Polybasic aluminum chloride, dynamic water balance wet sterilization dressing, and preparation methods therefor

Abstract

Disclosed in the present invention are a polybasic aluminum chloride, a dynamic water balance wet sterilization dressing, and preparation methods therefor, relating to the technical field of dressings. Provided in the present invention is a dynamic water balance wet sterilization dressing, comprising components such as polybasic aluminum chloride and deionized water. According to the present invention, liquid high polybasic aluminum chloride particles are used as a substrate of a dressing combination, and water is used as a dispersant to form a dynamic water balance wet sterile dressing, which can form a uniform, complete, and continuous aqueous film layer on the surface of the skin and on the surface of exposed wound tissues, the thickness of the film layer being greater than 10 microns. The substrate always maintains saturated water content in an ordinary earth's surface environment, and the water content automatically changes with changes in parameters such as ambient temperature, humidity, and air pressure.

Description

Polymeric basic aluminum chloride, dynamic water balance wet sterilization dressing and preparation method thereof TECHNICAL FIELD

[0001] The present application relates to the technical field of dressing, in particular to a polymeric basic aluminum chloride, dynamic water balance wet sterilization dressing and a preparation method thereof. BACKGROUND

[0002] Dressing is an isolation material applied to the wound surface after body surface trauma. Since the establishment of microbiology, the main function of dressing is to isolate infectious pathogens in the environment, obtain non-infectious wounds, and provide a basic physical barrier for the wound to prevent secondary trauma or aggravate the wound. Common dressing products are rich in variety, generally composed of various functional materials, including fiber textile materials, hydrogel materials, liquid film-forming materials, antibacterial and bacteriostatic materials, etc.

[0003] Existing dressing products can be roughly divided into two categories: hydrophilic isolation and hydrophobic isolation. The material matrix of hydrophilic isolation products exhibits hydrophilicity, high tissue affinity, direct contact with wound tissue, and even can become a tissue scaffold structure in the wound healing process. Typical materials include collagen hydrogel dressing; this type of material generally does not have antibacterial properties and needs to add antibacterial materials to form a functional composite, which cannot prevent passive dehydration of the wound. Hydrophobic isolation materials are more widely used and have been the main clinical dressing tool for a long time. Hydrophobic isolation dressing generally uses oily materials as hydrophobic functional materials to directly cover the wound or be combined with carrier materials, such as absorbent cotton sheets loaded with vaseline, animal fats, beeswax, etc. Hydrophobic dressing can partially isolate infectious sources in the environment and reduce passive dehydration of the wound. Physiologically, the source of body surface trauma pain, in addition to physical damage to the wound, mainly includes infection and passive dehydration of exposed tissue. One of the current clinical medical regulations for body surface trauma is to prohibit the wound from contacting water; preventing wound wetness is also a long-standing and widely accepted common sense and even a standard. Existing dressing technology and products cannot simultaneously have high-efficiency anti-infection function and automatic water balance function of the wound.

[0004] Obtaining a dynamic water balance non-infectious wound with permanent moisture will be a substantial progress in dressing technology and products, and may also be a substantial progress in general anti-infection technology.

[0005] SUMMARY

[0006] Therefore, the present application aims to overcome the shortcomings of the prior art and provide a polymeric basic aluminum chloride, dynamic water balance wet sterilization dressing and a preparation method thereof.

[0007] To achieve the above object, the technical scheme adopted by the present application is as follows: a preparation method of polymeric basic aluminum chloride, comprising the following steps:

[0008] (1) The mixed crystal phase fumed alumina nanopowder is mixed with deionized water to obtain a first reactant, and a chlorine source material is added; the molar ratio of aluminum element to chlorine element is (0.9-1):3; the mass ratio of deionized water used for dispersing the alumina powder to the alumina powder is (4.5-5.0):1;

[0009] (2) The first reactant is heated to boiling under one standard atmosphere, and the volume is reduced by evaporation to foam the whole, and the foamed material is heated to no free water at 100-110°C to obtain a second reactant;

