Modified black talc doped zeolite composite particle hemostatic material and preparation method thereof

Abstract

The invention discloses a zeolite composite particle hemostatic material based on modified black talc doping and a preparation method thereof, the hemostatic material is prepared by taking calcium exchange zeolite, modified black talc and seawater pearl powder as raw materials and guar gum as a binder through granulation; wherein the modified black talc is obtained by calcining black talc at 600-900 DEG C for 1-3 hours; the novel composite hemostatic material is designed for the first time by utilizing the characteristics that black talc subjected to high-temperature calcination modification is high in water absorbability and has an obvious inhibition effect on staphylococcus aureus, has the advantages of rapid hemostasis and lasting antibiosis, effectively improves the shortages of a traditional zeolite hemostatic material, and can promote rapid healing of wounds; in addition, the preparation method is simple and convenient, low in raw material cost and very suitable for large-scale industrialized production.

Description

Technical Field

[0001] The invention belongs to the field of medical hemostatic materials, and in particular relates to a zeolite composite particle hemostatic material doped with modified black talc and a preparation method thereof. Background Art

[0002] Traditional hemostatic products, used to treat traumatic bleeding, often face defects such as slow hemostasis, fluctuating effects, easy to induce allergies, residues in the body, and high cost of use. Zeolite, as an emerging hemostatic material, has gradually attracted people's attention due to its excellent hemostatic function, wide application scenarios, and good safety. However, the water absorption performance of zeolite itself is not enough to meet the needs of rapid hemostasis; in addition, pure zeolite materials lack antibacterial ability, cannot effectively promote wound healing, and easily lead to secondary bleeding of unhealed wounds. Therefore, improving the water absorption and antibacterial properties of zeolite hemostatic materials is an important research and development direction in the medical field at this stage.

[0003] Black talc is a natural clay mineral, classified as talc, with organic carbon components interlayered. The amount of organic carbon contained in this mineral is very limited, accounting for only about 2%, which is evenly distributed between the mineral layers in the form of tiny dust. The basic chemical composition of black talc can be simply expressed as Mg 3 Si 4 O 10 (OH) 2 Or 3MgO·4SiO 2 ·H 2 O, its structural feature is a typical 2:1 (TOT) layered structure, that is, two silicon-oxygen tetrahedral layers (T) and one magnesium-oxygen octahedral layer (O) are alternately stacked, so it is also called TOT-type clay mineral. Black talc exhibits excellent water absorption properties. If calcined at a temperature range of 600-800°C, the magnesium element between the layers can be partially exposed, thereby significantly enhancing the inhibitory effect on Staphylococcus aureus and other bacteria.

[0004] The present invention innovatively utilizes the inherent water absorption and antibacterial properties of black talc materials and the high hemostatic properties of zeolite, and for the first time fuses black talc and zeolite to develop a hemostatic material with both excellent hemostatic and antibacterial effects. This not only fills the gap in the research field of black talc-zeolite composite hemostatic materials, but also opens up a new technical path and development direction for the industrial application of the medical and health industry. Summary of the invention

[0005] In view of the problems of slow hemostasis and poor antibacterial performance of existing zeolite hemostatic materials, the present invention provides a zeolite composite particle hemostatic material doped with modified black talc and a preparation method thereof.

[0006] The present invention mixes and granulates the calcined and modified black talc with zeolite, and utilizes the porous structure of zeolite and the multilayer structure of black talc to quickly absorb water, thereby accelerating the hemostasis rate. At the same time, the lasting antibacterial effect of the calcined and modified black talc helps the rapid healing of wounds after hemostasis. In addition, the calcium-exchanged zeolite can release calcium ions, which can participate in the cascade reaction of blood coagulation and promote the generation of thrombin; substances such as taurine and amino acids in seawater pearl powder help to quickly stop bleeding.

[0007] The hemostatic material provided by the invention has the advantages of rapid hemostasis and lasting antibacterial properties.

[0008] The technical solution of the present invention is as follows:

[0009] A zeolite composite particle hemostatic material based on modified black talc is prepared by granulation using calcium exchanged zeolite, modified black talc, seawater pearl powder as raw materials and guar gum as a binder;

[0010] in,

[0011] The mass ratio of calcium exchanged zeolite, modified black talc and seawater pearl powder is 60-80:10-30:1-10;

[0012] The modified black talc is obtained by calcining black talc at 600-900°C for 1-3h.

