CN109641252B - Method for manufacturing metal thin tube - Google Patents
Method for manufacturing metal thin tube Download PDFInfo
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- CN109641252B CN109641252B CN201780044087.4A CN201780044087A CN109641252B CN 109641252 B CN109641252 B CN 109641252B CN 201780044087 A CN201780044087 A CN 201780044087A CN 109641252 B CN109641252 B CN 109641252B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C1/00—Manufacture of metal sheets, metal wire, metal rods, metal tubes by drawing
- B21C1/16—Metal drawing by machines or apparatus in which the drawing action is effected by other means than drums, e.g. by a longitudinally-moved carriage pulling or pushing the work or stock for making metal sheets, bars, or tubes
- B21C1/22—Metal drawing by machines or apparatus in which the drawing action is effected by other means than drums, e.g. by a longitudinally-moved carriage pulling or pushing the work or stock for making metal sheets, bars, or tubes specially adapted for making tubular articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
- B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
- B21C9/00—Cooling, heating or lubricating drawing material
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
- C10M169/00—Lubricating compositions characterised by containing as components a mixture of at least two types of ingredient selected from base-materials, thickeners or additives, covered by the preceding groups, each of these compounds being essential
- C10M169/04—Mixtures of base-materials and additives
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G1/00—Cleaning or pickling metallic material with solutions or molten salts
- C23G1/24—Cleaning or pickling metallic material with solutions or molten salts with neutral solutions
Abstract
The method for manufacturing a metal capillary tube according to the present invention is characterized by including: the method for manufacturing the metal pipe includes a pipe-making step of forming a metal pipe blank by processing a flat metal plate, a wall thickness-determining step of processing the metal pipe blank obtained in the pipe-making step into a predetermined wall thickness using a water-soluble lubricant, and a washing step of washing the metal pipe obtained in the wall thickness-determining step using an aqueous washing liquid.
Description
Technical Field
The present invention relates to a method for manufacturing a metal tubule such as a stainless steel tubule. More specifically, the present invention relates to a method for producing a metal capillary tube, which can wash the metal capillary tube without using an organic solvent as a washing medium during processing. In addition, the present invention also relates to a water-soluble lubricant for metal working used for such a purpose, and a combination of the water-soluble lubricant and an aqueous cleaning solution.
Background
In medical instruments such as injection needles, metal thin tubes having a small diameter have been used. Such a metal thin tube is often produced by drawing, etc., but lubricating oil is used for the inner and outer surfaces of the tube in order to suppress scorching and vibration generated when the blank tube is drawn (for example, japanese patent laid-open nos. 2015-137345 and 2015-167953). Such a lubricating oil is indispensable for metal working, but if the lubricating oil is left without being sufficiently washed in a subsequent step, it may cause product defects. Therefore, in the manufacturing stage of the product, the lubricating oil needs to be completely washed and removed.
In particular, in order to produce a very small diameter metal thin tube such as an extremely small stainless steel tube, a wall thickness determining step of drawing a blank tube to a desired wall thickness and a washing step of washing a lubricating oil used in the wall thickness determining step are required more times in the processing step than in the case of producing a large diameter metal tube. Therefore, it is necessary to wash and remove the lubricating oil corresponding to the number of machining cycles, and there is a problem that the time required for washing and the amount of the organic solvent for washing used are also increased as compared with those in the production process of a normal metal pipe. In addition, since the diameter of the fine tube is small and the length of the tube is long, it is difficult for the washing solvent to enter the tube, which also results in an increase in the time required for washing and the amount of washing solvent used.
Conventionally, an organic solvent such as trichloroethylene having a high detergency has been mainly used as a washing liquid for washing lubricating oil. However, in recent years, the use of such organic solvents has been strictly limited from the viewpoint of considering the load on the environment and the viewpoint of reducing the health risk of the operator.
For example, in europe, by limiting hazardous substances contained in products sold in the EU range, Reach restriction and RoHS directive are made in order to minimize the risk of causing environmental damage or the risk of causing adverse effects on human health, and the use of hazardous substances in the production process is strictly restricted. In particular, in Reach's limitation, 1500 substances of high interest are the subject of limitation in almost all industries, including trichloroethylene. Further, in order to obtain global customers, it is desired to satisfy ISO14000 which is an international standard relating to an environmental management system, and therefore, an environment-conscious manufacturing method which does not use harmful substances is also required.
In japan, the organic chlorine compound trichloroethylene is specified as a first specified chemical substance according to a chemical substance discharge grasping and management promoting law, and enterprises are under an obligation to grasp the amount and report it to the country when discharging/moving the substance. In addition, trichloroethylene is specified as the second specific chemical by law relating to the limits of examination and manufacture of the chemical, and there are obligations for manufacture, import of a predetermined amount, and actual presentation.
