KR20200106877A - Apparatus and method for producing a product using the autoclave - Google Patents

Abstract

The present invention relates to a method and apparatus for producing a product using an autoclave. In particular, in order to satisfy the difficult molding conditions, the temperature and pressure conditions inside the autoclave are sensed in real time, and the conditions of the product to be molded are automatically set, thereby being capable of producing products of the same quality at low cost by reducing the temperature and pressure deviation inside the autoclave.

Description

Apparatus and method for producing a product using the autoclave}

According to one disclosure, the present invention relates to a technology capable of producing a product of uniform quality at a low cost by maintaining a constant temperature and pressure using an autoclave.

Autoclave is a collective term for a high-pressure reactor and means a heat-resistant and pressure-resistant container capable of chemical treatment such as synthesis, decomposition, sublimation, and extraction under high temperature and high pressure for industrial and research purposes.

Since the autoclave must have a uniform internal temperature and pressure, the internal fan is rotated to circulate hot air, and the inside of the autoclave must maintain a constant pressure, so the fan is driven using a magnetic drive for airtightness. It is common to do.

A conventional autoclave using a magnetic drive uses a magnetic drive and a motor separately provided as a means to operate it.Since the motor and the magnetic drive are connected using pulleys or couplings, they take up a lot of space and cause noise. Is done. In addition, since the magnetic drive loses its magnetism when the temperature increases due to the influence of the internal temperature of the autoclave, a heat exchange space is placed inside the magnetic drive and the magnetic drive is cooled by cooling water or industrial water. As a result, additional devices such as a cooling device and cooling water are required, thus taking up more space.

In addition, the hot air circulating inside the autoclave has a problem that it is difficult to maintain a uniform temperature inside the autoclave because it is not transmitted evenly inside the autoclave due to the resistance caused by the materials to remove air bubbles. There is a method of manufacturing a gear by high frequency heat treatment. However, during contour high-frequency heat treatment of existing carbon steel and medium carbon-based alloy steel, molten loss occurs at the end of the gear tooth, causing the gear tooth to deform, requiring additional processing and reducing durability.

0001)(KR) Patent Publication 10-2004-0079595 0002)(KR) Registered Patent 10-1344950

Accordingly, the present invention was conceived to solve the above problems. In the present invention, a method and apparatus capable of efficiently manufacturing a product while maintaining high temperature and high pressure inside the autoclave by using a plurality of temperature sensors are manufactured. There is a purpose in doing.

According to the first embodiment, a method of producing a product using an autoclave is disclosed, which is a basic condition for molding a product, based on the material of the product and the molding method, the internal temperature, pressure, and pressure of the autoclave. Setting the internal environment including humidity and air components, bisphenol A epoxy 20 to 30 parts by weight, bisphenol F epoxy resin 20 to 30 parts by weight, carbon black 10 to 15 parts by weight bentonite 30 to 40 parts by weight, triethylene Into an epoxy resin composition containing 0.1 to 1 parts by weight of a tetraamine curing catalyst, 3 to 10 parts by weight of diethylamino propylamine, and 7 to 10 parts by weight of sodium carbonate, 2.5 times the weight of the epoxy resin composition is added and mixed. In the step of generating, the raw material composition is put into an autoclave, and the first high-pressure hydrothermal process is performed at a temperature of 100 to 130°C and a pressure of 0.1 to 0.4 MPaG, and a temperature of 150 to 190°C and 0.2 After performing the second high-pressure hydrothermal reaction at a pressure of ~0.4 MPaG, and performing the third high-pressure hydrothermal reaction at a temperature of 210 to 280°C and a pressure of 0.4 to 0.5 MPaG, the temperature of 300 to 350°C and 0.1 to A step of obtaining a reaction composition by performing a fourth high-pressure hydrothermal reaction under a pressure of 0.2 MPaG. Using a plurality of temperature sensors and a plurality of pressure sensors installed inside the autoclave, the temperature inside the autoclave and The step of measuring the pressure, when the autoclave is at a temperature of 100 to 150°C and a pressure of 0.25 to 0.35 MPaG, inserting the mold of the product into the autoclave and fixing it, setting the temperature inside the autoclave to 100 to The step of converting the interior of the autoclave into a vacuum state with a vacuum degree of 10 ^-2 torr or less while maintaining at 150°C. The reaction composition is injected into the mold of the product, and the temperature inside the autoclave is maintained in a vacuum state. The step of increasing to 300℃, after placing the mold of the product inside the molding room, 10 The step of forming a product by applying a pressure of kg/cm ² to 500 kg/cm ² , while maintaining the inside of the autoclave in a vacuum state, lowering the temperature inside the autoclave to 20 to 30°C, The step of removing air bubbles and moisture, and the molded product can be separated from the mold of the product and transferred to the outside of the autoclave.

