NiCu alloy filter material for laparoscopic surgery, preparation method thereof and purifier

Abstract

The present invention provides a NiCu alloy filter material for laparoscopic surgery, comprising an alloy layer, the alloy layer comprising copper and nickel, the ratio of the copper content to the nickel content being (65-62): (35-38), the copper content accounting for more than 20% of the alloy layer, the average pore size of the NiCu alloy filter material being about 0.3-3 μm; further comprising a 300-500 mesh stainless steel mesh material, the alloy layer covering the stainless steel mesh material; the thickness of the NiCu alloy filter material being 50-160 μm. The NiCu alloy filter material for laparoscopic surgery provided by the present invention, the preparation method thereof, and the laparoscopic surgery purifier have good filtering effects when used during laparoscopic surgery.

Description

Technical Field

[0001] The invention belongs to the technical field of filter materials, and in particular relates to a NiCu alloy filter material used for laparoscopic surgery, a preparation method thereof, and a laparoscopic surgery purifier. Background Art

[0002] With the development of medicine, many surgical operations have been performed through minimally invasive surgery. Minimally invasive surgery refers to the use of modern medical equipment and related equipment such as laparoscopes and thoracoscopes. Its advantages are small trauma, light pain, fast recovery, short hospitalization, and less bleeding. The basic process of laparoscopic surgery is to use a pneumoperitoneum machine to inject CO2 gas into the human body cavity and maintain the gas pressure in the cavity stable, so that the cavity is stretched to provide space for endoscope observation and scalpel operation. During the operation, the doctor only needs to make a few small holes in the human body for the endoscope and scalpel to insert, which causes little harm to the patient. However, in laparoscopic surgery, ultrasonic knives and electric knives will produce a lot of smoke when cutting human tissue. If the smoke cannot be discharged in time, it will cause smoke to fill the cavity and affect the field of view of the endoscope; if the smoke is discharged directly, it will pollute the gas environment in the operating room and affect the health of medical staff. And the smoke itself has a very obvious smell, which will make people feel uncomfortable.

[0003] At present, the main materials for filtering particles in gases are organic filter membranes and metal filter membranes. Organic membranes are widely used due to their excellent filtering performance and extremely good flexibility. However, the disadvantages of organic membranes, such as easy breeding of bacteria, short service life, and not resistant to high temperatures, also hinder their wider application.

[0004] For example, the patent application number is 201310122035.8, and the invention name is: A disposable laparoscopic surgical exhaust gas filter. The patent application number is 201710027952.6, and the invention name is: A new type of graded gas filtration device. The patent application number is 201610308031.2, and the invention name is: A filtration puncture device for laparoscopy. However, the filter materials of the above schemes mainly use organic filter membranes (HEPA membranes / non-woven filter membranes) to filter smoke particles in the gas. However, most organic membranes have several disadvantages: 1. The filtration mechanism is mainly electrostatic adsorption, which is not suitable for use in overly humid environments; 2. Short life; 3. Low strength and easy to damage.

[0005] Metal filtration membranes have high strength, high interception accuracy, can be cleaned and reused, and the NiCu alloy system in particular has a strong sterilization effect. However, most metal porous membranes currently consist of a macroporous support layer and a microporous separation layer, which are thick and inflexible, so their application environments are very limited. In addition, there are few reports on porous membranes for antibacterial applications. Summary of the invention

[0006] In view of this, an object of the present invention is to provide a NiCu alloy filter material for laparoscopic surgery with good filtering effect and a preparation method thereof, as well as a laparoscopic surgery purifier using the filter material as a core filtering element.

[0007] The present invention provides a NiCu alloy filter material for laparoscopic surgery, comprising an alloy layer, wherein the alloy layer comprises copper elements and nickel elements, wherein the ratio of the copper content to the nickel content is (65-62):(35-38), the proportion of the copper content in the alloy layer is greater than 20%, and the average pore size of the NiCu alloy filter material is about 0.3-3 μm.