In addition, trichloroethylene has been pointed out as carcinogenic (National cancer Institute (NRI): Carinogenic BioAssay of trichoethylene. Bethesda, MD, US Department of Health, Edutation and Welfare, Public Health Service, National Institutes of Health, National cancer Institute (NCI-CGTR-2, NIH 76-802. 1976), and thus there is also concern about Health damage to persons engaged in metal processing.
Documents of the prior art
Patent document
Patent document 1: japanese patent laid-open publication No. 2015-137345
Patent document 2: japanese patent laid-open publication No. 2015-
Non-patent document
Non-patent document 1: carinogenesis bioassay of trichoethylene Bethesda, MD, US Department of Health, birth and Welfare, Public Health Service, National institutes of Health, National Cancer Institute (NCI-CGTR-2, NIH76-802).1976
Disclosure of Invention
The treatment of chlorine-based organic solvents such as trichloroethylene, which have been pointed out to have such problems, needs to be performed on a strict basis, and the labor and cost required for the management and disposal thereof cannot be ignored. For the above reasons, in the production process of a metal narrow tube including a conventional method for washing a lubricating oil using an organic solvent such as trichloroethylene, since the discharge standard of trichloroethylene is limited, a sufficient washing step may not be necessarily performed on the metal tube after the thickness determining step, and there is a problem that product defects and yield decreases due to residual oil may occur.
Further, even if the production line has a manufacturable capacity, there is a problem that the emission standard of the organic solvent for washing used in the washing step is regulated in a legal manner as described above and strict management is required while considering the environment, so that the washing step is inevitably rate-limited and the manufacturing capacity of the factory cannot be fully utilized. This also becomes a factor that hinders reduction of the shipment period from the receipt of orders to the delivery of the goods.
Therefore, in order to reduce the load on the environment and health and to improve the industrial productivity, development of a new method for producing a metal narrow tube, which does not include a step of washing a lubricant with an organic solvent such as trichloroethylene, is urgently required.
In view of such circumstances, in the field of metal processing, there is a demand for a water-soluble detergent or a hydrocarbon-based cleaning solvent which can replace an organic solvent such as trichloroethylene. However, in the production methods thus far studied, the detergency of the lubricant is insufficient, which causes product defects. In particular, in a fine metal capillary tube used as a component of a medical instrument such as an injection needle, an endoscope component, and a catheter component, which are required to have high product quality, the standard required for the washing property is extremely high, and therefore, improvement of such quality is an unavoidable problem. In particular, when the metal capillary has a small diameter and a long length, the liquid flow resistance in the tube becomes large, and therefore, the cleaning effect of the inner surface of the tube is reduced as compared with a tube having a large diameter, and the time required for the working process becomes long.
In order to solve the above problems, a method for manufacturing a metal capillary according to the present invention is characterized in that a water-soluble lubricant is used as a lubricant for machining and an aqueous cleaning solution is used as the cleaning solution.
That is, the present invention provides a method for efficiently producing a metal capillary, which uses an aqueous cleaning solution instead of an organic solvent in a cleaning step while maintaining high cleaning performance.
The method for manufacturing a metal capillary tube according to the present invention is characterized by including: the method for manufacturing the metal pipe includes a pipe-making step of forming a metal pipe blank by processing a flat metal plate, a wall thickness-determining step of processing the metal pipe blank obtained in the pipe-making step into a predetermined wall thickness using a water-soluble lubricant, and a washing step of washing the metal pipe obtained in the wall thickness-determining step using an aqueous washing liquid. Here, the thickness determining step and the washing step may be repeated as many times as desired.
In addition, the method for manufacturing a thin metal tube according to the present invention may further include, as desired, in addition to the tube forming step, the thickness determining step, and the washing step: an annealing step of heat-treating the metal pipe after the pipe making, the wall thickness determination, and the washing, a drawing step of elongating the metal pipe obtained in the annealing step to a desired outer diameter, and a straightening step of machining the metal pipe obtained in the drawing step to a desired shape.
The method for manufacturing a metal capillary tube according to the present invention may further include, as desired, in addition to the steps described above: an inspection step of checking whether or not a hole is formed in the metal narrow tube, and a drying step of washing and then drying the metal narrow tube.
The metal tubule manufactured by the present invention is not limited to a tubule having a circular or elliptical cross section, and may include a tubule having a rectangular cross section such as a square or rectangle.
Drawings
Fig. 1 is a diagram showing a specific example of a preferred process of the method for producing a metal capillary according to the present invention.