According to a second embodiment, a device for producing a product using an autoclave is provided, and the device includes a molding room for molding a product, a control unit, and a memory including instructions executed by the control unit, and the control unit is , As a basic condition for molding a product, based on the material and molding method of the product, the internal environment including the internal temperature, pressure, humidity and air components of the autoclave is set, and 20 to 30 parts by weight of bisphenol A epoxy, bisphenol F Epoxy resin 20 to 30 parts by weight, carbon black 10 to 15 parts by weight Bentonite 30 to 40 parts by weight, Triethylene tetraamine curing catalyst 0.1 to 1 parts by weight, Diethylamino propylamine 3 to 10 parts by weight and Sodium carbonate 7 to To an epoxy resin composition containing 10 parts by weight, 2.5 times the weight of the epoxy resin composition was added and mixed to form a raw material composition, and the raw material composition was placed in an autoclave, and a temperature of 100 to 130°C and 0.1 to 0.4 MPaG The first high-pressure hydrothermal process was carried out under pressure, and the second high-pressure hydrothermal reaction was carried out at a temperature of 150 to 190°C and a pressure of 0.2 to 0.4 MPaG, and a temperature of 210 to 280°C and 0.4 After performing the third high pressure hydrothermal reaction at a pressure of ~0.5 MPaG, the fourth high pressure hydrothermal reaction was carried out at a temperature of 300 to 350°C and a pressure of 0.1 to 0.2 MPaG to obtain a reaction composition, and then inside the autoclave. When the temperature and pressure inside the autoclave are measured once every 2 seconds using a plurality of installed temperature sensors and a plurality of pressure sensors, and the interior of the autoclave is at a temperature of 100 to 150°C and a pressure of 0.25 to 0.35 MPaG, After inserting the mold of the product into the autoclave, fix it, and while maintaining the temperature inside the autoclave at 100 to 150℃, convert the inside of the autoclave into a vacuum with a degree of vacuum of 10-2torr or less, and convert the reaction composition into the mold of the product. To the inside of the autoclave and keep the inside of the autoclave under vacuum. After increasing the temperature to 300°C and putting the mold of the product inside the molding room, the product is molded by applying a pressure of 10 kg/cm2 to 500 kg/cm2, and the autoclave is maintained in a vacuum state. By lowering the internal temperature to 20~30℃, it is possible to generate a command to remove air bubbles and moisture contained in the molded product, separate the molded product from the mold of the product and transfer it to the outside of the autoclave.

According to the present invention by one disclosure, it is possible to efficiently adjust the internal conditions of the autoclave, which must meet difficult temperature and pressure conditions in order to produce products of uniform quality.

According to one disclosure, by using a plurality of devices for controlling the temperature inside the autoclave and a plurality of devices for maintaining the internal pressure, the inner surface is in a pressurized state, while supplying air with air to meet the difficult conditions, thereby achieving a stable speed and You can produce products with efficiency.

By heating the saturated steam at the beginning of the day to make superheated steam and using it, the pressure range on the lower pressure side than the saturated steam pressure is covered, and as a result, it is possible to control the pressure and temperature in a full range. , Due to the supply of a large amount of heat by superheated steam, temperature variation in the molding chamber is difficult to occur, and the curing time of the composite material can be drastically reduced. In addition, it has the advantage that it can be implemented by improving the already installed autoclave.

1 is a view schematically showing an apparatus for producing a product using an autoclave according to one disclosure.
2 is a flow chart showing a method of producing a product using an autoclave according to one disclosure.
3 is a view showing a pattern diagram showing a change in time for controlling the temperature and pressure of the autoclave device according to one start.
4 is a flow chart illustrating a method of forming a product using an autoclave according to one disclosure.
5 shows an embodiment showing an apparatus for producing a product using the autoclave of the present invention.

Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings so that those of ordinary skill in the art can easily implement the present invention. However, the present invention may be implemented in various different forms and is not limited to the embodiments disclosed below. In addition, parts irrelevant to the present invention are omitted in the drawings in order to clearly disclose the present invention, and the same or similar reference numerals denote the same or similar components in the drawings.

Objects and effects of the present invention may be naturally understood or more clearly understood by the following description, and the objects and effects of the present invention are not limited only by the following description.

Objects, features and advantages of the present invention will become more apparent through the following detailed description. In addition, in describing the present invention, when it is determined that a detailed description of a known technology related to the present invention may unnecessarily obscure the subject matter of the present invention, a detailed description thereof will be omitted. Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.

1 is a view schematically showing an apparatus for producing a product using an autoclave according to one disclosure.

It is preferable that the autoclave molding apparatus of the present invention is implemented as follows.

As a supplementary pressurization source necessary for molding, it is preferable to provide compressed air supply means 33 for supplying air or nitrogen or a mixture gas thereof having a predetermined pressure higher than the saturated steam pressure to the molding chamber.

In this way, it is configured to be able to add air or nitrogen of a predetermined pressure to be supplemented, or a mixed gas thereof, so that the pressure and temperature for molding can be easily controlled.

