CN115656029A - Bone meal crushing process - Google Patents
Bone meal crushing process Download PDFInfo
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- CN115656029A CN115656029A CN202211308467.3A CN202211308467A CN115656029A CN 115656029 A CN115656029 A CN 115656029A CN 202211308467 A CN202211308467 A CN 202211308467A CN 115656029 A CN115656029 A CN 115656029A
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Abstract
The invention discloses a bone meal crushing process, which comprises the following steps: 1) Preparing; 2) Crushing; 3) Screening; 4) Circularly crushing; 5) Crushing the rest sample; 6) Determining the optimal crushing amount; 7) Determining the optimal single crushing time; 8) And determining the optimal crushing times. The bone meal crushing process can form crushing standards aiming at non-standard crushing equipment so as to guide the crushing processing of the bone meal, has high crushing efficiency and high yield, and ensures the quality of the bone meal.
Description
Technical Field
The invention relates to the technical field of bone meal crushing, in particular to a bone meal crushing process.
Background
The bone powder is a powdery bone repair material with small physical appearance characteristic particle size, and is suitable for repairing and filling small, irregular and cavity bone defects or gap bone defects; or the block or granular filling is carried out for further filling to fill the gap, so as to achieve the effect of compact bone grafting (compact grafting), obtain the micro-environmental mechanical stability of the repair or fusion part and be beneficial to the tissue osteogenesis process.
The temperature rise of the bone meal during high-speed crushing is an important concern, and too high a temperature rise will have an adverse effect on the crushed bone meal. The crushing of bone meal does not have standard equipment, so the crushing of bone meal can appear smashing too much the yield low, or single crushing time is short, crushing inefficiency problem.
Disclosure of Invention
In view of the above-mentioned defects or shortcomings in the prior art, it is desirable to provide a bone meal pulverizing process which has high pulverizing efficiency and high yield, can monitor the pulverizing temperature of the bone meal in real time and ensure the quality of the bone meal.
The invention provides a bone meal crushing process, which comprises the following steps:
1) Preparing: weighing a plurality of groups of dry weight bone blocks with different weights respectively as a sample a for later use, and setting the single operation time of the crusher;
2) Crushing: putting a group of samples a into a crusher, starting the crusher to finish primary timing crushing treatment to form a crushing intermediate material;
3) Screening: pouring the crushed intermediate material into a combined standard sieve, repeatedly shaking the combined standard sieve left and right, sieving out aggregates with too small particle sizes, namely waste materials and oversized aggregates, collecting qualified aggregates, namely bone meal, and weighing the weight of the bone meal;
4) And (3) circulating crushing: placing the oversized aggregate into a grinder, and circularly repeating the steps 2) -3) until the residual amount of the oversized aggregate is too small to be ground;
5) And (3) crushing the rest samples: respectively finishing the crushing treatment of the rest a samples according to the steps 2) to 4);
6) Determining the optimal crushing amount: calculating the yield eta = M of each group a of samples Powder 100% of/M, wherein M Powder The total weight of the bone powder, M is the weight of dry bone pieces; selecting a sample a with the highest yield through comparison, wherein the weight of the sample a is the optimal crushing amount;
7) Determining the optimal single crushing time: setting a plurality of different single crushing times, weighing a plurality of groups of dry weight bone blocks according to the optimal crushing amount to serve as samples b for later use, wherein the number of the groups of the samples b is the same as the set number of the single crushing times, each group of the samples b corresponds to one single crushing time, finishing crushing treatment according to the steps 2) -4), recording the initial temperature and the final temperature of aggregate in each single crushing process, calculating the temperature rise delta t of the aggregate in each single crushing process, and taking the bone powder after each single crushing as an experimental sample I; recording the time t consumed by each group of samples b for completing crushing;
then, the yield and the crushing efficiency of each group b of samples are calculated, and the crushing efficiency is alpha = M Powder T; respectively carrying out Fourier infrared spectrum analysis experiments and differential scanning calorimetry analysis experiments on each group of experimental samples I, and detecting whether the performance of the experimental samples I is damaged;
the crushing efficiency of the samples b with undamaged performance and qualified rate meeting the requirements is highest by comparison, and the corresponding single crushing time is the optimal single crushing time;
8) Determining the optimal crushing times: weighing a group of dry weight bone blocks as a sample c for later use according to the optimal crushing amount, and setting the single running time of the crusher according to the optimal single crushing time; finishing crushing treatment on the sample c according to the steps 2) to 4), and taking the bone meal subjected to single crushing each time as an experimental sample II; respectively carrying out in-vivo implantation experiments on each group of experimental samples II, and observing osteogenesis effects; and on the premise that the osteogenesis effect meets the requirement, selecting the experimental sample II with the largest crushing times, wherein the corresponding crushing times are the optimal crushing times.