[0010] (3) The second reactant is diluted to 1 liter with deionized water, stirred and mixed uniformly, then centrifuged to remove the precipitate to obtain a third reactant; the third reactant is a light yellow clear sol system, which is a clear sol system composed of polybasic aluminum chloride (〔Al2(OH) n Cl (6-n) 〕 m ), residual chlorine source material, alumina crystal particles and water;

[0011] (4) The third reactant is heated to boiling under one standard atmosphere, and the boiling state is maintained until a film appears on the surface of the system, the system is turbid, and then foaming occurs again, and the heating is stopped to obtain a bright orange system;

[0012] (5) The bright orange system is left to stand or centrifuged to remove the precipitate to obtain a yellow clear thick matrix finished product, i.e. the polybasic aluminum chloride.

[0013] The application provides a granular liquid polybasic aluminum chloride, which is infinitely miscible with water and keeps granular form. The polybasic aluminum chloride has the following advantages: (1) the granular liquid polybasic aluminum chloride is hygroscopic, and the water content of the material changes with the relative humidity and temperature of air when the material is in liquid state, and keeps dynamic balance with the environment. The boiling point of the material is higher than that of water, and the material does not evaporate and disperse in the ground surface environment. (2) The granular liquid polybasic aluminum chloride has strong hygroscopicity in the common natural environment on the ground surface, and is connected by water molecules between the particles to form a continuous aqueous film layer. The particle size is normally distributed in the range of 0.01-4.0 microns, and the dynamic multi-layer particle structure is easy to form dense accumulation. In the general ground habitable environment, the granular material is accumulated on the wound to form a viscous flexible isolation layer, and the layer thickness can be dynamically maintained at about 5-100 microns. The viscous flexible film layer has conformability, allows the relative displacement of different parts of the wound and keeps the film layer intact. (3) The melting point of the liquid high-polybasic aluminum chloride particle material is about -150 DEG C, and the specific surface area of the water-soluble liquid micro-nano particle material is difficult to directly measure under the current technical conditions. According to the normal distribution data of the particle size, the liquid high-polybasic aluminum chloride particle material has a specific surface area of more than 50 square meters per square meter. 3

[0014] Preferably, in the step (1), the mass percentage of each crystal form in the mixed crystal form gas phase alumina nano powder is determined by XRD as follows: the mass percentage of theta crystal form is about 79.71%, the mass percentage of alpha crystal form is 0.1014%, the mass percentage of gamma crystal form is about 19.97%, and the mass percentage of eta crystal form is 0.227%; the average particle size of the mixed crystal form gas phase alumina nano powder is 4-5 microns; and the chlorine source material is at least one of hydrogen chloride and titanium chloride.

[0015] Further preferably, the average particle size of the mixed crystal form gas phase alumina nano powder is 4.43016 microns; and the chlorine source material is hydrogen chloride.

[0016] Preferably, the average particle size of the polybasic aluminum chloride is 105-115 nm, the D50 particle size is 340-360 nm, and the D90 particle size is 3630-3650 nm; preferably, the average particle size of the polybasic aluminum chloride is 111.8 nm, the D50 particle size is 349 nm, and the D90 particle size is 3640 nm.

[0017] Preferably, the particle size detection result of the polybasic aluminum chloride is obtained by using the particle size distribution laser diffraction method for testing according to GB / T19077-2016. ​

[0018] The application provides the granular liquid polymeric basic aluminum chloride prepared by the preparation method of the polymeric basic aluminum chloride.

[0019] The application provides application of the polymeric basic aluminum chloride in preparation of a dynamic water balance wet sterilization dressing.

[0020] The application provides a dynamic water balance wet sterilization dressing, which comprises the following components: the polymeric basic aluminum chloride and deionized water; and the volume fraction of the polymeric basic aluminum chloride is 10-20%.