Further, as a heating source and a predetermined pressurization source, a saturated steam heating means 35 for heating the saturated steam having a predetermined pressure required for the composite material 13, the saturated steam heating means 35 are included, and the saturated steam is heated. Accordingly, it is preferable to provide superheated steam supply means 36 for supplying the superheated steam having a predetermined temperature higher than the saturated steam and then supplying it to the molding chamber.

Thereby, the pressure range on the lower pressure side than the saturated water vapor pressure is covered, and as a result, the pressure and temperature can be controlled in the full range. Further, due to the supply of a large amount of heat by the superheated water vapor, the temperature in the molding chamber It exhibits a remarkable effect that it is unlikely to cause variation, and that the curing time of the composite material can be significantly shortened. In addition, it has the advantage that it can be implemented by improving the already installed autoclave device.

In the saturated steam supply means 32, a pressure reducing valve 23 for obtaining a desired pressure is installed, and an automatic valve for passing main steam 24 and an automatic temperature control valve 25 are connected in parallel. The pressure reducing valve 23, the main steam passing automatic valve 24, and the temperature control automatic valve 25 are preferably configured to be controlled by the control means 34.

By providing these valves, it is easy to individually control the temperature and pressure control of the molding chamber 1, and the control is easily performed.

A plurality of nozzles 7 for supplying saturated water vapor into the molding chamber 1 are disposed so as to be able to spray almost all of the composite material 13, and the nozzle 7 is provided with air or nitrogen at a predetermined pressure. Alternatively, it is preferable to serve as a nozzle for supplying these mixed gases.

By constituting in this manner, by using both of the nozzles in this way, the heat quantity supply point and the pressure supply point can be made the same place while simplifying the structure, and the distribution variation of pressure temperature is reduced.

A preferred embodiment of the autoclave molding method and apparatus according to the present invention will be described in detail with reference to the drawings. This device is mainly composed of a molding chamber (1), a drying chamber (2), a water ring vacuum pump (3), a control panel (4), an automatic conveyance line (conveyor) (5), a boiler (6), and a connection between them. It is composed of a pipe and a plurality of valves described later, but has the following configuration.

That is, a composite material 13 in which a fiber base material (here, carbon fiber) is impregnated with a thermosetting resin (here, an epoxy resin) as a matrix is accommodated in a vacuum bag 15 and installed in the molding chamber 1 and heated. Saturated steam supply means 32 for supplying saturated steam at a predetermined temperature (here, 130°C) required for the composite material 13 as a heating source and a predetermined pressurizing source to the molding chamber 1, and , Air (or nitrogen or a mixture gas thereof) of a predetermined pressure (here, 0.31 MPaG. However, MPaG represents a gauge pressure (differential pressure from atmospheric pressure)) as a supplementary pressurization source necessary for molding is used. Compressed air supply means 33 to be supplied to the molding chamber, the supply of these saturated steam and air at a predetermined pressure (or nitrogen or a mixture thereof) is controlled, so that the inside of the molding chamber 1 is required for the composite material 13 It consists of a control means 34 that controls to maintain a predetermined temperature (here, 130°C) and a predetermined pressure (here, 0.3 MPaG).

In the saturated steam supply means 32, a pressure reducing valve for obtaining a desired pressure (here, 0.2 MPaG) for live steam boiled in the boiler 6 (here, 0.4 MPaG, 150°C) ( 23) is installed and the main steam passing automatic valve 24 and the temperature control automatic valve 25 are connected in parallel, and these pressure reducing valves 23, the main steam passing automatic valve 24, and the temperature control automatic valve ( 25) is configured to be controlled by the control means (34).

In addition, a plurality of nozzles 7 for supplying saturated steam into the molding chamber 1 (here, 20/row 2 rows = 40) can be sprayed almost all over the composite material 13 It is excreted (配設). In addition, although described later as a modified example, the nozzle 7 may also serve as a nozzle for supplying air (or nitrogen or a mixed gas thereof) of a predetermined pressure.

The specific configuration of the autoclave device will be described in detail next.

In the molding chamber 1, a plurality of (here, 40) steam nozzles 7 are provided so that saturated steam injected into the molding chamber 1 from the boiler 6 covers the entire molding chamber 1 The having pipe 8 is installed. In addition, a pipe 10 having a plurality of cooling nozzles 9 opened so as to cover the entire molding chamber 1 is installed, similar to the pipe 8 having the steam nozzle 7, and is compressed. An air nozzle 11 opened so that air is injected into the molding chamber 1 is installed. These boilers 6, pipes 8, and steam nozzles 7 constitute the saturated steam supply means 32.