[0008] The NiCu alloy filter material for laparoscopic surgery provided by the present invention has a small membrane pore size and has a very high filtration efficiency for particulate matter PM2.5, and can remove laparoscopic surgery smoke. Since the copper content is controlled at more than 20%, it has an excellent bactericidal effect. The filter material was used for simulating intraoperative smoke filtration and was found to have a good filtration effect. And after the NiCu alloy filter material was removed and cleaned, it was tested again and still had a good filtration effect.

[0009] Compared with the organic filter membrane used for laparoscopic surgery in the prior art, the NiCu alloy filter material used for laparoscopic surgery provided by the present invention has the advantages of good filtering effect, strong antibacterial property, long service life and not easy to be damaged.

[0010] Preferably, it also includes a 300-500 mesh stainless steel mesh substrate, and the alloy layer is covered on the stainless steel mesh substrate. In this embodiment, the stainless steel mesh substrate is used as the base, which is easy to process and provides strength guarantee for the filter material.

[0011] Preferably, the thickness of the NiCu alloy filter material is 50-160 μm. In the special working environment of laparoscopic surgery, the filtering equipment needs to be small in size, easy to use, and not affect the normal operation of medical staff. The average thickness of the NiCu alloy membrane of the present invention is relatively thin, and can be well used in small filtering equipment.

[0012] Preferably, the preparation method of the NiCu alloy filter material is: coating a spray slurry on a stainless steel mesh substrate to obtain an alloy powder layer, the mass ratio of nickel and copper in the spray slurry is (60-70): (30-35), and the mesh base is a stainless steel mesh with a mesh size of 300-500.

[0013] The present invention also provides a method for preparing a NiCu alloy filter material for laparoscopic surgery, comprising the following steps:

[0014] S0. Pretreatment of stainless steel mesh substrate: Select 304 or 316L stainless steel mesh substrate with 300-500 mesh, first perform ultrasonic cleaning, and then dry. 304 or 316L stainless steel mesh has good processing performance, high toughness, high temperature resistance, and corrosion resistance. It is easy to process as a substrate and also provides strength guarantee for the filter material. At the same time, the substrate itself does not deform during the sintering process; the small holes of 300-400 mesh can not only ensure the flux, but also facilitate the adhesion of slurry during the spraying process to avoid defects.

[0015] S1, spraying a spray slurry containing nickel and copper onto a stainless steel mesh substrate, and then drying it;

[0016] S2. Sinter the dried product and then roll it to obtain NiCu alloy filter material for laparoscopic surgery. The sintering process is carried out in a hydrogen atmosphere. The powder has a high activity in a reducing atmosphere, which is conducive to the formation of pores and the homogenization of components. After sintering, it is cooled in the furnace. The purpose of rolling is to further reduce the pore size and increase the strength of the membrane layer.

[0017] Preferably, the spraying slurry is a solution system and a mixed metal powder raw material in a mixing ratio of (1-2): (1-2). The specific preparation method of the spraying slurry is: the solution system and the metal powder are mixed in a ratio of (1-2): (1-2), and the mixture is stirred and dispersed at a relatively low speed for 30 minutes in combination with ultrasound; after the mixture is evenly dispersed, the obtained slurry is vacuum degassed. The vacuuming speed should not be too fast, and the slurry should produce more bubbles without boiling. When no bubbles are generated, the degassing is completed to obtain the NiCu metal mixed spraying slurry to be used.

[0018] Preferably, the solution system is a solution system of PVB and ethanol. The ratio of PVB to ethanol in the solution system is about (0.6-1) g: 1 mL. The solution system of PVB and ethanol is selected and the reasonable ratio can prevent Ni and Cu powders from being oxidized by water vapor contained in the solution system or generated during decomposition during the preparation process.

