A bone meal pulverization process
By optimizing the pulverization process parameters and real-time temperature monitoring, the problem of excessive temperature rise during bone meal pulverization was solved, achieving efficient and high-quality bone meal production.
Patent Information
- Application Number
- CN202211308467.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-10-25
- Publication Date
- 2025-11-18
- Estimated Expiration
- 2042-10-25
AI Technical Summary
Bone meal production suffers from problems such as excessive temperature rise during the grinding process, leading to low yield and low grinding efficiency. Furthermore, there is a lack of standardized grinding equipment and monitoring methods.
The optimal grinding amount, single grinding time and number of times were determined through multiple experiments. The temperature of the bone meal was monitored by combining Fourier transform infrared spectroscopy and differential scanning calorimetry to ensure that the grinding was carried out below 40℃. Combined standard sieves were used to separate the particle size and oversized aggregates were circulated for grinding, thus forming an efficient bone meal grinding process.
This improved the yield and grinding efficiency of bone meal, ensuring its quality and performance, and achieving efficient grinding of bone meal.
Smart Images
Figure CN115656029B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of bone powder crushing, in particular to a bone powder crushing process. BACKGROUND
[0002] Bone powder is a powdery bone repair material with fine physical appearance and small particle size, which is suitable for repairing, filling of small volume, irregular, cavity or gap bone defects; or further filling after using block or granular filling to fill the gap and achieve the effect of compact grafting, so as to obtain the microenvironment mechanical stability of the repaired or fused site, thereby facilitating the process of tissue osteogenesis.
[0003] In the process of high-speed crushing of bone powder, temperature rise is an important concern, and excessive temperature rise will adversely affect the crushed bone powder. There is no standard equipment for bone powder crushing, so the bone powder crushing may have problems such as over-crushing, low yield, short single crushing time and low crushing efficiency. SUMMARY
[0004] In view of the above-mentioned defects or deficiencies in the prior art, it is desirable to provide a bone powder crushing process with high crushing efficiency and high yield, which can monitor the crushing temperature of bone powder in real time and ensure the quality of bone powder.
[0005] The present application provides a bone powder crushing process, which comprises the following steps:
[0006] 1) Preparation: a plurality of groups of dry bone blocks with different weights are respectively weighed as a sample for standby, and the single running time of the crusher is set;
[0007] 2) Crushing: a group of a sample is put into the crusher, and the crusher is started to complete a timed crushing process to form a crushing intermediate material;
[0008] 3) Screening: the crushing intermediate material is poured into a combined standard sieve, the combined standard sieve is repeatedly shaken left and right, the bone material with too small particle size, i.e. waste material and oversized bone material, is screened out, the qualified bone material, i.e. bone powder, is collected, and the weight of the bone powder is weighed;
[0009] 4) Recycle crushing: the oversized bone material is put into the crusher, and steps 2)-3) are recycled until the remaining amount of oversized bone material is too small to be crushed;
[0010] 5) Residual sample crushing: the crushing process of the residual a sample is completed according to steps 2)-4);
[0011] 6) Determining the optimal crushing amount: the yield of each group of a sample is calculated as η=M 粉 / M*100%, wherein M 粉M is the weight of the dry weight bone block; the a sample with the highest yield is selected by comparison, and the weight of the a sample is the optimal crushing amount;
[0012] 7) determining the optimal single crushing time: a plurality of different single crushing times are set, a plurality of groups of dry weight bone blocks are weighed according to the optimal crushing amount as b samples for standby, the number of groups of b samples is the same as the set number of single crushing times, each group of b samples corresponds to a single crushing time, the crushing process is completed according to steps 2)-4), the initial temperature and the final temperature of the bone aggregate in each single crushing process are recorded, the temperature rise Δt of the bone aggregate in each single crushing is calculated, and the bone powder after each single crushing is taken as an experimental sample I; the time length t consumed by each group of b samples to complete the crushing is recorded;
[0013] Then, the yield and the crushing efficiency of each group of b samples are calculated, the crushing efficiency α = M 粉 / t; then, Fourier infrared spectrum analysis experiments and differential scanning calorimetry experiments are respectively performed on each group of experimental samples I to detect whether the performance of the experimental sample I is damaged;
[0014] The b sample with the highest crushing efficiency, whose performance is not damaged and whose yield meets the requirements, is selected by comparison, and the single crushing time corresponding to the b sample is the optimal single crushing time;
[0015] 8) determining the optimal crushing number: a group of dry weight bone blocks are weighed according to the optimal crushing amount as c samples for standby, the single running time of the crusher is set according to the optimal single crushing time; the c samples are crushed according to steps 2)-4), and the bone powder after each single crushing is taken as an experimental sample II; the in-vivo implantation experiments are respectively performed on each group of experimental samples II, and the bone formation effect is observed; under the premise that the bone formation effect meets the requirements, the experimental sample II with the largest crushing number is selected, and the crushing number corresponding to the experimental sample II is the optimal crushing number.