In addition, a drain pipe 12 for draining condensed water droplets and cooling water collected at the bottom of the molding chamber 1, and a composite material 13 are previously placed in a molding mold 14. A vacuum nozzle (16) is installed for preliminary vacuum evacuation of the stacked and wrapped whole with a vacuum bag (15), and a flexible hose (17a) connected to the vacuum nozzle (16) is installed. ) And a vacuum coupler 18 for connecting the vacuum bag 15 to each other. In addition, a door 19 for sealing the molding chamber 1 and an opening and closing device 20 for the door 19 are provided.

In this embodiment, the composite material 13 is a laminate of carbon fibers, and an epoxy resin is used as the thermosetting resin to be used. In addition, a phenol resin or the like may also be used.

In addition, although nylon is used here as a constituent material of the vacuum bag 15, it is good to have heat resistance and water resistance, such as silicone rubber.

In addition, as the constituent material of the molding frame 14, FRP is used here, but compared to the mold used in a hot press device, a built-in heating source is unnecessary, and the thickness and strength of the frame are also caused by saturated steam and compressed air. Since the pressure is solved to the minimum required, various materials such as pearl board and gypsum can be selected.

In the drying chamber 2, blowers 21 and 22 for heating the inside of the drying chamber 2 are installed outside the drying chamber 2, and the vacuum bag 15 conveyed by the automatic conveying line 5 ) To fit into the drying room (2).

The water-sealed vacuum pump 3 is a vacuum pump that performs suction, compression, and exhaust by rotating a blade vehicle by means of sealed water. Unlike the oil circulation type vacuum pump, the water ring type vacuum pump 3 does not cause oil to be transmitted to the vacuum piping to pollute the inside of the molding chamber 1.

The control panel 4 is an operation panel for controlling a series of processes (adjusting the supply of saturated steam, compressed air, etc.) for automatic conveyance and molding of the vacuum bag 15 to be described later, and a pressure reducing valve for controlling the above-described steam. (23), automatic valve for passing main steam (24), automatic temperature control valve (25), pressure reducing valve for compressed air control (29), automatic air introduction valve (30), door opening and closing device (20), automatic cooling water introduction A control means 34 is constituted, including operation mechanisms such as a valve 26, an automatic drain and drainage valve 31, and a vacuum pump 3.

The automatic conveyance line 5 automatically conveys the composite material 13 on-line by stacking the composite material 13 on the forming mold 14 offline and wrapping the entire material in a vacuum bag 15 to remove the pre-vacuum on-line. And a conveying line (conveyor) for automatically carrying in and out of the drying chamber 2 and for automatically conveying the vacuum bag 15 to a place (not shown) for removing the molded product from the mold.

Next, a piping system including a valve will be described.

The steam pipe 8 leading to a pipe having a plurality of steam nozzles 7 is a pipe for sending saturated steam boiled in the boiler 6, in order from the upstream, and a pipe from the boiler 6 It leads to a pressure reducing valve 23 for reducing the vapor pressure to the original pressure from the flange connecting the. From there, the main steam passage automatic valve 24 which controls the amount of steam and has the main role of increasing the temperature, and the temperature control automatic valve 25 which has the main role of maintaining the predetermined temperature are connected in parallel. Further, the pipe 8 extends from there and leads to the pipe 8 of the steam nozzle 7.

The cooling pipe 10 leading to a pipe having a plurality of cooling nozzles 9 is a pipe for sending cooling water from a water tank (not shown), and an automatic cooling water introduction valve that controls the water quantity from a flange connecting the pipes from the water tank It is connected to 26 and leads to a pipe 10 having a cooling nozzle 9.

Next, the air pipe 27 leading to the pipe having the air nozzle 11 is a pipe for sending compressed air from the compressor 28, and from a flange connecting the pipe from the compressor 28 It leads to a pressure reducing valve 29 for reducing the air pressure to the original pressure, an automatic air introduction valve 30 for controlling the amount of air, and a pipe 27 having an air nozzle 11.

These compressors 28, air pipes 27, and air nozzles 11 constitute compressed air supply means 33. In addition, nitrogen is used alone instead of compressed air in some cases, but it is referred to as compressed air supply means here.

In the drain pipe 12, a drain hole is disposed at the bottom of the molding room 1 to drain condensed water droplets or cooling water collected at the bottom of the molding room 1, from which the pipe 12 extends downward. A drainage and drainage automatic valve 31 for draining out and draining is connected to a drain tank (not shown). In addition, the automatic drain and drain valve 31 also serves as an action (exhaust) to pull out the pressure in the molding chamber 1.

Next, a vacuum line leading to the vacuum nozzle 16 is arranged to couple the water ring type vacuum pump 3 and the vacuum nozzle 16 in the forming chamber 1. The water-sealed vacuum pump 3 is a device that performs suction, compression, and exhaust by rotating the blade difference in the casing by feeding water into the pump. The flexible hose 17a is connected to the vacuum nozzle 16, and the vacuum coupler 18 is connected to the opposite side. There is an exhaust port of the vacuum bag 15 in front, and the exhaust port and the vacuum coupler 18 are connected with a flexible hose 17b, and the remaining air in the vacuum bag 15 is discharged by the vacuum pump 3. .