In fig. 2, fig. 2a to 2g show the results of lubricant residue analysis by infrared spectroscopic analysis in the metal capillary tube washing test. Fig. 2a is an analysis result of the outer surface of the tubule after the thickness determining step (before washing), fig. 2b is an analysis result of the inner surface of the tubule after the thickness determining step (before washing), fig. 2c is an analysis result of the outer surface of the tubule after the thickness determining step (after washing), fig. 2d is an analysis result of the inner surface of the tubule after the thickness determining step (after washing), fig. 2e is an analysis result of the outer surface of the tubule after the correcting step (before washing), fig. 2f is an analysis result of the inner surface of the tubule after the correcting step (before washing), fig. 2g is an analysis result of the outer surface of the tubule after the correcting step (after washing), and fig. 2h is an analysis result of the inner surface of the tubule after the correcting step (after washing).
Detailed Description
As described above, one feature of the method for producing a metal capillary tube according to the present invention is that a water-soluble lubricant is used as a lubricant used in processing (particularly, in the thickness determining step) instead of a conventional lubricant, and an aqueous cleaning solution is used as a cleaning solution for cleaning and removing the lubricant.
In a preferred embodiment of the present invention, water is used as the aqueous cleaning solution. As water, a common aqueous medium capable of dissolving and removing a water-soluble lubricant, such as tap water, well water, spring water, pure water, and other industrial water, can be widely used, and is industrially very advantageous in view of the versatility.
In a preferred embodiment of the present invention, the water-soluble lubricant is composed of a composition containing a paraffin-based lubricating component, a surfactant and a synthetic oil, and the balance being unavoidable impurities.
In this case, the paraffin-based lubricating component is preferably a chlorinated paraffin, and the chlorinated paraffin includes a short-chain chlorinated paraffin, a medium-chain chlorinated paraffin, a long-chain chlorinated paraffin, and the like, and from the viewpoint of both lubricating performance as a lubricant and washing performance by washing with an aqueous medium, the medium-chain chlorinated paraffin is particularly preferably used.
In general, chlorinated paraffins are a generic term for chlorinated hydrocarbons in which chlorine is bound to paraffins, and are represented by the following general formula.
CnH2n+2-xClx
(wherein n represents an integer of 1 or more and x represents the amount of chlorine.)
In the general formula, when n is 10 to 13, the chlorinated paraffin is called a short-chain chlorinated paraffin, when n is 14 to 19, the chlorinated paraffin is called a medium-chain chlorinated paraffin, and when n is 20 to 30, the chlorinated paraffin is called a long-chain chlorinated paraffin. According to this definition, the paraffin-based lubricating component as a blending component of the water-soluble lubricant in the present invention is most preferably a medium-chain chlorinated paraffin in which n is 14 to 19, from the viewpoint of balance between the lubricating performance and the washing performance by washing with a water-soluble medium. Particularly preferred are medium chain chlorinated alkanes having the formula:
C14.5H22.7C8.3
the content of the paraffinic lubricating component to be blended with the water-soluble lubricant is preferably about 30 to about 95 wt%, more preferably about 50 to about 90 wt%, and most preferably about 70 to about 90 wt%.
In a preferred embodiment of the present invention, a nonionic surfactant is preferred as the surfactant that functions as an emulsifier contained in the water-soluble lubricant. Specifically, the method comprises the following steps: ester-type nonionic surfactants such as polyoxyethylene fatty acid esters, glycerin fatty acid esters, sorbitan fatty acid esters, sucrose fatty acid esters; ether type nonionic surfactants such as polyoxyethylene fatty acid ether, alkylpolyethylene glycol, polyoxyethylene alkylphenyl ether; alkyl glycosides, etc., but are not limited thereto.
In particular, the medium-chain chlorinated paraffin is most preferable from the viewpoint of lubricating performance, and a combination with a nonionic surfactant is most preferable from the viewpoint of achieving good emulsification of the medium-chain chlorinated paraffin and excellent detergency.
In a preferred embodiment of the present invention, the nonionic surfactant is preferably a polyoxyethylene fatty acid ester having the following formula,
RCOO(EO)nH
(wherein R represents an alkyl group, (EO) represents ethylene oxide, and n represents an integer of 1 or more.)
Or polyoxyethylene fatty acid ethers of the formula,
RO(EO)nH
(wherein R represents an alkyl group, (EO) represents ethylene oxide, and n is an integer of 1 or more.)
Or a mixture thereof.
The content of the surfactant to be blended with the water-soluble lubricant of the present invention is preferably about 2 to about 30 wt%, more preferably about 4 to about 20 wt%, and most preferably about 5 to about 15 wt%.
As the synthetic oil contained in the water-soluble lubricant, for example, synthetic oil containing a fatty acid ester compound such as Fatty Acid Methyl Ester (FAME), a fatty acid amide or the like can be preferably used, but the present invention is not limited to these.