[0021] The application provides a dynamic water balance wet sterilization dressing, which comprises the following components: the polymeric basic aluminum chloride, oxide powder and deionized water; and the volume fraction of the polymeric basic aluminum chloride is 2.0-5.0%.

[0022] Preferably, the oxide powder is at least one of titanium oxide, zinc oxide, aluminum oxide and bismuth oxide.

[0023] The application further provides a preparation method of the dynamic water balance wet sterilization dressing, which comprises the following steps: dissolving the polymeric basic aluminum chloride in deionized water, and obtaining the dynamic water balance wet sterilization dressing after constant volume.

[0024] The application further provides a preparation method of the dynamic water balance wet sterilization dressing, which comprises the following steps:

[0025] S1, dissolving the polymeric basic aluminum chloride in deionized water, adding oxide powder, uniformly mixing, and obtaining a clear and transparent dressing matrix;

[0026] S2, dissolving the dressing matrix in deionized water, adding titanium oxide powder dispersed in deionized water, using deionized water to constant volume to 1 liter, and obtaining the dynamic water balance wet sterilization dressing.

[0027] The application uses granular liquid high polybasic aluminum chloride as the matrix of dressing combination, adds oxide powder with water as dispersant to form dynamic water balance wet sterile dressing. The material mixed by matrix material and deionized water in proportion is also high efficiency dressing product without adding other oxide particles as functional strengthening component. The above-mentioned dressing matrix is the product of specific process, forms stable sol with water, the colloidal particle size range is about 10-4000 nanometers, can form uniform, complete and continuous aqueous film layer on the skin surface and exposed wound tissue surface, the film layer thickness is greater than 10 microns. The matrix always keeps saturated water under ordinary ground surface environment, the water content automatically changes with the change of environmental temperature, humidity, air pressure and other parameters. The matrix is prepared by continuous hydrolysis, polymerization and purification process. The gas phase method nanometer alumina powder is used as aluminum source, the chlorine source material is introduced, the reaction is carried out in boiling aqueous normal pressure environment, after two times of impurity removal, the granular liquid polybasic aluminum chloride polymer with high polymerization degree is obtained, the polymer can form stable and homogeneous solution with water, the polybasic aluminum chloride in the solution maintains granular state, the rated amount of oxide particles can be added in the solution to form sol without aggregation.

[0028] The interaction between the polybasic aluminum chloride of the application and the wound surface is an important link for realizing the function of the dressing. On the one hand, the fresh wound (open wound, skin damage, tissue exposure) after hemostasis exists tissue exudate, exudate, serum, electrolyte and easily cross-linked hydrophilic protein, peptide and other substances, which can easily form an aqueous complex with the polybasic aluminum chloride of the application. The aqueous complex forms an inert isolation layer on the wound surface. On the other hand, the surface of the polybasic aluminum chloride particles is a water film layer, which does not induce immune recognition. The aqueous complex formed by the polybasic aluminum chloride and the wound exudate is deposited and adhered on the surface of the fresh wound, and forms a physiological inert isolation layer without immune recognition effect; the inert isolation layer is solidified on the surface of the active tissue of the wound base due to the immune and metabolism of the tissue, and forms a dense inert isolation layer, which can be considered as a pseudo-skin isolation tissue; the newly added liquid high polybasic aluminum chloride film layer on the inert isolation layer and the composite structure formed by the base inert layer ensure that the wound is not invaded by biological invaders, and infection is not caused.

[0029] The application also provides the application of the dynamic water balance wet sterile dressing in the field of medical devices and medical consumables.