[0013] The preparation method of the zeolite composite particle hemostatic material based on modified black talc doping of the present invention is as follows:

[0014] (1) Grind the zeolite and add it to CaCl 2 The solution is stirred at 25-60°C for 3-9h, centrifuged, washed with deionized water, and dried (60-80°C) to obtain calcium-exchanged zeolite;

[0015] CaCl is preferred 2 Solution concentration 3~6mol / L;

[0016] CaCl is preferred 2 The volume mass ratio of the solution to the zeolite is 15-35:1, mL / g;

[0017] (2) grinding the black talc and placing it in a muffle furnace, and calcining it at 600-900° C. for 1-3 hours to obtain modified black talc;

[0018] (3) mixing the calcium exchanged zeolite obtained in step (1), the modified black talc obtained in step (2), and seawater pearl powder to obtain a mixed powder; adding the mixed powder to a disc granulator in batches and continuously spraying the guar gum solution for granulation, collecting the composite particles and drying them, and screening the composite particles with a particle size between 0.3 and 0.7 mm, which is the zeolite composite particle hemostatic material doped with modified black talc;

[0019] Calcium exchanged zeolite, modified black talc, and seawater pearl powder are all in powder form, preferably with a particle size of 100 to 150 meshes;

[0020] The preferred mass fraction of the guar gum solution is 0.2 to 1%;

[0021] The preferred volume mass ratio of the guar gum solution to the mixed powder is 0.1-1.5:1, mL / g.

[0022] Compared with the prior art, the advantages of the present invention are:

[0023] The present invention applies modified black talc material to the preparation process of zeolite hemostatic material for the first time, and designs a novel zeolite composite particle hemostatic material doped with modified black talc. The calcined and modified black talc can absorb a large amount of water, thereby effectively promoting the zeolite hemostatic material to quickly absorb water in the blood, thereby achieving the effect of rapid hemostasis. At the same time, the magnesium ions exposed on the surface of the modified black talc can have a long-lasting antibacterial effect, promote wound healing, and prevent secondary bleeding of wounds. The present invention has rapid hemostasis, low heat release, easy-to-obtain materials, low cost, simple preparation, and is suitable for large-scale factory production. DETAILED DESCRIPTION

[0024] The present invention is further described below by specific examples, but the protection scope of the present invention is not limited thereto. For specific conditions not clearly stated in the examples, the conditions recommended by conventional standards or manufacturers should be followed. For reagents or instruments, if the manufacturer is not specified, they are all regarded as conventional commodities that can be purchased on the market.

[0025] In the following embodiments,

[0026] Zeolite was purchased from Lingshou County Jiushun Mineral Products Co., Ltd.;

[0027] Black talc was collected from Guangfeng District, Shangrao City;

[0028] Seawater pearl powder was purchased from Shaanxi Qingmiao Biotechnology Co., Ltd.;

[0029] Guar gum was purchased from Hefei Jushengyuan Biotechnology Co., Ltd.

[0030] Example 1

[0031] Preparation of zeolite-black talc composite hemostatic material: 750g zeolite, 300g black talc, 50g seawater pearl powder were taken, ground, and passed through a 150-mesh sieve. 250g zeolite was added to 5000mL of 5mol / L CaCl 2The solution was stirred at room temperature for 6 hours, centrifuged, and the obtained zeolite powder was washed with deionized water several times and dried at 65°C to obtain calcium exchanged zeolite. The above operation was repeated until all zeolites completed calcium exchange. The black talc powder was calcined at 700°C using a muffle furnace and kept warm for 2 hours to obtain modified black talc. 700g of calcium exchanged zeolite, 250g of modified black talc, and 20g of seawater pearl powder were fully mixed, and one-quarter of the obtained mixed powder was added to a disc granulator to ensure that it was fully dispersed. While continuously spraying 0.5% guar gum solution, the remaining mixed powder was gradually added until 1000mL of guar gum solution was used up, the obtained particles were collected, and dried, and the particles with a particle size between 0.3mm-0.7mm were screened with a 24-mesh sieve and a 48-mesh sieve, respectively, which was the zeolite-black talc composite hemostatic material.