In a preferred embodiment of the present invention, the synthetic oil is a synthetic oil containing a fatty acid methyl ester, a fatty acid amide, or a mixture thereof,
the fatty acid methyl ester has the formula:
RCOOCH3
(wherein R represents an alkyl group)
The fatty amide has the formula:
RCONH2
(wherein R represents an alkyl group).
The content of the synthetic oil blended with the water-soluble lubricant of the present invention is preferably about 2 to about 30 wt%, more preferably about 4 to about 20 wt%, and most preferably about 5 to about 15 wt%.
In the method for producing a metal capillary tube of the present invention, it is particularly preferable that the water-soluble lubricant contains about 85 wt% of a medium-chain chlorinated paraffin, about 8 wt% of a nonionic surfactant, and about 7 wt% of a synthetic oil, based on the weight of the water-soluble lubricant.
In the method for producing a metal capillary tube of the present invention, the water-soluble lubricant is composed of a composition in the form of an emulsion obtained by combining the above components. The emulsion-form water-soluble lubricant of the present invention is excellent in lubricity, coolability, and flame retardancy, and not only exerts an excellent effect when the coolability and lubricity at the time of processing are required, but also has properties such as lubricity, particle diameter, viscosity, and viscosity index suitable for the method for producing a metal capillary unique to the present invention.
In a preferred embodiment, the water-soluble lubricant of the present invention has a kinematic viscosity (kineticiviscosensitivity) of about 2010cST at 40 ℃, a kinematic viscosity of about 90cST at 100 ℃, and a viscosity index of about 111 (wherein the passable kinematic viscosity (cST) ═ viscosity (cP)/density (g/cm/g/cm)2) Found).
Further, since the water-soluble lubricant of the present invention is used in the form of an emulsion, the dispersed particles have a larger particle size than other forms, for example, a soluble form and a solution form, and further advanced treatment (advanced treatment) is not required, and thus the water-soluble lubricant has an advantage that waste liquid treatment can be easily performed.
In addition, the water-soluble lubricant described above brings about a remarkable and unexpected advantageous effect described below in the method for producing a metal capillary tube of the present invention by combining with washing with an aqueous washing liquid described below.
In the method for producing a metal capillary tube of the present invention, an aqueous cleaning solution is used for cleaning the water-soluble lubricant. The preferred aqueous wash is water. The water can be tap water, well water, spring water, pure water, or other industrial water. Since the metal capillary tube can be sufficiently washed by using water as the washing liquid, the washing liquid can be used continuously, which contributes to improvement of quality, and since there is no legal limit related to the discharge standard of chlorine-based organic solvents such as trichloroethylene, the production efficiency can be maximized according to the production scale and the production capacity, which is industrially very advantageous as compared with organic solvents that must be handled with attention paid to the latest limit under strict management, and since the production capacity of a factory can be utilized to the maximum, an excellent effect is exhibited in that the shipment period from order acceptance to delivery can be further shortened.
In another preferred embodiment of the present invention, the preferred temperature of the water used for washing is about 20 ℃ to about 95 ℃, more preferably about 60 ℃ to about 80 ℃. By using water in such a temperature range, the washing effect can be further improved.
In another preferred embodiment of the present invention, the washing effect can be further improved by washing with water containing a surfactant and then washing with water containing no surfactant.
Examples of the metal used for the thin metal tube of the present invention include, but are not limited to, metals selected from the group consisting of stainless steel, titanium-nickel alloys, tantalum, niobium, cobalt-chromium alloys, and combinations thereof.
The metal used in the metal capillary of the present invention is preferably stainless steel. For example, as applications of the stainless steel narrow tube obtained by the method of the present invention, there are medical instruments such as injection needles, endoscope components, catheter components, connectors for brain surgery, and nozzles for otorhinology, which are required to be stable and high in quality because the quality of the stainless steel narrow tube as a core material has a large influence on the product quality.
In another embodiment of the present invention, for example, in the case of a stainless steel tubule used for a medical instrument, a tubule having a thinnest thickness of about 0.038mm, an outer diameter of at least about 0.127mm, and an inner diameter of at least about 0.0508mm can be manufactured as the tubule that can be manufactured in the present invention.
Hereinafter, a case of manufacturing a stainless steel tubule according to the method for manufacturing a metal tubule of the present invention will be described with reference to the process diagram of fig. 1.
First, in the tube forming process, a stainless steel flat plate is processed to form a stainless steel raw tube. The tube-making process itself may be carried out according to a conventional method. In this case, the cross section of the pipe to be formed is not limited to a circular or oval shape, but may include a rectangular cross section such as a square or rectangle depending on the application.