[0030] Compared with the prior art, the beneficial effects of the present invention are as follows: (1) The dynamic water balance wet sterilization dressing is an oxide quantum dot hydrosol composite material. This material acts directly on the surface of the wound tissue to form a tissue denaturation isolation membrane. The hydrosol material added to the membrane evaporates and dehydrates naturally to form a sterile water film structure. This structure maintains a dynamic balance of water content in an open environment. The oxide quantum dot material contained in the membrane has a photothermal catalytic sterilization function, thereby obtaining a permanently moist sterile wound. The wet sterile wound, while free from infection, does not cause passive dehydration of adjacent tissues, which can greatly reduce pain and achieve the goal of reliable sterile and painless wound management. As a wound dressing, this type of material does not induce drug resistance, does not distinguish the biological type and state of the infection source, is not consumed or lost during the sterilization process, is not absorbed by the tissue and maintains physiological inertness, is non-toxic, and has the same extremely high adsorption, isolation and killing efficiency for all biological types and states (including spores). (2) The principle of achieving dynamic water balance in the air is related to the hygroscopicity of chloride salts. When applied to animal husbandry or human health, this material can be used as a direct aqueous dressing for aseptic management and water balance management of wounds on the body surface. No bandaging is required, and the wound is painless. This material can be used for large-scale population epidemic prevention and control. It can effectively kill microbial pathogens from any infectious environmental source, including spores, sporozoites, bacteria, viruses, fungi, mycoplasma, etc., without inducing drug resistance. Attached Figure Description

[0031] Figure 1 shows the microscope morphology of the matrix product prepared in Example 1;

[0032] Figure 2 shows the particle size distribution of DLS nanoparticles, where (a) is the particle size-particle number fraction curve; (b) is the particle size-particle volume fraction curve; and (c) is the particle size-light scattering intensity fraction curve.

[0033] Figure 3 shows the recovery status of mice after dorsal skin removal surgery. (a) shows the recovery status of mice 6 hours after surgery; (b) shows the recovery status of mice 24 hours after surgery; (c) shows the recovery status of mice 36 hours after surgery; (d) shows the recovery status of mice 48 hours after surgery; and (e) shows the recovery status of mice 80 hours after surgery. Detailed Implementation

[0034] To better illustrate the purpose, technical solution, and advantages of this invention, the invention will be further described below with reference to the accompanying drawings and specific embodiments. Unless otherwise specified, the experimental methods used in the embodiments are conventional methods, and the materials and reagents used are commercially available unless otherwise specified.

[0035] The mass percentage of each crystal form in the mixed crystal form fumed aluminum oxide nanopowder used in the application is as follows: the mass percentage of theta crystal form is about 79.71%, the mass percentage of alpha crystal form is 0.1014%, the mass percentage of gamma crystal form is about 19.97%, and the mass percentage of eta crystal form is 0.227%; the mass percentage of each crystal form is the factory detection data of the manufacturer, and the conditions of batch production may have slight fluctuations, and each batch of product detection may have corresponding differences.

[0036] Example 1

[0037] 1. Preparation of materials. Take 100 grams of mixed crystal form fumed aluminum oxide nanopowder, 1 liter of 6 mol / L hydrochloric acid aqueous solution, and 500 milliliters of deionized water.

[0038] 2. Dissolution and acidification. After thoroughly mixing the aluminum oxide powder with pure water, stir and add hydrochloric acid to obtain the first reactant.

[0039] 3. Cracking and polymerization reaction. Heat the first reactant to boiling under one standard atmosphere, and evaporate and reduce the volume to foaming of the whole, and heat the foaming material to no free water at 100-110 DEG C.

[0040] 4. First impurity removal. The reaction system after cracking and polymerization reaction is diluted to 1 liter with deionized water, stirred and mixed, centrifuged, and the precipitate is removed to obtain a light yellow clear liquid, and the first impurity removal is completed. The product obtained is a light yellow clear sol system composed of polybasic aluminum chloride (Al2(OH) n Cl (6-n) ] m ), residual hydrogen chloride, aluminum oxide crystal particles and water.

[0041] 5. Acid removal and purification reaction. Heat the obtained hydrosol system to boiling under one standard atmosphere, maintain the boiling state, and stop heating after film-like material appears on the surface of the hydrosol system, the system becomes turbid, and foaming occurs again.

[0042] 6. Second impurity removal. The reaction system after acid removal and purification reaction appears bright orange, and the precipitate is removed by standing or centrifugation to obtain a yellow clear thick matrix finished product.