[0032] (1) Hemostatic performance test

[0033] Six healthy domestic pigs of either sex with a weight range of 11–14 kg were included. They were stopped from feeding the day before the experiment, but water was not restricted. The animals were anesthetized by intramuscular injection of 0.3% sodium pentobarbital (30 mg / kg) and then placed in a supine position and fixed on a laboratory table. A longitudinal incision was made from the thyroid cartilage to the sternal notch to expose the trachea and the right carotid artery. The trachea was cut open and a tube was inserted to connect to a ventilator, while the carotid artery was connected to a physiological parameter analysis recorder through a cannula for monitoring arterial blood pressure. At the same time, a puncture was made in the marginal auricular vein to establish an intravenous infusion channel. A 10-cm longitudinal incision was made in the right anterior upper thigh to expose the femoral artery and vein. Lidocaine was used to infiltrate the paravascular muscle tissue to prevent vasospasm. When the arterial blood pressure remained stable for about 5 min, the femoral artery, femoral vein, and quadriceps femoris muscle about 2 cm thick were cut using a scalpel. After 15 minutes of hemostasis measures, anti-shock treatment was started through intravenous infusion, and 250 ml of sodium lactate balanced salt solution was infused within half an hour. The death criteria of animals were zero blood pressure, heartbeat and respiratory arrest. During the 120-minute observation period, the mortality rate and death time distribution of animals (i.e., the survival rate of animals) were recorded. At 20 seconds after the femoral blood vessels were cut off, the experimental group immediately sprinkled 25g of zeolite-black talc composite hemostatic particles on the wound surface of vascular bleeding. If there was still bleeding, 5g was added and gauze was used to apply pressure to stop bleeding.

[0034] Before the blood vessels were cut, gross observation revealed that the diameters of the femoral artery and femoral vein were 3.09±0.21mm and 3.07±0.25mm, respectively. After the blood vessels were cut, the bleeding was jet-like. After the zeolite particles were spread on the wound, the bleeding site gradually bulged, the zeolite particles spread to the surrounding area, and quickly condensed into a thick brown scab. The top of the scab was the location of the cut blood vessel, which was dry and hard in texture and tightly combined with the wound. Before the blood vessels were cut, the animal's arterial blood pressure was 109.42±8.26mmHg. After the blood vessels were cut, the animal's blood pressure immediately dropped sharply to 55.13mmHg. After the hemostatic treatment started from the 20th second after the blood vessels were cut, the animal's blood pressure gradually and continuously increased, reaching normal levels at the 120th minute. During the 120-minute observation period, all animals in the experimental group survived, with a mortality rate of 0%.

[0035] (2) Water absorption performance test

[0036] Water absorption refers to the amount of clean water that the zeolite-black talc composite hemostatic material can completely absorb and retain within a specified time at a specific mass. The instruments required for the experiment include: a 150mL beaker, an electronic scale and a separatory funnel. The experimental steps are as follows: First, accurately weigh 30g of zeolite-black talc composite hemostatic material and place it in a beaker. Next, use a separatory funnel to drip 150mL of warm water into the beaker at a constant rate until water that has not been absorbed by the material is observed and the dripping is stopped. Subsequently, let the mixture stand for 10 minutes, then pour out the suspended liquid part in the beaker, and accurately weigh the weight of the poured liquid, recorded as m grams. This test process needs to be repeated three times. The water absorption of the zeolite-black talc composite hemostatic material is expressed as a mass fraction A, and its value is in the form of a percentage:

[0037] A= 150-m ×100% 30

[0039] Where: m is the weight of the suspended liquid poured out, in grams (g)

[0040] The water absorption rates of zeolite-black talc composite hemostatic materials in three experiments were 141%, 138% and 144% respectively.