Next, the flow of the vacuum bag 15 will be described with reference to FIG. 2. Fig. 2 is a schematic plan view showing the entire apparatus of the present invention. The composite material 13 is laminated on a molding mold at a bagging site, and it is inserted into the vacuum bag 15 to perform preliminary vacuum evacuation (bagging step). The pre-vacuum bag 15 is placed at the start position of the automatic transfer line 5, and the control panel 4 sets a predetermined temperature, pressure, and time, and the automatic transfer starts by pressing the automatic transfer start button. do.

The vacuum bag 15 flows from left to right in FIG. 2 and temporarily stops when it reaches the stage in front of the molding chamber 1, and the stage integrated with the door 19 is in the door opening and closing device 20. As a result, it enters the molding chamber 1 with the vacuum bag 15 mounted thereon, and the molding chamber 1 is sealed by the door 19. When the vacuum bag 15 reaches a predetermined position, it is connected to the vacuum nozzle 16 by the vacuum coupler 18, and this vacuum evacuation is started (molding chamber loading step). The molding process will be described later, and the vacuum bag 15, which has completed the exhaust cooling process, is taken out from the molding room, moved to the right again by the automatic transfer line 5, and carried into the drying room 2 (drying room Import process). Dry the vacuum bag 15 in the drying chamber 2 (drying process), and when the drying process is completed, the vacuum bag 15 is moved to the right again by the automatic transfer line 5, and the vacuum bag 15 stops at the stop position. . The vacuum bag 15 is moved to a release location, where the vacuum bag 15 is disassembled, and the molded product is removed from the mold (release process).

However, in this case, the vacuum bag 15 is dried in the drying chamber 2, but it is also possible to dry the surroundings of the vacuum bag 15 in the molding chamber 1 by vacuum removal. In that case, the drying chamber 2 can be omitted.

2 is a flow chart showing a method of producing a product using an autoclave according to one disclosure.

As a basic condition for molding a product in block 101 according to one disclosure, a step of setting an internal environment including an internal temperature, pressure, humidity, and air component of the autoclave based on the material and molding method of the product may be provided. have.

Bisphenol A epoxy 20 to 30 parts by weight, bisphenol F epoxy resin 20 to 30 parts by weight, carbon black 10 to 15 parts by weight bentonite 30 to 40 parts by weight, triethylene tetraamine curing catalyst 0.1 to 1 In an epoxy resin composition containing 3 to 10 parts by weight of diethylamino propylamine and 7 to 10 parts by weight of sodium carbonate, 2.5 times the weight of the epoxy resin composition is added and mixed to provide a step of producing a raw material composition. I can.

In block 103 according to the start of the day, the raw material composition was put into an autoclave, and the first high-pressure hydrothermal process was performed at a temperature of 100 to 130°C and a pressure of 0.1 to 0.4 MPaG, and a temperature of 150 to 190°C. And a second high-pressure hydrothermal reaction at a pressure of 0.2 to 0.4 MPaG, a third high pressure hydrothermal reaction at a temperature of 210 to 280°C and a pressure of 0.4 to 0.5 MPaG, and then a temperature of 300 to 350°C and It is possible to provide a step of obtaining a reaction composition by performing a fourth high-pressure hydrothermal reaction under a pressure of 0.1 to 0.2 MPaG.

At this time, the fourth high-pressure hydrothermal reaction is performed in a mixture of 10:90~90:10 v/v of water and ethanol at a temperature of 330°C and stirring at 1~100rpm for 2~3 hours while stirring the polymer material. Can be removed.

In block 104 according to one disclosure, a step of measuring the temperature and pressure inside the autoclave once every 2 seconds using a plurality of temperature sensors and a plurality of pressure sensors installed inside the autoclave may be provided.

In block 105 according to one disclosure, when the interior of the autoclave is at a temperature of 100 to 150°C and a pressure of 0.25 to 0.35 MPaG, a step of inserting a mold of the product into the interior of the autoclave and fixing it may be provided.

In block 106 according to one disclosure, a step of converting the inside of the autoclave into a vacuum state of 10 ^-2 torr or less may be provided while maintaining the temperature inside the autoclave at 100 to 150°C.

In block 107 according to one initiation, a step of increasing the temperature inside the autoclave to 300° C. may be provided by injecting the reaction composition into the mold of the product and maintaining the inside of the autoclave in a vacuum state.

In block 108 according to one disclosure, after placing a mold of the product into the interior of the molding room, a step of molding the product may be provided.

According to one disclosure, the step of molding the product may provide a step of blowing argon gas into the interior of the autoclave at a flow rate of 150 to 180 Nm 3 /hr.