Further, the dry weight bone block is formed by removing, cleaning and freeze-drying the tubular bone from the qualified donor, cutting the backbone into bone strips with the width of 5-10 mm along the length direction of the backbone of the tubular bone, and cutting the bone strips into bone strips with the length of 5-10 mm along the transverse direction of the bone strips.
Further, the bone meal is crushed in a production-grade clean room with the ambient temperature of 18-25 ℃ and the air humidity of 45-65%.
Further, the combined standard sieve comprises an upper standard sieve and a lower standard sieve, wherein the aperture of the upper standard sieve is 1.25mm, and the aperture of the lower standard sieve is 0.05mm.
Compared with the prior art, the invention has the beneficial effects that:
the bone meal crushing process provided by the invention aims at the selected crusher, obtains the optimal process parameters under the condition of ensuring the bone meal performance through a plurality of groups of crushing tests, forms a processing standard for guiding the bone meal crushing, effectively improves the yield and the processing efficiency, and ensures the crushing quality of the bone meal.
It should be understood that the statements herein reciting aspects are not intended to limit the critical or essential features of any embodiment of the invention, nor are they intended to limit the scope of the invention. Other features of the present invention will become apparent from the following description.
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Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments made with reference to the following drawings:
FIG. 1 is a flow chart of a bone meal pulverizing process.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant invention and not restrictive of the invention. It should be noted that, for convenience of description, only the portions related to the present invention are shown in the drawings.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
Referring to fig. 1, an embodiment of the present invention provides a bone meal pulverizing process, including the following steps:
1) Preparing: weighing a plurality of groups of dry weight bone blocks with different weights respectively as a sample a for later use, and setting the single operation time of the crusher;
2) Crushing: putting a group of samples a into a crusher, and starting the crusher to finish primary timing crushing treatment to form a crushing intermediate material;
3) Screening: pouring the crushed intermediate material into a combined standard sieve, repeatedly shaking the combined standard sieve left and right, sieving out aggregates with too small particle sizes, namely waste materials and oversized aggregates, collecting qualified aggregates, namely bone meal, and weighing the weight of the bone meal;
4) And (3) circulating crushing: placing the oversized aggregate into a grinder, and circularly repeating the steps 2) -3) until the residual amount of the oversized aggregate is too small to be ground;
5) Crushing the rest samples: respectively finishing the crushing treatment of the rest a samples according to the steps 2) to 4);
6) Determining the optimal crushing amount: calculating the yield eta = M of each group a of samples Powder 100% of/M, wherein M Powder The total weight of the bone powder, M is the weight of dry bone pieces; selecting a sample a with the highest yield through comparison, wherein the weight of the sample a is the optimal crushing amount;
7) Determining the optimal single crushing time: setting a plurality of different single crushing times, weighing a plurality of groups of dry weight bone blocks according to the optimal crushing amount to serve as b samples for later use, wherein the group number of the b samples is the same as the set number of the single crushing times, corresponding each group of the b samples to one single crushing time, completing crushing treatment according to the steps 2) -4), recording the initial temperature and the final temperature of aggregate in each single crushing process, calculating the temperature rise delta t of the aggregate in each single crushing, and taking the bone powder after each single crushing as an experimental sample I; recording the time t consumed by each group b of samples for completing crushing;
then, the yield and the crushing efficiency of each group b of samples are calculated, and the crushing efficiency is alpha = M Powder T; respectively carrying out Fourier infrared spectrum analysis experiments and differential scanning calorimetry analysis experiments on each group of experimental samples I, and detecting whether the performance of the experimental samples I is damaged;
the crushing efficiency of the samples b with undamaged performance and qualified rate meeting the requirements is highest by comparison, and the corresponding single crushing time is the optimal single crushing time;
8) Determining the optimal crushing times: weighing a group of dry weight bone blocks as a sample c for later use according to the optimal crushing amount, and setting the single running time of the crusher according to the optimal single crushing time; finishing crushing treatment on the sample c according to the steps 2) to 4), and taking the bone meal subjected to single crushing each time as an experimental sample II; respectively carrying out in-vivo implantation experiments on each group of experimental samples II, and observing osteogenesis effects; and on the premise that the osteogenesis effect meets the requirement, selecting the experimental sample II with the largest crushing times, wherein the corresponding crushing times are the optimal crushing times.