Next, in the wall thickness determining step, the metal shell obtained in the tube forming step is processed to a predetermined desired wall thickness using the water-soluble lubricant. In the present invention, the thickness determining step is carried out by a conventional method except that the above-mentioned water-soluble lubricant is used instead of the conventional lubricating oil. Specifically, the method includes a method selected from the group consisting of drawing, extruding, forging, and rolling of a stainless steel blank tube, and a combination of 2 or more of these methods, but is not limited to these methods, and the method may be processed by a metal working method known in the art. In a preferred embodiment of the present invention when manufacturing a stainless steel thin tube, in the thickness determining step, the metal is worked by drawing or extrusion, and particularly preferably by drawing.
The stainless steel pipe adjusted to a predetermined thickness in the thickness determination step is subjected to an air inspection for inspecting whether holes or flaws are generated in the pipe, as necessary. The air check can be performed by pressing water into the tube and detecting the presence or absence of water leakage.
After the air examination, washing was performed using an aqueous washing solution (water in this specific example). In the washing step, not only the outer surface of the narrow tube but also the water-soluble lubricant remaining on the inner surface of the tube is removed.
In a preferred embodiment of the present invention, the washing may be spray washing, and may be performed by introducing a washing liquid from an opening of the metal capillary by a spray nozzle. The temperature conditions and the like of the aqueous washing solution are as described above.
In a preferred embodiment of the present invention, the liquid used in the inspection step (air inspection) may be different from or the same as the cleaning liquid used in the cleaning step, but in the case of the same medium, water can be used in both the cleaning liquid and the inspection, and therefore, the present invention is also excellent in that the production process can be further efficiently performed.
In addition, the thickness determination step and the washing step may be repeated a plurality of times as shown in fig. 1 according to the process requirements of the thin tube to be manufactured.
In the method for manufacturing a metal tubule of the present invention, the ventilation can be switched to the air ventilation at the same time as the completion of the water washing step. By this air ventilation, the narrow tube can be sufficiently dried well immediately after washing, and the quality defect of the inner surface of the narrow tube can be prevented.
Next, the thin tube having passed through the thickness determining step and the washing step is transferred to the annealing step. In this annealing step, the stainless steel structure deformed by work hardening is restored to the original structure by heating to a predetermined temperature, and the deformation of the structure is eliminated. As the heat treatment temperature for this purpose, a heat treatment of about 1000 ℃ or higher is generally required in the case of a stainless steel narrow tube.
The above-mentioned water washing step is important because the lubricant component from the previous step remains in the annealing step, which also causes generation of defective portions such as discoloration on the surface of the stainless steel. According to the present invention, as described above, since a combination of a water-soluble lubricant and an aqueous cleaning solution is used, the occurrence of such defective portions can be eliminated as much as possible.
The stainless steel pipe obtained in the annealing step is elongated to a predetermined outer diameter according to a required standard by a conventional method as necessary. This is called a tube drawing process.
In another embodiment of the present invention, the outer surface of the metal capillary can be cleaned in the tube drawing step. At this time, since the cut surface is closed by cutting the coil (coil) in the drawing step, the washing water for washing the outer surface does not flow into the metal thin tube. The washing of the outer surface can be performed by using an aqueous washing liquid, as in the case of the washing of the inner surface.
The stainless steel tube obtained in the tube drawing step is, for example, formed straight, and then transferred to a straightening step for processing the tube into a predetermined shape in accordance with the manufacturing process requirements, thereby completing a stainless steel thin tube.
Examples
Example 1
Hereinafter, among the steps of manufacturing the thin metal tube according to the present invention, particularly, the washing step after the thickness determination processing will be described by way of example of the case of the thin stainless steel tube.
Test specimen
In the thickness determining step, a washing test was performed using 4 coils Z1 to Z4 having different thicknesses, inner diameters, outer diameters, and lengths, in which a water-soluble lubricant MD15 (about 80 to about 90 wt% of medium-chain chlorinated paraffin, about 5 to about 10 wt% of nonionic surfactant, and about 5 to about 10 wt% of synthetic oil) was used on the inner surface of a thin metal tube made of stainless steel. The characteristics of Z1-Z3 are shown in Table 1 below.
TABLE 1
| Sample number | Weight (kg) | Inner diameter (mm) | Outer diameter (mm) | Length (m) |
| Z1 | 10.3 | 2.42 | 2.85 | 727.2 |
| Z2 | 10.33 | 1.70 | 2.33 | 651 |
| Z3 | 5.7 | 1.91 | 2.10 | 1197 |
Method of producing a composite material
As a metal capillary sample, Z1 (stainless steel, having a mass of 10.3kg, an inner diameter of 2.42mm, an outer diameter of 2.85mm, and a length of 727.2m) was used.
As the lubricant, MD15 (medium chain chlorinated paraffin about 80 to about 90 wt%, nonionic surfactant about 5 to about 10 wt%, synthetic oil about 5 to about 10 wt%) was used.
As a washing solution, tap water 5.7L was used at 55 ℃.