[0016] Further, the dry weight bone block is obtained by the following steps: removing, cleaning and freeze-drying a tubular bone taken from a qualified donor, cutting the bone shaft of the tubular bone into bone strips with a width of 5-10 mm along the length direction of the bone shaft, and then cutting the bone strips into bone blocks with a length of 5-10 mm along the transverse direction of the bone strips.
[0017] Further, the crushing of the bone powder is performed in a production-grade clean room with an ambient temperature of 18-25 °C and an air humidity of 45%-65%.
[0018] Further, the combined standard screen comprises an upper standard screen and a lower standard screen, the upper standard screen has a pore size of 1.25 mm, and the lower standard screen has a pore size of 0.05 mm.
[0019] Compared with the prior art, the present application has the following beneficial effects:
[0020] The bone powder crushing process of the present application is aimed at selecting a crusher, through multiple crushing tests, to obtain the best process parameters under the condition of ensuring the performance of the bone powder, form a processing standard to guide the crushing of the bone powder, effectively improve the yield and processing efficiency, and ensure the crushing quality of the bone powder.
[0021] It should be understood that the content described in the summary section is not intended to limit the key or important features of the embodiments of the present application, nor to limit the scope of the present application. Other features of the present application will become apparent through the following description. BRIEF DESCRIPTION OF DRAWINGS
[0022] Other features, objects, and advantages of the present application will become more apparent from the following detailed description of non-limiting embodiments, made with reference to the drawings:
[0023] Figure 1 Flow chart of the bone powder crushing process. DETAILED DESCRIPTION
[0024] The present application will be further described in detail below with reference to the drawings and embodiments. It should be understood that the specific embodiments described herein are merely intended to explain the related application, but not to limit the application. In addition, it should be noted that only the parts related to the application are shown in the drawings for ease of description.
[0025] It should be noted that the embodiments in the present application and the features in the embodiments can be combined with each other without conflict. The present application will be described in detail below with reference to the drawings and embodiments.
[0026] Reference should be made to Figure 1 The embodiments of the present application provide a bone powder crushing process, comprising the following steps:
[0027] 1) Preparation: a plurality of groups of dry bone blocks with different weights are weighed as a sample for standby, and the single running time of the crusher is set;
[0028] 2) Crushing: a group of a samples is put into the crusher, the crusher is started to complete a timed crushing process, and a crushed intermediate material is formed;
[0029] 3) Screening: the crushed intermediate material is poured into a combined standard sieve, the combined standard sieve is repeatedly shaken left and right, the bone material with a particle size too small, i.e. waste material and oversized bone material, is screened out, the qualified bone material, i.e. bone powder, is collected, and the weight of the bone powder is weighed;
[0030] 4) Recycle crushing: the oversized bone material is put into the crusher, and steps 2)-3) are recycled until the remaining amount of the oversized bone material is too small to be crushed;
[0031] 5) The remaining sample is crushed: the crushing process of the remaining a sample is completed according to steps 2)-4);
[0032] 6) Determine the optimal crushing amount: the yield of each group of a sample is calculated η = M 粉 / M*100%, wherein M 粉 is the total weight of bone powder, and M is the weight of dry bone block; the a sample with the highest yield is selected by comparison, and the weight thereof is the optimal crushing amount;
[0033] 7) Determine the optimal single crushing time: a plurality of different single crushing times are set, a plurality of groups of dry bone blocks are weighed as b samples according to the optimal crushing amount, the number of groups of b samples is the same as the number of set single crushing times, each group of b samples corresponds to a single crushing time, the crushing process is completed according to steps 2)-4), the initial temperature and the final temperature of the bone aggregate in each single crushing process are recorded, the temperature rise Δt of the bone aggregate in each single crushing is calculated, and the bone powder after each single crushing is taken as experimental sample I; the time length t consumed by the completion of the crushing of each group of b samples is recorded;
[0034] Then the yield and the crushing efficiency of each group of b samples are calculated, the crushing efficiency α = M 粉 / t; then the Fourier infrared spectrum analysis experiment and the differential scanning calorimetry analysis experiment are respectively performed on each group of experimental sample I to detect whether the performance of the experimental sample I is destroyed;
[0035] The b sample with the highest crushing efficiency and the undestroyed performance and meeting the yield requirement is selected by comparison, and the single crushing time corresponding to the b sample is the optimal single crushing time;
[0036] 8) Determine the optimal crushing number: a group of dry bone blocks are weighed as c samples according to the optimal crushing amount, and the single running time of the crusher is set according to the optimal single crushing time; the c samples are crushed according to steps 2)-4), and the bone powder after each single crushing is taken as experimental sample II; the in-vivo implantation experiment is respectively performed on each group of experimental sample II, and the osteogenesis effect is observed; under the premise that the osteogenesis effect meets the requirement, the experimental sample II with the largest crushing number is selected, and the crushing number corresponding to the experimental sample II is the optimal crushing number.