[0043] Subsequent dressing preparation, all taking the preparation of 1 liter of dressing product as an example.

[0044] Application Example 1 (preparation of dressing finished product with addition of other oxide particles)

[0045] 1. Preparation of materials. Take 20 grams of the polymer matrix prepared in the foregoing process, 0.8 grams of zinc oxide powder with an average particle size of about 30 nanometers, 0.8 grams of titanium oxide powder with an average particle size of 3-5 nanometers, and 1 liter of deionized water.

[0046] 2. Preparation of the dressing matrix. The polymer matrix is added to deionized water, and the volume is made up to 150 mL; the zinc oxide powder is mixed uniformly to obtain a clear and transparent dressing matrix.

[0047] 3. Volume making up. The aforementioned dressing matrix is added to deionized water, and the volume is made up to 800 mL; the titanium dioxide powder is dispersed in deionized water, and the volume is made up to 100 mL. After the obtained titanium dioxide sol is mixed with the dressing matrix sol, deionized water is added, and the volume is made up to 1 L, which is the finished product of the dressing.

[0048] Application Example 2 (Preparation of the finished product of the dressing without adding other oxide particles)

[0049] 1. 100 mL of the polymer matrix prepared in the foregoing procedure is taken;

[0050] 2. Deionized water is added, and the volume is made up to 1 L.

[0051] Performance Test 1 Microscopic observation.

[0052] Test method: 10% by volume of the finished product of the dressing, i.e., the finished product of the dressing without adding other oxide particles in Application Example 2, is taken, and the inverted microscope is used at 800 times magnification for microscopic observation.

[0053] Test result: The result is shown in FIG. 1, which is a microscopic morphology diagram of the finished product of the matrix prepared in Example 1. The morphology that can be visually distinguished under the microscope is micron-sized particles, which are dispersed and less aggregated.

[0054] Performance Test 2 DLS nanoparticle size distribution.

[0055] Test method: Referring to GB / T 19077-2016 “Particle Size Distribution-Laser Light Diffraction Method”.

[0056] Test result: FIG. 2 is a DLS nanoparticle size distribution diagram, wherein (a) is a particle size-particle number fraction curve diagram; (b) is a particle size-particle volume fraction curve diagram; and (c) is a particle size-light scattering intensity fraction curve.

[0057] The average particle size of the polybasic aluminum chloride is 111.8 nm, the PDI polydispersity index is 0.93, the D5 particle size is 14 nm, the D10 particle size is 16.9 nm, the D50 particle size is 349 nm, and the D90 particle size is 3640 nm.

[0058] Performance Test 3

[0059] Test method: The mouse back skinning operation is performed in an open indoor environment under non-laboratory clean conditions, and the subsequent feeding and observation environment is an open indoor environment, without using antibiotics, antiviral drugs, and antifungal drugs, and without operating environmental disinfection and sterilization, etc.

[0060] Immediately after surgery, the wound surface was irrigated and covered with a 10% by volume balance sol sol sol (base dressing) and maintained every 12 hours 2.0 milliliters dressing increase coverage, throughout the use of water to clean the wound surface.

[0061] Test results: the observed results as shown in Figure 3.

[0062] Figure 3 is a mouse back skinning surgery recovery chart, wherein (a) is a mouse recovery chart 6 hours after surgery, visually no infection; (b) is a mouse recovery chart 24 hours after surgery, visually no infection; (c) is a mouse recovery chart 36 hours after surgery, visually no infection; (d) is a mouse recovery chart 48 hours after surgery, visually no infection; (e) is a mouse recovery chart 80 hours after surgery, visually no infection.

[0063] Performance test 4

[0064] Test method: 10% by volume of granular liquid high polybasic aluminum chloride aqueous solution, according to the Ministry of Health of the People's Republic of China 2002 edition "disinfection technical specification" to carry out the test of bacteriostatic efficiency. The use of pathogen material is: Staphylococcus aureus, Candida albicans, polio virus (PV-Ⅰ type vaccine strain).