[0041] (3) Water absorption temperature rise test

[0042] Pour 75mL of water into a 150mL beaker, then stick a layer of aluminum foil on the outside of the beaker and wrap it tightly with insulation material to ensure that the temperature inside the beaker is not easily lost to the external environment. Use a thermometer to measure and record the water temperature T1 in the beaker at this time. Next, take out 50g of the zeolite-black talc hemostatic material involved in the present invention, add it to 75mL of water, and stir slowly with a thermometer. During this period, record and read the highest temperature T2 reached. This test step needs to be repeated three times. The temperature increase value is calculated according to the following formula:

[0043] △T=T2-T1

[0044] According to tests, the temperature rises of the zeolite-black talc hemostatic material of the present invention are 48° C., 47° C. and 50° C. respectively.

[0045] The experimental results show that the zeolite-black talc hemostatic material of the present invention exhibits excellent hemostatic performance. It can not only quickly stop bleeding, but also keep the temperature rise within an appropriate range during the whole process, ensuring that the survival rate of all tested animals reaches 100%.

[0046] Example 2

[0047] Take 750g zeolite, 350g black talc, 50g seawater pearl powder, grind, and pass through a 150 mesh sieve. Add 250g zeolite to 5000mL of 5mol / L CaCl 2 The solution was stirred at room temperature for 6 hours, centrifuged, and the obtained zeolite powder was washed with deionized water several times and dried at 65°C to obtain calcium exchanged zeolite. The above operation was repeated until all zeolites completed calcium exchange. The black talc powder was calcined at 700°C using a muffle furnace and kept warm for 2 hours to obtain modified black talc. 600g of calcium exchanged zeolite, 300g of modified black talc, and 20g of seawater pearl powder were fully mixed, and one-quarter of the obtained mixed powder was added to a disc granulator to ensure that it was fully dispersed. While continuously spraying 0.5% guar gum solution, the remaining mixed powder was gradually added until 1000mL of guar gum solution was used up, and the obtained particles were collected and dried. The particles with a particle size between 0.3mm-0.7mm were screened with a 24-mesh sieve and a 48-mesh sieve, respectively, which were the zeolite-black talc composite hemostatic material.

[0048] (1) Hemostatic performance test

[0049] Before the blood vessel was cut, it was found through gross observation that the diameters of the femoral artery and femoral vein were 3.12±0.43mm and 3.25±0.16mm, respectively. After the blood vessel was cut, the bleeding was jet-like. After the zeolite particles were spread on the wound, the bleeding site gradually bulged, the zeolite particles spread to the surrounding area, and quickly condensed into a thick brown scab. The top of the scab was the location of the cut blood vessel. Its texture was dry and hard, and it was closely integrated with the wound. Before the blood vessel was cut, the animal's arterial blood pressure was 111.65±6.39mmHg. After the blood vessel was cut, the animal's blood pressure immediately dropped sharply to 58.26mmHg. After the hemostasis treatment started from the 20th second after the blood vessel was cut, the animal's blood pressure gradually and continuously increased, reaching normal levels at the 120th minute. During the 120-minute observation period, all animals in the experimental group survived, with a mortality rate of 0%.

[0050] (2) Water absorption performance test

[0051] The water absorption rates of zeolite-black talc composite hemostatic materials in three experiments were 135%, 142% and 137% respectively.

[0052] (3) Water absorption temperature rise test

[0053] According to tests, the temperature rises of the zeolite-black talc hemostatic material of the present invention are 45° C., 43° C. and 45° C. respectively.

[0054] Example 3

[0055] Take 1000g zeolite, 200g black talc, 50g seawater pearl powder, grind, and pass through a 150-mesh sieve. Add 250g zeolite to 5000mL of 5mol / L CaCl 2 The solution was stirred at room temperature for 6 hours, centrifuged, and the obtained zeolite powder was washed with deionized water several times and dried at 65°C to obtain calcium exchanged zeolite. The above operation was repeated until all zeolites completed calcium exchange. The black talc powder was calcined at 700°C using a muffle furnace and kept warm for 2 hours to obtain modified black talc. 800g of calcium exchanged zeolite, 150g of modified black talc, and 20g of seawater pearl powder were fully mixed, and one-quarter of the obtained mixed powder was added to a disc granulator to ensure that it was fully dispersed. While continuously spraying 0.5% guar gum solution, the remaining mixed powder was gradually added until 1000mL of guar gum solution was used up, and the obtained particles were collected and dried. The particles with a particle size between 0.3mm and 0.7mm were screened with a 24-mesh sieve and a 48-mesh sieve, respectively, which were the zeolite-black talc composite hemostatic material.