[0037] In this embodiment, the crusher with an internal diameter of 20 cm is selected, 100 g, 300 g and 500 g of dry bone blocks are weighed as a samples for crushing, and the yield presents: the 500 g group > the 300 g group > the 100 g group, so that 500 g is selected as the optimal crushing amount.
[0038] The single crushing time is set to 1s, 2s, 3s, and 500g of dry bone pieces is weighed in triplicate as sample b, and the crushing test is carried out, and the yield rate is: 1s group>2s group>3s group; the crushing efficiency is: 3s group>2s group>1s group. The yield rate of 1s group and 2s group has little difference, but the yield rate of 3s group is significantly reduced, and the crushing efficiency of 2s group is significantly higher than that of 1s group.
[0039] The degradation performance and degradation degree of bone powder are closely related to the collagen performance in the bone powder. The normal collagen performance is that the bone powder material has a degradation time matching the bone formation speed, the degradation product has good biocompatibility with the environment of the implanted area, and is the guarantee of the osteogenic performance.
[0040] Taking the crushing test of the 2s group as an example: it can be seen from the Fourier infrared spectrum test that the peak positions of the samples I of each group are basically the same, indicating that the chemical components in the bone powder are basically the same.
[0041] The main organic components of bone powder are type I collagen and a small amount of bone morphogenetic protein. The structure thermal stability of type I collagen is analyzed by differential scanning calorimetry, and the breaking of hydrogen bonds inside the collagen protein can be observed at 40.4℃, indicating that the spatial structure of collagen protein is destroyed, but it can be recovered by standing in a 37℃ cooling liquid; at 60℃, the thermal denaturation of collagen is irreversible. The thermal stability of type I collagen is observed by high performance liquid chromatography / mass spectrometry, and it is found that the collagen protein does not change obviously at 40℃; at 50℃, the triple helix structure begins to dissociate, and the single chain does not degrade; at 60℃, irreversible thermal denaturation change occurs, the triple helix structure disappears, and the single chain appears random degradation. Therefore, in the preparation process of bone powder, the destruction of collagen protein caused by friction heat should be avoided, and the temperature should be controlled below 40℃, i.e. max =40℃.
[0042] The temperature change recorded during the crushing process is shown in Table 1:
[0043] Table 1: Temperature change and temperature rise process of bone powder during crushing(℃)
[0044]
[0045] As can be seen from Table 1, the average temperature rise of bone powder caused by crushing is 2.94±0.67℃, and the temperature of bone powder during crushing does not reach t max Therefore, the optimal single crushing time is set to 2s.
[0046] 500 g of the dry bone pieces are weighed as a group as a c sample for standby, and the single crushing time is set as 2 s; the crushing of the bone powder is completed after 13 times of crushing. The bone powder of each time is taken as an experimental sample II, and the in-vivo implantation experiment is carried out respectively, and the influence of the bone powder with different crushing times on the bone implantation performance is evaluated. The manual palpation and X-ray results are taken as the observation indexes in the in-vivo implantation experiment, and the new bone piece size, appearance and the like of the bone powder with different crushing times implanted in the living body are not obviously different in the experiment, so that the optimal crushing time is 13, that is, the different crushing times have no influence on the performance of the bone powder.
[0047] In a preferred embodiment, the dry bone pieces are obtained by cutting the diaphysis of the tubular bone taken from the qualified donor into bone strips with a width of 5-10 mm along the diaphysis length of the tubular bone, and then cutting the bone strips into bone pieces with a length of 5-10 mm along the transverse direction of the bone strips. The low-temperature freeze drying is carried out before the crushing, so that the bone material is fully brittle, the bone material is brittle and loses elasticity, and the crushing effect is improved.