[0065] Test results: the obtained bacteriostatic efficiency data as shown in Table 1.

[0066] Table 1

[0067] Finally, it should be noted that the above examples are merely used to illustrate the technical solutions of the present application and are not intended to limit the scope of protection of the present application. Although the present application has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present application can be modified or replaced by equivalents without departing from the essence and scope of the technical solutions of the present application.

Claims

1. A method for preparing polymeric basic aluminum chloride, characterized in that, Includes the following steps: (1) After uniformly mixing mixed crystalline fumed alumina nanoparticles and deionized water, a chlorine source material is added to obtain the first reactant; wherein, the molar ratio of aluminum to chlorine is (0.9-1):3; the mass ratio of deionized water used to disperse the alumina powder to the alumina powder is (4.5-5.0):

1. (2) The first reactant is heated to boiling under one standard atmosphere, evaporated and reduced in volume until it is foamed, and the foamed material is heated at 100-110℃ until there is no free water to obtain the second reactant; (3) The second reactant was diluted with deionized water, stirred and mixed, and centrifuged to remove the precipitate, thus obtaining the third reactant. (4) Heat the third reactant to boiling at one standard atmosphere, maintain boiling state until a film appears on the surface of the system and the system becomes turbid. After foaming again, stop heating to obtain a bright orange system. (5) Let the bright orange system stand or centrifuge to remove the precipitate and obtain a yellow, clear, thick matrix product, which is the polymeric basic aluminum chloride.

2. The method for preparing polymeric basic aluminum chloride as described in claim 1, characterized in that, In step (1), the mass percentage of each crystal form in the mixed crystalline fumed alumina nanoparticles is as follows: Θ crystal form mass percentage is 79.71%, α crystal form mass percentage is 0.1014%, γ crystal form mass percentage is 19.97%, and η crystal form mass percentage is 0.227%; the average particle size of the mixed crystalline fumed alumina nanoparticles is 4-5 μm; and the chlorine source material is at least one of hydrogen chloride and titanium chloride.

3. The method for preparing polymeric basic aluminum chloride as described in claim 1, characterized in that, The polymeric basic aluminum chloride has an average particle size of 105-115 nm, a D50 particle size of 340-360 nm, and a D90 particle size of 3630-3650 nm.

4. Polymer basic aluminum chloride prepared by the method of preparing polymeric basic aluminum chloride as described in any one of claims 1-3.

5. The application of the polymeric basic aluminum chloride as described in claim 4 in the preparation of a dynamic water balance wet sterilization dressing.

6. A dynamic water balance moist sterilization dressing, characterized in that, It comprises the following components: the polymeric basic aluminum chloride as described in any one of claims 1-3 and deionized water; wherein the volume fraction of the polymeric basic aluminum chloride is 10-20%.

7. A dynamic water balance moist sterilization dressing, characterized in that, It comprises the following components: the polymeric basic aluminum chloride as described in any one of claims 1-3, oxide powder, and deionized water; wherein the volume fraction of the polymeric basic aluminum chloride is 2.0-5.0%.

8. A method for preparing a dynamic water balance moist sterilization dressing as described in claim 6, characterized in that, The process includes the following steps: dissolving polyaluminum chloride in deionized water and adjusting the volume to obtain the dynamic water balance wet sterile dressing.

9. A method for preparing a dynamic water balance moist sterilization dressing as described in claim 7, characterized in that, Includes the following steps: S1, dissolve polyaluminum chloride in deionized water, add oxide powder, mix well, and obtain a clear and transparent dressing matrix; S2, dissolve the dressing matrix in deionized water, add the oxide powder dispersed in deionized water, and then use deionized water to adjust the volume to obtain the dynamic water balance wet sterilization dressing.

10. Application of a dynamic water balance wet sterilization dressing in the field of medical devices and medical consumables.

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