[0019] The preparation method of the solution system is as follows: PVB powder is poured into ethanol in batches, and a stirrer is used to assist the dissolution of PVB at a stirring speed of 600-900 r / min, and then the mixture is capped and stirred at 400-600 r / min for about 10-30 minutes to make the solution system uniform, wherein the function of the cap is to prevent a large amount of ethanol from volatilizing during the stirring process and affecting the viscosity of the solution.

[0020] The preparation method of the mixed metal powder raw material is: nickel powder and copper powder with a particle size of 1 to 8 μm (laser particle size D50) are mixed in a mass ratio of (60 to 70): (30 to 40). The particle size of the raw material powder used in the powder metallurgy porous material is one of the important factors affecting its pore size. Smaller powder particle size can usually obtain a porous material with a smaller pore size.

[0021] Preferably, in step S1, the specific method of spraying is: using compressed air as the air source, spraying the nozzle onto the stainless steel mesh at a speed of 10 to 30 cm / min, and the feeding amount is 60 to 100 g / m 2 The ethanol solution dries faster, and the green body is basically dry after being air-dried for 0.5-2 hours.

[0022] Preferably, in step S2, the specific steps of sintering are:

[0023] (1) heating the sample to 100 to 140° C. at a heating rate of 3 to 8° C. / min and maintaining the temperature for 20 to 50 minutes for dehydration;

[0024] (2) The temperature is raised to 280-320°C at a rate of 3-8°C / min, and kept at this temperature for 10-30 minutes. The temperature is then raised to 350°C at a rate of 1-4°C / min and kept at this temperature for 1-3 hours. The temperature is then raised to 400-500°C at a rate of 1-4°C, and kept at this temperature for 1-3 hours. The temperature is then raised to 500-600°C at a rate of 3-8°C / min, and kept at this temperature for 0.5-1.5 hours for degreasing. Since 300-450°C is the main decomposition stage of PVB, the heating rate is slow and the holding time is long.

[0025] (3) First, keep the temperature at 700-900°C for 1-3 hours, then keep the temperature at 900-1100°C for 0.5-2 hours for sintering, and then cool the furnace to obtain a flexible NiCu alloy filter material.

[0026] The present invention also provides a purifier for laparoscopic surgery, comprising a purifier body and a NiCu alloy filter material located in the purifier body; the purifier body also has an activated carbon layer or manganese dioxide, and the NiCu alloy filter material and the activated carbon layer or manganese dioxide are arranged in sequence along the gas flow direction. The purifier provided by the present invention is cylindrical as a whole, wherein the NiCu alloy filter material 2 is a filter membrane arranged in a vertical folding manner, and the whole is also cylindrical; and the smoke generated by the operation is arranged to enter from the outside and to exit from the inside. These two designs can make full use of the space and maximize the effective filtration area of ​​the porous NiCu alloy in the limited space. At the same time, the interior of the NiCu alloy filter material is filled with high iodine value activated carbon or manganese dioxide to adsorb extremely fine gaseous organic matter that is not filtered out by the NiCu alloy filter material membrane.

[0027] The NiCu alloy filter material for laparoscopic surgery and the preparation method thereof, as well as the laparoscopic surgery purifier provided by the present invention have good filtering and sterilization effects when used during laparoscopic surgery. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] The above and other purposes, features and advantages of the present invention will become more clear by more specific description of the preferred embodiments of the present invention shown in the accompanying drawings. The same reference numerals indicate the same parts in all the accompanying drawings, and the accompanying drawings are not deliberately scaled to the actual size, and the focus is on illustrating the main purpose of the present invention.

[0029] Figure 1 A schematic diagram of the overall structure of the laparoscopic surgery purifier provided for the invention. DETAILED DESCRIPTION

[0030] The technical solution of the present invention is further described in detail below in conjunction with specific embodiments so that those skilled in the art can better understand the present invention and implement it, but the embodiments are not intended to limit the present invention.

[0031] In order to have a further understanding and recognition of the technical solution of the present invention, several preferred embodiments are listed and described in further detail.

[0032] Example 1

[0033] Pretreatment of stainless steel mesh substrate: Select 400 mesh 304 stainless steel mesh, first perform ultrasonic cleaning, and then dry.