[0048] In a preferred embodiment, the crushing of the bone powder is carried out in a production-grade clean room with an ambient temperature of 18-25℃ and an air humidity of 45%-65%, so as to ensure the crushing quality of the bone powder.
[0049] In a preferred embodiment, the combined standard screen includes an upper standard screen and a lower standard screen, the upper standard screen has a pore size of 1.25 mm, and the lower standard screen has a pore size of 0.05 mm. The bone material with a diameter of 0.05-1.25 mm is qualified bone powder, the bone material smaller than 0.05 mm is waste, and the bone material larger than 1.25 mm needs to be crushed again.
[0050] In the description of the present specification, the description of the terms "one embodiment", "some embodiments", and the like means that the specific features, structures, materials or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present application. In the present specification, the illustrative description of the above terms does not necessarily mean the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.
[0051] The above is only the preferred embodiment of the present application and is not used to limit the present application. For those skilled in the art, the present application can have various modifications and changes. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims
1. A bone meal pulverizing process, characterized in that, Includes the following steps: 1) Preparation: Weigh out multiple groups of dry bone blocks of different weights as sample a for later use, and set the single run time of the pulverizer; 2) Crushing: Place a set of sample a into the crusher, start the crusher to complete one timed crushing process, and form the intermediate crushing material; 3) Screening: Pour the crushed intermediate material into the combined standard sieve, shake the combined standard sieve left and right repeatedly to screen out the aggregate with too small a particle size (i.e., waste material) and the oversized aggregate, and collect the qualified aggregate (i.e., bone meal) and weigh the bone meal. 4) Circulating crushing: Put the oversized aggregate into the crusher and repeat steps 2)-3) in a circulating manner until the remaining amount of oversized aggregate is too small to be crushed further. 5) Grinding the remaining sample: Grind the remaining sample a according to steps 2)-4); 6) Determine the optimal grinding amount: Calculate the yield of each sample in group a, η = M 粉 / M*100%, where M 粉 M represents the total weight of bone meal, and M represents the weight of dry bone blocks. By comparison, sample a, which has the highest yield, is selected, and its weight is the optimal amount of bone meal. 7) Determine the optimal single crushing time: Set multiple different single crushing times, weigh multiple groups of dry weight bone blocks according to the optimal crushing amount as samples b for later use. The number of groups of samples b is the same as the number of single crushing times set. Assign each group of samples b to a single crushing time, and complete the crushing process according to steps 2)-4). Record the initial temperature and final temperature of the aggregate during each single crushing process, and calculate the temperature rise Δt of the aggregate during each single crushing. Take the bone powder after each single crushing as experimental sample I. Record the time t taken for each group of b samples to complete the pulverization process; Then calculate the yield and grinding efficiency of each group of b samples, where grinding efficiency α = M 粉 / t; Then, Fourier transform infrared spectroscopy and differential scanning calorimetry were performed on each group of experimental sample I to detect whether the performance of experimental sample I was damaged. By comparing the experimental sample I, the sample b with the highest pulverization efficiency and the required yield was selected. The corresponding single pulverization time was the optimal single pulverization time. 8) Determine the optimal number of grinding cycles: Weigh a set of dry bone blocks as sample c with the optimal grinding amount, and set the single run time of the grinder to the optimal single grinding time; grind sample c according to steps 2)-4), and take the bone powder after each single grinding as experimental sample II; conduct in vivo implantation experiments on each group of experimental sample II and observe the osteogenic effect; under the premise that the osteogenic effect meets the requirements, select the experimental sample II with the most grinding cycles, and the corresponding grinding cycle is the optimal number of grinding cycles.
2. The bone meal pulverizing process according to claim 1, characterized in that, The dry weight bone block is formed by removing, cleaning and freeze-drying tubular bone taken from qualified donors, then cutting the bone shaft into strips with a width of 5-10 mm along the length of the bone shaft, and then cutting the bone strips into strips with a length of 5-10 mm along the transverse direction of the bone strips.
3. The bone meal pulverizing process according to claim 1, characterized in that, The bone meal is pulverized in a production-grade cleanroom with an ambient temperature of 18–25°C and an air humidity of 45%–65%.
4. The bone meal pulverizing process according to claim 1, characterized in that, The combined standard sieve includes an upper standard sieve and a lower standard sieve. The upper standard sieve has an aperture of 1.25 mm, and the lower standard sieve has an aperture of 0.05 mm.