In addition, it is possible to provide a step of performing vacuum de-treatment for 20 to 30 minutes at a vacuum degree of 10 ^-2 torr or less. At this time, the interior of the autoclave is made into a vacuum state, but the pressure in the molding chamber is treated differently to increase the completeness of the product to be molded. In other words, the pressure inside the molding chamber may be different from the inside of the autoclave.

In addition, it may include cooling the mold of the de-treated product, applying a pressure of 10 kg / cm ² to 500 kg / cm ² to gradually solidify the reaction composition to form the product.

According to one disclosure, the step of forming the product may include the following processes.

By the start of work, the saturated steam having a pressure of 0.4 MPaG and a temperature of 150°C is depressurized, changed to a pressure of 0.1 MPaG and a temperature of 120°C, and heated to generate superheated steam having a pressure of 0.1 MPaG and a temperature of 130°C. You can provide the process of making.

According to one disclosure, it is possible to provide a heating process in which superheated steam is introduced into the molding chamber and the temperature is raised to 90°C.

By one start, by automatically opening and closing the temperature control valve and the drain drainage automatic valve of the autoclave, it is possible to provide a dwell process in which the molding chamber is maintained at 90°C for 1 to 1.5 hours.

At the beginning of the day, the automatic drain and drain valve is opened and closed. If the pressure inside the molding room is 0.095 MPaG or less, the automatic drain drainage valve is closed, and if the pressure inside the molding room is 0.095 MPaG or more, the automatic drain and drainage valve is opened. It is possible to provide a pressure boosting process in which the temperature is 130°C and the pressure is 0.1 MPaG.

By one start, it is possible to provide a curing process in which water vapor is automatically supplied so that the temperature and pressure inside the molding chamber are maintained until a predetermined curing time elapses.

By the start of work, after the curing process is completed, external air is injected by setting the set value of the automatic drainage valve to 0.2MPaG, and when the temperature inside the molding room is less than 100℃, the compressed air inside the molding room is discharged to the outside. And, a method for producing a product using an autoclave, characterized in that it further comprises an exhaust cooling process for discharging the cooling water.

By the beginning, the curing process senses the temperature and pressure inside the molding room inside the autoclave in real time, and if the temperature inside the molding room is 130°C and the pressure is not maintained at 0.1 MPaG, the water vapor injected into the molding room By controlling the amount, it is characterized in that the temperature inside the autoclave is maintained at 130° C. and the pressure is 0.1 MPaG for a predetermined curing time.

As a supplementary pressurization source necessary for molding, air or nitrogen or a mixture thereof of a predetermined pressure higher than the saturated water vapor pressure is supplied to the molding chamber, and supply of the saturated water vapor and air or nitrogen or a mixture thereof of a predetermined pressure is controlled, At least one of the temperature and pressure is controlled to perform the curing process so that the inside of the molding chamber is maintained at a predetermined temperature and pressure required for the composite material.

In this way, it is easy to control the pressure and temperature for molding by adding air or nitrogen or a mixed gas of a predetermined pressure to be supplemented.

In addition, air of a predetermined pressure, nitrogen, or a mixture of these gases used as a supplementary pressurization source may be at room temperature, or may be preheated to a predetermined temperature. And when using a mixed gas, the mixing ratio may be freely selected.

In addition, as a heating source and a pressurizing source of a predetermined pressure, saturated steam of a predetermined pressure required for the composite material is heated to make superheated steam having a predetermined temperature higher than the saturated steam, and then supplied to the molding chamber, and the inside of the molding chamber It is preferable to perform the curing step by controlling at least one of the temperature and pressure so as to be maintained at a predetermined temperature and pressure required for this.

In addition, when supplemented and described, in general, saturated steam contains very little moisture, so it is referred to as wet saturated steam or wet steam. When 1 kg of wet steam contains x kg of dry saturated steam and (1-x) kg of moisture, x is called dryness and (1-x) is called humidity. Next, heating the dried saturated steam further increases the temperature. Water vapor having a temperature higher than the temperature equivalent to the saturated water vapor pressure is called superheated water vapor. Saturated water vapor is white steam, while superheated water vapor is a colorless, transparent gas, and does not condense until it reaches the saturation temperature. When superheated water vapor is blown onto a substance, its surface temperature rises, and the moisture contained in the substance evaporates. Using this property, it is applied to dryers and cookers.

The superheated steam used in the present invention can be used, for example, by heating saturated steam at 100°C and 0.1 MPa (standard or atmospheric pressure) to create superheated steam at 130°C and 0.1 MPa.

In addition, the molding chamber is partially opened, only saturated steam is supplied, the temperature of the molding chamber is raised to a predetermined temperature, and then the dwell process is maintained for a predetermined time, and then the molding chamber is sealed, and saturated steam and air of a predetermined pressure are applied, or It is preferable to supply nitrogen or a mixture of these gases to transfer from the boosting step to the curing step.

