enriched with low molecular sodium chondroitin sulfate, characterized in that, The extraction tank is used for stirring, crushing and enzymatic hydrolysis of animal cartilage, has a cylindrical tank body, the lower part of the tank body is conical, a motor is arranged at the top of the tank body, a stirring shaft controlled by the motor is located at the center of the tank body and extends to the conical bottom, a stirring paddle with shearing function is arranged at the lower part of the stirring shaft, and stirring paddles are arranged at the middle and upper parts of the stirring shaft; The bottom cover of the tank body is provided with a bottom water inlet pipe, a valve and an air inlet pipe, and the top of the tank body is provided with a discharge outlet for discharging the enzymatic slurry into the oil removal tank.
8. The extraction tank of claim 7, wherein, The top of the extraction tank is also provided with a feeding hole, an alkali pipe and an acid pipe.
9. The extraction tank of claim 7, wherein, From bottom to top, a lower temperature detection pipe, a middle temperature detection pipe and an upper temperature detection pipe are arranged on the side wall of the extraction tank.
10. The extraction tank of claim 7, wherein, A sampling and analysis pipe and a disinfectant pipe are also arranged on the side wall of the extraction tank.