[0056] (1) Hemostatic performance test

[0057] Before the blood vessels were cut, gross observation revealed that the diameters of the femoral artery and femoral vein were 2.97±0.32mm and 3.16±0.10mm, respectively. After the blood vessels were cut, the bleeding was jet-like. After the zeolite particles were spread on the wound, the bleeding site gradually bulged, the zeolite particles spread to the surrounding area, and quickly condensed into a thick brown scab. The top of the scab was the location of the cut blood vessel, which was dry and hard in texture and tightly combined with the wound. Before the blood vessels were cut, the animal's arterial blood pressure was 107.63±7.32mmHg. After the blood vessels were cut, the animal's blood pressure immediately dropped sharply to 57.26mmHg. After the hemostatic treatment started from the 20th second after the blood vessels were cut, the animal's blood pressure gradually and continuously increased, reaching normal levels at the 120th minute. During the 120-minute observation period, all animals in the experimental group survived, with a mortality rate of 0%.

[0058] (2) Water absorption performance test

[0059] The water absorption rates of zeolite-black talc composite hemostatic materials in three experiments were 149%, 147% and 150% respectively.

[0060] (3) Water absorption and temperature rise test

[0061] According to tests, the temperature rises of the zeolite-black talc hemostatic material of the present invention are 50° C., 52° C. and 49° C. respectively.

[0062] The applicant declares that the present invention is intended to illustrate an example of a zeolite-black talc hemostatic material through the above-mentioned embodiments, but the application scope of the present invention is not limited to these specific examples, that is, the implementation of the present invention does not depend on the above-mentioned specific embodiments. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of raw materials, addition of auxiliary components, and selection of specific implementation methods, etc., all fall within the scope of protection and disclosure of the present invention.

Claims

1. A hemostatic material based on zeolite composite particles doped with modified black talc, characterized in that: The product is prepared by granulation with calcium exchange zeolite, modified black talc, seawater pearl powder as raw materials and guar gum as a binder; in, The modified black talc is obtained by calcining black talc at 600-900°C for 1-3h.

2. The hemostatic material based on modified black talc-doped zeolite composite particles according to claim 1, characterized in that: The mass ratio of calcium exchange zeolite, modified black talc and seawater pearl powder is 60-80:10-30:1-10.

3. The method for preparing a hemostatic material based on zeolite composite particles doped with modified black talc according to claim 1, characterized in that: The preparation method is as follows: (1) grinding the zeolite and adding it to a CaCl2 solution, stirring at 25-60°C for 3-9 hours, centrifuging, washing with deionized water, and drying to obtain a calcium-exchanged zeolite; (2) grinding the black talc and placing it in a muffle furnace, and calcining it at 600-900° C. for 1-3 hours to obtain modified black talc; (3) Mixing the calcium-exchanged zeolite obtained in step (1), the modified black talc obtained in step (2), and seawater pearl powder to obtain a mixed powder; adding the mixed powder to a disc granulator in batches and continuously spraying the guar gum solution for granulation, collecting the composite particles and drying them, and screening the composite particles with a particle size between 0.3 and 0.7 mm, which is the zeolite composite particle hemostatic material doped with modified black talc.

4. The preparation method according to claim 3, characterized in that: In step (1), the concentration of the CaCl2 solution is 3 to 6 mol / L.

5. The preparation method according to claim 3, characterized in that: In step (1), the volume mass ratio of the CaCl2 solution to the zeolite is 15 to 35:1, mL / g.

6. The preparation method according to claim 3, characterized in that: In step (2), the calcium exchanged zeolite, modified black talc and seawater pearl powder are all in powder form with a particle size of 100 to 150 meshes.

7. The preparation method according to claim 3, characterized in that: In step (2), the mass fraction of the guar gum solution is 0.2-1%.

8. The preparation method according to claim 3, characterized in that: In step (2), the volume mass ratio of the guar gum solution to the mixed powder is 0.1-1.5:1, mL / g.