[0034] Prepare the solution system: the ratio of PVB (polyvinyl butyral): ethanol is about 0.8g: 1mL. After weighing the raw materials according to the proportion, pour the PVB powder into the ethanol in small amounts and multiple times, and use a stirrer at a stirring speed of 800r / min to assist the dissolution of PVB. After the solution system is prepared, cover and stir at 500r / min for about 20 minutes to obtain the solution system.

[0035] Preparation of mixed metal powder raw material: Ni and Cu powders with a laser particle size D50 of about 5 μm are selected and mixed in a mass ratio of 65:35.

[0036] Preparation of spray slurry: metal powder and solution system are mixed in a mass ratio of 1:1, and are fully stirred and dispersed at a low speed for 30 minutes in combination with ultrasound; after being evenly dispersed, the obtained slurry is vacuum degassed until no bubbles are generated, and the degassing is completed to obtain the NiCu metal mixed spray slurry to be used.

[0037] The prepared NiCu metal mixed spray slurry is sprayed onto the pre-treated 304 stainless steel mesh material, and compressed air is used as the air source. The nozzle is sprayed uniformly on the required stainless steel substrate surface at a speed of about 20cm / min in a fixed path, and the loading amount is about 80g / m2. The green body is basically dry after being blown and air-dried for 1 hour.

[0038] The dried green body is hydrogen sintered. The sintering process is divided into three steps: dehydration, degreasing and sintering:

[0039] The temperature was raised to 120°C at a rate of 5°C / min and kept at that temperature for 30 min for dehydration;

[0040] The temperature was increased to 300°C at a rate of 5°C / min and kept for 20 minutes, then increased to 350°C at a rate of 2°C / min and kept for 2 hours, then increased to 450°C at a rate of 2°C / min and kept for 2 hours, and then increased to 550°C at a rate of 5°C / min and kept for 1 hour for degreasing.

[0041] In a hydrogen atmosphere, the steel was sintered at 800°C for 2 h and then at 1000°C for 1 h, and then cooled in the furnace.

[0042] The sintered NiCu alloy porous membrane is precision rolled, and the membrane thickness after rolling is about 150 μm, thereby obtaining the final NiCu alloy porous membrane.

[0043] The obtained NiCu alloy porous membrane includes an alloy layer, the alloy layer includes copper elements and nickel elements, the ratio of copper content to nickel content is (65-62): (35-38), the proportion of copper content in the alloy layer is greater than 20%, and the average pore size of the NiCu alloy porous membrane is 0.5-2μm.

[0044] refer to Figure 1 , a NiCu alloy filter material 2 (NiCu alloy porous membrane) is installed in the purifier body 1 to obtain a laparoscopic surgery gas purifier. The activated carbon layer 3 in the purifier body 1 surrounds the outside of the gas outlet channel 5, the NiCu alloy filter material 2 surrounds the outside of the activated carbon layer 3, and the inlet channel 4 is connected to the NiCu alloy filter material 2. The gas passes through the NiCu alloy filter material 2 and the activated carbon layer 3 in sequence from the inlet channel 4, and then enters the gas outlet channel 5 from the activated carbon layer 3, and is discharged from the purifier body 1 through the gas outlet channel 5.

[0045] The laparoscopic surgery gas purifier prepared in Example 1 was used in the smoke filtration process during the simulated surgery. The specific test results are shown in Table 1.

[0046] Table 1

[0047]

[0048] From the data in Table 1, it can be seen that the laparoscopic surgery gas purifier provided by the present invention has a good filtering effect, and the effective filtering time is longer than 3 hours.