Thereby, by heating the saturated steam to make superheated steam and using it, the pressure range on the lower pressure side than the saturated steam pressure is covered, and as a result, it becomes possible to control the pressure and temperature in a full range. Due to the supply of a large amount of heat by superheated steam, temperature variation in the molding chamber is difficult to occur, and the curing time of the composite material can be significantly shortened. In addition, it has the advantage that it can be implemented by improving the already installed autoclave.

In addition, the step of molding the product may increase the bonding strength by mixing and molding polyvinyl alcohol in a ratio of 3 to 14 wt% based on the weight of the reaction composition.

In block 109 according to one disclosure, a step of removing air bubbles and moisture contained in the molded product may be provided by lowering the temperature inside the autoclave to 20 to 30° C. while maintaining the inside of the autoclave in a vacuum state.

It is possible to provide a step of separating the product molded in block 110 according to one disclosure from the mold of the product and transferring it to the outside of the autoclave.

3 is a view showing a pattern diagram showing a change in time for controlling the temperature and pressure of the autoclave device according to one start.

4 is a flow chart illustrating a method of forming a product using an autoclave according to one disclosure.

Next, an example of the autoclave molding process will be described with reference to FIGS. 3 and 4. 3 is a pattern diagram showing a time change for controlling the temperature and pressure of the present invention, and a chart diagram of the pressures of saturated steam, compressed air, and exhaust that are linked in synchronization with the progress of the pattern diagram. Show. However, the vertical axis of the chart shows the gauge pressure (differential pressure from atmospheric pressure). 4 shows a flow chart of the molding process.

In advance, the boiler 6 prepares saturated steam at a source pressure of 0.4 MPaG and 150°C, and the pressure is reduced to 0.2 MPaG by a pressure reducing valve 23. The amount of steam is controlled by the main steam passage automatic valve 24, and the automatic drain and drain valve 31 is opened to introduce saturated steam into the molding chamber 1 under no pressure (atmospheric pressure) to raise the temperature to 90°C ( Heating process).

Next, 90° C. is maintained for 1 to 1.5 hours by appropriate opening/closing of the automatic temperature control valve 25 and the exhaust according to the opening of the automatic drain and drainage valve 31 (dwell process).

Next, once the automatic drain and drain valve 31 is closed, the exhaust pressure is set to 0.3 MPaG, and when the molding chamber 1 is 0.295 MPaG or less, the automatic drain and drain valve 31 remains closed, and is 0.305 MPaG or more. When it becomes, the automatic drain and drainage valve 31 is opened, and when it becomes 0.295 MPaG or less, the automatic drain and drainage valve 31 is closed. As curing conditions, the target temperature and pressure are set so that the ambient temperature in the molding chamber 1 is 130°C and 0.3 MPaG. Again, the main steam passage automatic valve 24 is operated to introduce saturated steam to raise the temperature to 130°C. There is no pressure (atmospheric pressure) up to 100°C, but when it exceeds 100°C, the pressure in the molding chamber 1 rises, and the pressure reaches 0.2 MPaG, which is the saturated water vapor pressure at 130°C.

When the ambient temperature in the molding chamber 1 reaches 130° C., compressed air of slightly higher than 0.3 MPaG, for example, 0.31 MPaG, is introduced. The reason is that when the pressure of the compressed air is lower than the pressure in the molding chamber 1, the air does not enter the molding chamber. Compressed air is also determined by the capability of the compressor 28, similar to saturated steam, but, for example, 0.6 MPaG of compressed air is supplied from the compressor 28 to the air pipe 27, and the pressure reducing valve 29 It is reduced to 0.31 MPaG by The pressure in the molding chamber 1 compensates for the insufficient pressure with compressed air, and immediately reaches 0.3 MPaG (pressure boosting step).

Then, the atmosphere temperature in the molding chamber 1 is maintained at 130° C. and the pressure is maintained at 0.3 MPaG, and the state is maintained for a predetermined curing time. The curing time is determined by the composite material 13. For example, in the case of a conventional composite material 13 using the thermosetting resin of this example as a substrate, reaction curing is completed in about 1 hour. However, the temperature in the molding chamber 1 decreases if left unattended due to heat absorption by the introduced air, heat absorption of the molding target product (composite material 13) or the molding chamber 1, and heat dissipation from the molding chamber. Therefore, it is necessary to properly introduce steam. Further, when the pressure in the molding chamber 1 decreases, when the temperature in the molding chamber 1 reaches 130°C, it is necessary to introduce air.

Therefore, when the temperature in the molding chamber 1 is 130° C. and the pressure is 0.3 MPaG, the introduction of steam and air is once stopped, but the temperature and pressure in the molding chamber 1 decrease with time due to the above-described reason. Basically, the temperature drop is corrected by introducing water vapor, and the pressure drop is corrected by introducing air. When steam is introduced again, the temperature and pressure in the molding chamber 1 rise, and when the exhaust condition exceeds the set value, the automatic drain and drainage valve 31 opens and the pressure decreases. If the temperature in the molding chamber 1 is 130° C., since water vapor cannot be introduced, air is introduced. Then, the pressure in the molding chamber 1 also increases, and the temperature decreases. Again, the temperature and pressure in the molding chamber 1 are checked, and if it is not 130°C and 0.3 MPaG, it returns to the introduction of steam. In this way, the temperature and pressure in the molding chamber 1 are balanced by supply and exhaust of water vapor and air, and a series of operations are repeated until a predetermined curing time is reached (curing step).