After the washing water was injected from one end of the stainless steel capillary sample Z1, the washing water was discharged from the other end after about 23 minutes and 30 seconds. Immediately after the washing water started to be discharged, a precipitate of rust considered to be dark brown was confirmed in the collected washing water. Then, when the flow of the washing water was continued, the recovered washing water became clear by visual observation after about 53 minutes and 50 seconds from the start of the injection of the washing water. Then, the washing was further continued for about 6 minutes and 10 seconds from the start of the washing water injection to about 60 minutes. The washing water recovered from the beginning of washing water discharge after about 23 minutes and 30 seconds to about 29 minutes and 30 seconds after (period 1), the washing water discharged from the beginning of washing water injection after about 53 minutes and 50 seconds to about 60 minutes after (period 2), which was confirmed to be transparent by visual observation, and the washing water discharged from the beginning of washing water injection to about 60 minutes after (period 3), which was air-switched by stopping water and was air-switched after about 60 minutes to about 67 minutes and 40 seconds, were collected, and the washing result was visually confirmed. Further, it took about 30 minutes from the stop of water until water no longer flowed out.
Results
The results of the analysis of the cleanliness of the washing water are shown in table 2 below.
TABLE 2
Example 2
Method of producing a composite material
As the capillary sample, Z2 (stainless steel, having a mass of 10.33kg, an inner diameter of 1.70mm, an outer diameter of 2.33mm, and a length of 651m) described in Table 1 was used.
As the lubricant, MD15 (medium chain chlorinated paraffin about 80 to about 90 wt%, nonionic surfactant about 5 to about 10 wt%, synthetic oil about 5 to about 10 wt%) was used.
As a washing solution, tap water 2.4L was used at 55 ℃.
After the washing water was injected from one end of the stainless steel capillary sample Z2, it was confirmed that the washing water was drained from the other end after about 36 minutes. Immediately after the washing water started to be discharged, a precipitate of rust considered to be dark brown was confirmed in the collected washing water. Then, when the flow of the washing water was continued, it was confirmed that the turbidity of the collected washing water was reduced by visual observation after about 58 minutes from the start of the injection of the washing water. Then, the washing was further continued from the start of the washing water injection to about 20 minutes after about 78 minutes. The washing water recovered from about 36 minutes after the start of the washing water injection to about 58 minutes after (period 1) and discharged from the start of the washing water discharge, the washing water discharged from about 58 minutes after to about 78 minutes after the start of the washing water injection (period 2) and discharged from the start of the washing water injection to about 78 minutes after (period 3) and air-switched by stopping water injection was collected, and the washing result was visually confirmed. In addition, it took about 41 minutes to stop the water until the water was no longer discharged. The inner diameter of the specimen Z2 was very small, and therefore washing took a long time.
Results
The results of the analysis of the cleanliness of the washing water are shown in table 3 below.
TABLE 3
Example 3
Method of producing a composite material
As the metal capillary sample, Z3 (stainless steel, 5.7kg in mass, 1.91mm in inner diameter, 2.10mm in outer diameter, 1197m in length) described in Table 1 was used.
As the lubricant, MD15 (medium chain chlorinated paraffin about 80 to about 90 wt%, nonionic surfactant about 5 to about 10 wt%, synthetic oil about 5 to about 10 wt%) was used.
As a washing solution, tap water 4L was used at 55 ℃.
After the washing water was injected from one end of the stainless steel capillary sample Z3, the washing water was discharged from the other end after about 92 minutes. Immediately after the washing water started to be discharged, a precipitate of rust considered to be dark brown was confirmed in the collected washing water. Then, when the flow of the washing water was continued, the recovered washing water was visually confirmed to be clear of turbidity about 140 minutes after the start of the injection of the washing water. Then, the washing from the start of the washing water injection to about 5 minutes after about 140 minutes to about 145 minutes is further continued. The washing water recovered from about 92 minutes to about 115 minutes after the start of the washing water injection (period 1) and discharged from the start of the washing water injection, the washing water discharged from about 140 minutes to about 145 minutes after the start of the washing water injection (period 2) and the washing water discharged from about 145 minutes to about 172 minutes after the start of the washing water injection (period 3) and air-switched by stopping the water were collected, and the washing results were visually confirmed. Further, it took about 112 minutes from the stop of water until water was no longer discharged. The thickness of Z3 was as thin as 0.095mm, and the total length of the coil was long, so that a long water passage time was required.
Results
The results of the analysis of the cleanliness of the washing water are shown in table 4 below.
TABLE 4
Investigation of
The results of examples 1 to 3 are summarized in Table 5 below.
TABLE 5
As shown in examples 1 to 3, according to the method of the present invention, by using a specific water-soluble lubricant and an aqueous cleaning solution in combination in the production process, the application and cleaning of the lubricant can be efficiently and effectively performed.