[0049] The test method for effective filtration time is as follows: the porous membrane is used to filter simulated laparoscopic gas, and the gas standard after filtration is PM2.5 < 35 μg·m -3 , TVOC content <0.6mg·m -3 , formaldehyde content <0.1mg·m -3 When the filtered gas pollutants exceed the standard value, it is considered to be invalid. The NiCu alloy porous membrane was removed and cleaned and then installed again for testing. The filtering effects on PM2.5, formaldehyde and TVOC are basically consistent with Table 1, indicating that the NiCu alloy filter material provided by the present invention is not easy to be damaged and can be washed with water.

[0050] The test showed that the killing rate of NiCu alloy filter material on Staphylococcus aureus, Escherichia coli and Pseudomonas aeruginosa within 24 hours was above 99.0%.

[0051] The above are only preferred embodiments of the present invention, and are not intended to limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made using the contents of the present invention specification, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present invention.

Claims

1. A method for preparing a NiCu alloy filter material for laparoscopic surgery, characterized in that: The NiCu alloy filter material comprises an alloy layer and a 300-500 mesh stainless steel mesh substrate, the alloy layer covers the stainless steel mesh substrate, the alloy layer comprises copper and nickel elements, the ratio of the copper content to the nickel content is (65-62): (35-38), the copper content accounts for more than 20% of the alloy layer, and the average pore size of the NiCu alloy filter material is about 0.3-3 μm; The preparation method comprises the following steps: S1. Spraying a spray slurry containing nickel and copper onto a stainless steel mesh substrate, and then drying it; the spray slurry is a solution system and a mixed metal powder raw material obtained in a mixing ratio of (1-2): (1-2), and the solution system is a solution system of PVB and ethanol; S2, sintering the dried product, and then rolling it to obtain a NiCu alloy filter material for laparoscopic surgery; the specific steps of the sintering are: S11, heating to 100-140°C at a heating rate of 3-8°C / min, and keeping the temperature for 20-50 minutes for dehydration; S12, heating to 280-320°C at 3-8°C / min, keeping warm for 10-30min, then heating to 350°C at 1-4°C / min, keeping warm for 1-3 hours, then heating to 400-500°C at 1-4°C / min, keeping warm for 1-3 hours, then heating to 500-600°C at 3-8°C / min, keeping warm for 0.5-1.5 hours, and degreasing; S13, first keep the temperature at 700-900°C for 1-3 hours, then keep the temperature at 900-1100°C for 0.5-2 hours for sintering, and then cool the furnace to obtain a flexible NiCu alloy filter material.

2. The method for preparing the NiCu alloy filter material for laparoscopic surgery according to claim 1, characterized in that: The thickness of the NiCu alloy filter material is 50-160 μm.

3. The method for preparing the NiCu alloy filter material for laparoscopic surgery according to claim 1, characterized in that: The mass ratio of nickel to copper in the spraying slurry is (60-70):(30-35).

4. The method for preparing the NiCu alloy filter material for laparoscopic surgery according to claim 1, characterized in that: The ratio of PVB to ethanol in the solution system is about (0.6-1) g: 1 mL. The preparation method of the solution system is: pouring PVB powder into ethanol in batches, and using a stirrer at a stirring speed of 600-900 r / min to assist the dissolution of PVB, and then stirring at 400-600 r / min with a cap for about 10-30 minutes; The preparation method of the mixed metal powder raw material is as follows: nickel powder and copper powder with a particle size of 1 to 8 μm are mixed in a mass ratio of (60 to 70): (30 to 40).

5. The method for preparing the NiCu alloy filter material for laparoscopic surgery according to claim 1, characterized in that: In step S1, the specific method of spraying is: using compressed air as the air source, spraying the nozzle onto the stainless steel mesh at a speed of 10 to 30 cm / min, and the feeding amount is 60 to 100 g / m 2 .

6. A laparoscopic surgery purifier, characterized in that: It comprises a purifier body and a NiCu alloy filter material prepared by the NiCu alloy filter material preparation method according to any one of claims 1 to 5 and located in the purifier body; the purifier body also has an activated carbon layer or manganese dioxide, and the NiCu alloy filter material and the activated carbon layer or manganese dioxide are arranged in sequence along the gas flow direction.

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