In this example, a crusher with an inner diameter of 20cm was selected, 100g, 300g, and 500g of dry weight bone pieces were weighed as a sample and crushed, and the yield showed: 500g >300g >100g, thus 500g was chosen as the optimum crushing amount.
Setting single crushing time as 1s, 2s and 3s, weighing three parts of dry weight bone blocks of 500g as a sample b, and respectively carrying out crushing tests, wherein the yield shows that: 1s group >2s group >3s group; the crushing efficiency is: 3s group >2s group >1s group. The yield difference between the 1s group and the 2s group is not large, but the 3s group yield is obviously reduced, and the crushing efficiency of the 2s group is obviously higher than that of the 1s group.
The degradation performance and the degradation degree of the bone meal are closely related to the collagen property in the bone meal. The normal collagen properties are: the bone meal material has degradation time and degradation products matched with bone formation speed, has good biocompatibility with the environment of an implanted area, and is a guarantee for exerting the bone formation performance.
Taking the 2s set of crushing tests as an example: as can be seen by Fourier infrared spectrum tests, the peak positions of the experimental samples I are basically consistent, which indicates that the chemical components in the bone meal are basically the same.
The main organic components of bone meal are type I collagen and a small amount of bone morphogenetic protein. The structural thermal stability of the type I collagen is analyzed through micro differential thermal scanning, and the fracture of hydrogen bonds in the collagen can be observed at 40.4 ℃, which shows that the space structure of the collagen is damaged, but the collagen can be restorable through the standing of cooling liquid at 37 ℃; the thermal denaturation of collagen at 60 ℃ was not reversible. The thermal stability of the type I collagen is observed by utilizing a high performance liquid chromatography/mass spectrometry combined technology, and the collagen is not obviously changed at 40 ℃; the dissociation of triple helix structure at 50 ℃ and single strandDegradation occurs, and the cooling can realize the renaturation of the triple-helix structure; until 60 ℃, irreversible thermal denaturation change begins to appear, the triple helix structure disappears, and the single strand is randomly degraded. Therefore, the temperature should be controlled below 40 deg.C, i.e. t, during the preparation of bone meal without damaging collagen due to friction heat accumulation max ＝40℃。
The temperature changes recorded during comminution are given in table 1 below:
table 1: temperature change and temperature rise process (DEG C) in 2s group bone meal crushing process
As can be seen from Table 1, the average temperature rise of the bone meal due to the crushing is 2.94 +/-0.67 ℃, and the temperature of the bone meal does not reach t in the crushing process max Therefore, the optimum single pulverization time was set to 2s.
Weighing a group of 500g dry weight bone blocks as a sample c for later use, and setting the single crushing time to be 2s; the bone meal is crushed for 13 times. And taking the bone meal of each time as an experimental sample II, respectively carrying out in-vivo implantation experiments, and evaluating the influence of the bone meal of different crushing times on bone implantation performance through the in-vivo implantation experiments. In the in-vivo implantation experiment, the results of manual palpation and X-ray radiation are used as observation indexes, and the sizes, appearances and the like of new bone blocks implanted into a living body by the bone powder with different crushing times have no obvious difference in the experiment, so that the optimal crushing time is 13, namely the different crushing times have no influence on the bone powder performance.
In a preferred embodiment, the dry weight bone block is formed by removing, cleaning and freeze-drying tubular bones from qualified donors, cutting the backbone into bone strips with the width of 5-10 mm along the length direction of the backbone of the tubular bones, and cutting the bone strips into bone strips with the length of 5-10 mm along the transverse direction of the bone strips. The bone material is subjected to low-temperature freeze drying before crushing, so that the bone material is sufficiently embrittled, becomes brittle and loses elasticity, is easy to crush, and improves the crushing effect.