Example 4
In order to confirm the presence or absence of a residue of a lubricant (oil component) for machining in the thin metal tube manufactured by the method of the present invention, the amount of the lubricant residue on the outer surface and the inner surface of the thin metal tube after the thickness determination step and after the correction step was measured by an infrared spectroscopy (IR method).
Material
As a metal capillary sample, Z4 (stainless steel, inner diameter of 2.4mm, outer diameter of 2.8mm, length of 2000m) was used, and as a lubricant in the processing step, MD15 was used in the wall thickness determining step and CK (medium-chain chlorinated paraffin of about 80 to about 90 wt%, nonionic surfactant of about 5 to about 10 wt%, synthetic oil of about 5 to about 10 wt%) was used in the leveling step.
Conditions of analysis
(1) The infrared spectrometer was used with a Fourier transform infrared spectrometer Magna-750 and an infrared microscope Nic-Plan manufactured by ThermoFisher Scientific at 8cm-1The wave number resolution of (2) was determined.
(2) The measurement of the reflection object was performed by a micro-reflection method using a clean gold mirror.
(3) The obtained spectrum was subjected to absorbance display, and baseline correction was performed.
Test method
In the production of a narrow metal tube, narrow metal tube samples in the respective steps described in table 6 below were prepared, and the amount of lubricant residue in each sample was measured by the IR method.
TABLE 6
| Mark | Procedure (ii) | Measurement site |
| a | After the wall thickness determining step (before washing) | Outer surface |
| b | After the wall thickness determining step (before washing) | Inner surface |
| c | After the wall thickness determining step (after washing) | Outer surface |
| d | After the wall thickness determining step (after washing) | Inner surface |
| e | After the calibration procedure (before washing) | Outer surface |
| f | After the calibration procedure (before washing) | Inner surface |
| g | After calibration procedure (after washing) | Outer surface |
| h | After calibration procedure (after washing) | Inner surface |
Results and investigation
The analysis results of the respective samples are shown in FIGS. 2a to h.
(1) For the sample after the wall thickness determining step
The outer surface (fig. 2a) and the inner surface (fig. 2b) before washing were compared with the outer surface (fig. 2c) and the inner surface (fig. 2d) after washing.
The peak of the lubricant appearing in the outer surface sample before washing (fig. 2a) disappeared after washing (fig. 2 c). In addition, the wave number in FIG. 2c is 2,900-1The peak observed nearby is lower than that at wave number of 3,800-1Generated by a metal surface observed nearbyThe interference peak is therefore considered not to be a peak generated by the residue of the lubricant but to be an interference peak generated by the metal surface.
From this, it is understood that the lubricant used in the thickness determining step can be sufficiently washed by the washing method used in the method for manufacturing a thin metal tube according to the present invention.
(2) For the sample after the correction process
The outer surface (fig. 2e) and the inner surface (fig. 2f) before washing were compared with the outer surface (fig. 2g) and the inner surface (fig. 2h) after washing.
The peaks of the lubricant appearing in the outer surface sample before washing (fig. 2e and 2f) disappeared after washing (fig. 2g and 2 h).
From this, it is understood that the method for washing used in the method for manufacturing a metal capillary tube according to the present invention can sufficiently wash the lubricant used in the straightening step.
Since the straightening step is the final step, it is found that the use of the washing method used in the method for manufacturing a metal narrow tube according to the present invention eliminates the residue of the lubricant used in the machining step in the product.
Claims (13)
1. A method for manufacturing a thin metal tube used in a medical device including an injection needle, comprising:
a pipe-making step of forming a metal pipe blank by working a flat metal plate,
a wall thickness determining step of processing the metal shell obtained in the tube forming step to a predetermined wall thickness using a water-soluble lubricant, the wall thickness determining step including a processing method selected from the group consisting of drawing, extruding, forging, and rolling, and a combination of 2 or more thereof, and
a washing step of performing an air test for testing the metal narrow tube obtained in the thickness determination step for the presence of damage to the metal narrow tube using an aqueous washing liquid, and washing the metal narrow tube using the aqueous washing liquid;
wherein the water-soluble lubricant comprises medium-chain chlorinated paraffin, a surfactant, a synthetic oil, and the balance is composed of unavoidable impurities.
2. The method for manufacturing a metal tubule according to claim 1, comprising:
the wall thickness determining step and the washing step are repeated a plurality of times until the predetermined wall thickness is reached.
3. The method for manufacturing a metal tubule according to claim 1 or 2, further comprising:
an annealing step of subjecting the metal pipe to heat treatment after the pipe making, the wall thickness determination and the washing,
A tube drawing step of elongating the metal tube obtained in the annealing step to a predetermined outer diameter, and
and a straightening step of machining the metal pipe obtained in the pipe drawing step into a predetermined shape.