Next, when the curing process is completed, the automatic drain and drain valve 31 is controlled by setting the set value of the automatic drain and drainage valve 31 to 0.2 MPaG, and air is introduced and replaced with air. When the temperature in the molding chamber 1 falls below 100° C., the automatic drain and drain valve 31 is opened to the atmosphere to discharge compressed air in the molding chamber 1 at once. At the same time, cooling water is discharged from the cooling nozzle 9 to cool the vacuum bag 15. The cooling water flowing to the bottom of the molding chamber 1 is discharged to the drain tank through the automatic drain drain valve 31 (exhaust cooling process).

5 shows an embodiment showing an apparatus for producing a product using the autoclave of the present invention.

As shown in Fig. 5, the autoclave of the present invention is a heat-resistant and pressure-resistant device that performs chemical treatment such as synthesis, decomposition, sublimation, and extraction under high temperature and high pressure, and an air system for maintaining a constant pneumatic pressure, a temperature measuring device is an autoclave. It can be installed everywhere to reduce temperature and pressure deviation. Therefore, high quality products can be produced with a uniform error rate.

As described above, all of the steel materials in which the scale layer is formed on the surface of the holding steel material that satisfies the conditions of the present invention can exhibit excellent temporary rust prevention properties under severe atmospheric corrosion environment.

Preferred embodiments of the present invention described above are disclosed for the purpose of illustration, and those skilled in the art with ordinary knowledge of the present invention will be able to make various modifications, changes and additions within the spirit and scope of the present invention. It should be seen as falling within the scope of the above claims.

If a person of ordinary skill in the art to which the present invention pertains, various substitutions, modifications and changes are possible within the scope of the technical spirit of the present invention, so that the present invention is described in the foregoing embodiments and the accompanying drawings. Is not limited by.

In the exemplary system described above, the methods are described on the basis of a flowchart as a series of steps or blocks, but the present invention is not limited to the order of the steps, and certain steps may occur in a different order or concurrently with the steps described above. I can. In addition, those skilled in the art will appreciate that the steps shown in the flowchart are not exclusive, other steps may be included, or one or more steps in the flowchart may be deleted without affecting the scope of the present invention.

Claims (1)

As a basic condition for molding a product, setting an internal environment including an internal temperature, pressure, humidity and air component of the autoclave based on a material and a molding method of the product;
20 to 30 parts by weight of bisphenol A epoxy, 20 to 30 parts by weight of bisphenol F epoxy resin, 10 to 15 parts by weight of carbon black 30 to 40 parts by weight of bentonite, 0.1 to 1 parts by weight of triethylene tetraamine curing catalyst, diethylamino propyl Adding and mixing 2.5 times the weight of the epoxy resin composition into an epoxy resin composition comprising 3 to 10 parts by weight of an amine and 7 to 10 parts by weight of sodium carbonate to form a raw material composition;
Put the raw material composition in the autoclave, perform a first high-pressure hydrothermal process at a temperature of 100 to 130 °C and a pressure of 0.1 to 0.4 MPaG, and a temperature of 150 to 190 °C and a temperature of 0.2 to 0.4 MPaG After performing the second high-pressure hydrothermal reaction at a pressure of 210 to 280°C and a pressure of 0.4 to 0.5 MPaG, the third high pressure hydrothermal reaction is performed at a temperature of 300 to 350°C and a temperature of 0.1 to 0.2 MPaG. Performing a fourth high pressure hydrothermal reaction under pressure to obtain a reaction composition;
Measuring the temperature and pressure inside the autoclave once every 2 seconds using a plurality of temperature sensors and a plurality of pressure sensors installed inside the autoclave;
When the interior of the autoclave is at a temperature of 100 to 150°C and a pressure of 0.25 to 0.35 MPaG, inserting and fixing the mold of the product into the autoclave;
Converting the inside of the autoclave into a vacuum state of 10 ^-2 torr or less while maintaining the temperature inside the autoclave at 100 to 150°C;
Injecting the reaction composition into a mold of the product, maintaining the inside of the autoclave in a vacuum state, and increasing the temperature inside the autoclave to 300°C;
Molding the product after placing the mold of the product into the molding chamber;
Removing air bubbles and moisture contained in the molded product by lowering the temperature inside the autoclave to 20 to 30° C. while maintaining the interior of the autoclave in a vacuum state; And
A method for producing a product using an autoclave comprising the step of separating the molded product from the mold of the product and transferring it to the outside of the autoclave.

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