In a preferred embodiment, the crushing of the bone meal is carried out in a production-grade clean room with the ambient temperature of 18-25 ℃ and the air humidity of 45-65%, so that the crushing quality of the bone meal is ensured.
In a preferred embodiment, the combination standard screen comprises an upper standard screen and a lower standard screen, the upper standard screen has a pore size of 1.25mm, and the lower standard screen has a pore size of 0.05mm. The aggregate with the diameter of 0.05-1.25mm is qualified bone meal, the aggregate with the diameter of less than 0.05mm is waste, and the aggregate with the diameter of more than 1.25mm needs to be crushed again.
In the description of the present application, the description of the terms "one embodiment," "some embodiments," etc. means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the application. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. 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 (4)
1. The bone meal crushing process is characterized by comprising the following steps:
1) Preparing: weighing a plurality of groups of dry weight bone blocks with different weights respectively as a sample a for later use, and setting the single operation time of the crusher;
2) Crushing: putting a group of samples a into a crusher, starting the crusher to finish primary timing crushing treatment to form a crushing intermediate material;
3) Screening: pouring the crushed intermediate material into a combined standard sieve, repeatedly shaking the combined standard sieve left and right, sieving out aggregates with too small particle sizes, namely waste materials and oversized aggregates, collecting qualified aggregates, namely bone meal, and weighing the weight of the bone meal;
4) Circulating crushing: placing the oversize aggregate into a grinder, and circularly repeating the steps 2) -3) until the surplus of the oversize aggregate is too small to be ground;
5) Crushing the rest samples: respectively finishing the crushing treatment of the rest a samples according to the steps 2) to 4);
6) Determining the optimal crushing amount: calculating the yield eta = M of each group a of samples Powder 100% of/M, wherein M Powder The total weight of the bone powder, M is the weight of dry bone pieces; selecting a sample a with the highest yield through comparison, wherein the weight of the sample a is the optimal crushing amount;
7) Determining the optimal single crushing time: setting a plurality of different single crushing times, weighing a plurality of groups of dry weight bone blocks according to the optimal crushing amount to serve as b samples for later use, wherein the group number of the b samples is the same as the set number of the single crushing times, corresponding each group of the b samples to one single crushing time, completing crushing treatment according to the steps 2) -4), recording the initial temperature and the final temperature of aggregate in each single crushing process, calculating the temperature rise delta t of the aggregate in each single crushing, and taking the bone powder after each single crushing as an experimental sample I; recording the time t consumed by each group b of samples for completing crushing;
then, the yield and the crushing efficiency of each group b of samples are calculated, and the crushing efficiency is alpha = M Powder T; respectively carrying out Fourier infrared spectrum analysis experiments and differential scanning calorimetry analysis experiments on each group of experimental samples I, and detecting whether the performance of the experimental samples I is damaged;
the crushing efficiency of the samples b with undamaged performance and qualified rate meeting the requirements is highest by comparison, and the corresponding single crushing time is the optimal single crushing time;
8) Determining the optimal crushing times: weighing a group of dry weight bone blocks as a sample c for later use according to the optimal crushing amount, and setting the single running time of the crusher according to the optimal single crushing time; finishing crushing treatment on the sample c according to the steps 2) to 4), and taking the bone meal subjected to single crushing each time as an experimental sample II; respectively carrying out in-vivo implantation experiments on each group of experimental samples II, and observing osteogenesis effects; and on the premise that the osteogenesis effect meets the requirement, selecting the experimental sample II with the largest crushing times, wherein the corresponding crushing times are the optimal crushing times.
2. The bone meal crushing process according to claim 1, wherein the dry-weight bone pieces are formed by removing, cleaning and freeze-drying tubular bones from qualified donors, cutting the backbones into bone strips with the width of 5-10 mm along the length direction of the backbones of the tubular bones, and cutting the bone strips into bone strips with the length of 5-10 mm along the transverse direction of the bone strips.
3. The bone meal crushing process according to claim 1, wherein the crushing of the bone meal is performed in a production-grade clean room with an ambient temperature of 18-25 ℃ and an air humidity of 45-65%.
4. The bone meal crushing process according to claim 1, characterized in that the combined standard sieve comprises an upper standard sieve and a lower standard sieve, the upper standard sieve having a pore size of 1.25mm and the lower standard sieve having a pore size of 0.05mm.
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