4. The method for manufacturing a metal tubule according to claim 1 or 2, wherein,
the aqueous washing solution is water.
5. The method for manufacturing a metal tubule according to claim 1 or 2, wherein,
the water-soluble lubricant comprises 70-90 wt% of medium-chain chlorinated paraffin, 5-15 wt% of surfactant, 5-15 wt% of synthetic oil, and the balance of unavoidable impurities.
6. The method for manufacturing a metal tubule according to claim 1, wherein,
the surfactant is composed of a nonionic surfactant.
7. The method for manufacturing a metal tubule according to claim 6, wherein,
the nonionic surfactant comprises polyoxyethylene fatty acid ester and polyoxyethylene fatty acid ether.
8. The method for manufacturing a metal tubule according to claim 1 or 2, wherein,
the synthetic oil is synthetic oil containing fatty acid methyl ester and/or fatty acid amide.
9. The method for manufacturing a metal tubule according to claim 1 or 2, wherein,
the metal is selected from the group consisting of stainless steel, titanium-nickel alloys, tantalum, niobium, and cobalt-chromium alloys and combinations thereof.
10. The method for manufacturing a metal tubule according to claim 9, wherein,
the metal is stainless steel.
11. The method for manufacturing a metal tubule according to claim 1 or 2, wherein,
the washing step is carried out using an aqueous washing solution at 20 to 95 ℃.
12. The method for manufacturing a metal tubule according to claim 1 or 2, further comprising:
the washing is performed by spray washing, and then the washing liquid is switched to air and the inside of the metal capillary is dried.
13. The method for manufacturing a metal tubule according to claim 1 or 2, wherein,
the aqueous cleaning solution contains a surfactant.
Applications Claiming Priority (3)
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| JP2016-101728 | 2016-05-20 | ||
| JP2016101728 | 2016-05-20 | ||
| PCT/JP2017/018515 WO2017200002A1 (en) | 2016-05-20 | 2017-05-17 | Method of manufacturing thin metal tube |
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| CN109641252A CN109641252A (en) | 2019-04-16 |
| CN109641252B true CN109641252B (en) | 2020-07-28 |
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| JP (1) | JP6393839B2 (en) |
| KR (1) | KR101987360B1 (en) |
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| JP2758813B2 (en) * | 1993-11-04 | 1998-05-28 | 出光興産株式会社 | Capillary washing method and apparatus |
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| JP2013034611A (en) * | 2011-08-05 | 2013-02-21 | Iken Kogyo:Kk | Method for manufacturing eyeless suture needle |
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| JPH01116000A (en) * | 1987-10-29 | 1989-05-09 | Ryusaburo Koreeda | Aqueous solution |
| JP2010265462A (en) * | 1998-03-13 | 2010-11-25 | Chugoku Marine Paints Ltd | Antifouling coating material composition, antifouling coating film, ship or submerged structure covered with the film, and antifouling method of shell of ship or submerged structure |
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| JP6209454B2 (en) | 2014-01-24 | 2017-10-04 | 新日鐵住金株式会社 | Drawing lubricant, drawing method, and metal tube manufacturing method |
| JP6369743B2 (en) | 2014-03-05 | 2018-08-08 | 日立金属株式会社 | Stainless steel foil manufacturing method |
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2017
- 2017-05-17 KR KR1020187032235A patent/KR101987360B1/en active IP Right Grant
- 2017-05-17 CN CN201780044087.4A patent/CN109641252B/en active Active
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| JP2758813B2 (en) * | 1993-11-04 | 1998-05-28 | 出光興産株式会社 | Capillary washing method and apparatus |
| JPH09217073A (en) * | 1996-02-08 | 1997-08-19 | New Japan Chem Co Ltd | Lubricant oil for metal processing |
| JPH10298577A (en) * | 1997-04-25 | 1998-11-10 | Kao Corp | Lubricant composition |
| JP3738643B2 (en) * | 2000-03-02 | 2006-01-25 | 住友金属工業株式会社 | Lubricant composition for cold plastic working of steel |
| CN101812364A (en) * | 2002-12-26 | 2010-08-25 | 松下电器产业株式会社 | Water-soluble lubricant, metal working method and apparatus suitable for using the same |
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| JP2013034611A (en) * | 2011-08-05 | 2013-02-21 | Iken Kogyo:Kk | Method for manufacturing eyeless suture needle |
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| JP6393839B2 (en) | 2018-09-19 |
| WO2017200002A1 (en) | 2017-11-23 |
| KR101987360B1 (en) | 2019-06-10 |
| JPWO2017200002A1 (en) | 2018-05-31 |
| CN109641252A (en) | 2019-04-16 |
| KR20180125603A (en) | 2018-11-23 |
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