CN201247194Y - Viewing mirror capable of implementing in situ optical observation under high-temperature and high-pressure liquid circumstance - Google Patents

Abstract

The utility model relates to a viewing mirror structure, in particular to the viewing mirror structure whose sealing is safe and reliable and which can realize the optical original position viewing under the liquid condition of high temperature and high voltage, wherein the highest temperature is 350 DEG C and the highest voltage is 20MPa, which solves the problems of sealing and viewing (observation) under the conditions of high temperature and high voltage. The viewing structure is assembled on an autoclave and comprises a pressure cover, a butterfly-type washer, a flat washer, a lens, an O-shaped ring, a lens cone, a lens seat, a carbon washer, a compression ring and a pressure cover and the like. After parts, such as the pressure cover, the washers, the lens and the like are assembled, the parts extend into the autoclave through the lens seat, then the pressure cover is screwed on the lens seat until the compression ring and the washers are tightly pressed. For guaranteeing the lens structure to stably work for a long time under the liquid condition of high temperature and for realizing the original position optical viewing with high quality, monocrystal Sapphire sheets whose high-temperature strength is high, corrosion stability is good and optical performance is excellent is selected to be used as lens materials. Furthermore, the structure designs the lens cone into a conical shape for adding the light flux for realizing the optical original position viewing.

Description

A sight glass capable of realizing in-situ optical observation in high temperature and high pressure liquid environment

technical field

The utility model relates to a viewing mirror structure, in particular to a viewing mirror structure which is safe and reliable in sealing and can realize in-situ optical observation in a high temperature and high pressure liquid environment.

Background technique

In chemical, food, pharmaceutical fields and laboratories, some reactions are often carried out in a liquid environment with high temperature and high pressure. Due to the harsh reaction conditions, the monitoring of the reaction process can usually only be achieved by indirect means, and it is difficult to obtain direct and reliable information, which makes direct in-situ observation technology very necessary, and optical in-situ observation is one of them. important kind. In order to achieve optical in-situ observation in a high-temperature and high-pressure liquid environment, there must be a detection window leading into the airtight reaction vessel, and opening a detection window on the high-temperature and high-pressure vessel so that the window can work stably for a long time and obtain high-quality observation results requires The window material has good high-temperature performance and optical performance, and can solve the problem of high-temperature and high-pressure sealing. At present, the domestic conventional window design can not withstand high temperature and pressure, and the window design reported in foreign literature is often too expensive and troublesome to install and disassemble.

Utility model content

The purpose of the utility model is to provide a sight glass structure with safe and reliable sealing, which can realize in-situ optical observation under high-temperature and high-pressure liquid environment, and solve the problems of high-temperature and high-pressure sealing in the prior art.

The technical scheme of the utility model is as follows:

A sight glass capable of realizing in-situ optical observation in a high-temperature and high-pressure liquid environment, the sight glass structure includes a pressure cap, a butterfly washer, a flat washer, a lens, an O-ring, a lens barrel, a lens seat, a graphite washer, a pressure ring and The connection relationship between the gland and each part is as follows: the O-ring is placed in the slot on the end face of the lens barrel, the lens is placed flat on the O-ring, the flat washer and the butterfly washer are placed on the lens in turn, the press cap and The front part of the lens barrel is connected by threads, so that the butterfly gasket, flat gasket, lens, O-ring and the end surface of the lens barrel are tightly attached to each other, and the graphite gasket and pressure ring are sleeved on the cylindrical surface of the rear of the lens barrel to form a lens barrel assembly; The base is welded on the autoclave, which is the basis for the installation of the entire lens barrel structure; one end of the assembled lens barrel assembly extends into the autoclave through the lens base, and the other end surface is close to the inner end surface of the lens base; the gland Threaded onto the mirror mount, compressing the ferrule and graphite gasket.

In the sight glass, the lens is made of a single crystal sapphire sheet with high temperature strength, good corrosion resistance and excellent optical performance.

The sight glass is selected from a butterfly washer and a flat washer, and the material of the two washers is Inconel 718 alloy, which has good corrosion resistance and high temperature elasticity.

The sight glass is made of Kalrez O-ring, which is made of high-temperature fluorinated rubber, and the maximum operating temperature is 327°C.

The sight glass is selected from a graphite gasket, which is made of flexible graphite.

In the sight mirror, the lens barrel is a variable cross-section member, the front part is the thinnest, the upper part is threaded, the middle part is the thickest, the middle part is processed into an outer hexagon, and the tail part is processed into a cylindrical surface to place the pressure ring and the graphite gasket; The diameter of the inner surface of the barrel gradually decreases from the tail to the front, showing a bell mouth shape, and there is a groove on the front end of the lens barrel for placing an O-ring.

For the sight mirror, the gland is a member with a variable cross-section. The front part is a cylindrical surface, and the end face is in direct contact with the pressure ring. The middle part of the car has threads to cooperate with the mirror holder. There are threaded holes; the inner surface of the gland is a hole with a taper, and its taper is adapted to the bell mouth in the lens barrel.

The application of the sight glass capable of realizing in-situ optical observation in a high-temperature and high-pressure liquid environment includes the following steps:

(1) Place the lens barrel vertically on a plane, and place the O-ring in the slot on the front face of the lens barrel;

(2) Place the lens flat on the O-ring and keep the two evenly aligned;

(3) Place the flat washer and butterfly washer on the lens in sequence;

(4) Screw the pressure cap into the front of the lens barrel until the inner end surface of the pressure cap flattens the butterfly gasket;

(5) Turn the lens barrel assembled at the front up and down, put the graphite gasket on the cylindrical surface at the end of the lens barrel, and then put the pressure ring on the outermost layer to form the lens barrel assembly;

(6) Place the assembled lens barrel assembly horizontally, and extend into the autoclave through the lens base until the end surface of the middle of the lens barrel contacts the inner end surface of the lens base;

(7) Screw the gland into the mirror holder first, make the gland contact with the pressure ring and press it tightly;

(8) After the mirror structure is installed, put the sample in the autoclave, seal the lid of the autoclave, pass in the reaction medium, pressurize and heat up, and after reaching the parameters required for the reaction, use a long-focus microscope or a Raman spectrometer to see through the autoclave. The sight glass can observe the change of the surface state of the sample in the autoclave in situ or detect the composition change of the product on the surface of the sample.

The beneficial effects of the utility model are:

1. The utility model selects a single crystal sapphire sheet with high temperature strength, good corrosion resistance and excellent optical performance as the lens material, which can ensure that the sight glass is not easy to be crushed or corroded after being in contact with the high-pressure medium, and can be used safely and stably for a long time. work, and the lens has a high light transmittance and can obtain a strong optical signal.

2. This utility model selects two kinds of sealing materials, one is the Kalrez O-ring placed between the lens and the lens barrel, the material of this O-ring is fluorinated rubber, which can maintain good mechanical elasticity below 327°C And chemical stability; Another sealing material is the graphite gasket between the lens barrel and the gland, which is made of flexible graphite and has excellent high-temperature sealing performance. The selection of these two sealing materials can ensure long-term safe and stable sealing.

3. In this utility model, a flat washer and a butterfly washer made of Inconel 718 alloy are placed in front of the lens. Inconel 718 alloy has good corrosion resistance and high temperature elasticity. , The flattened butterfly gasket still has elasticity, so that the lens and the O-ring keep in close contact, and the seal can still be achieved.

4. In the utility model, the inner surfaces of the lens barrel and the gland are designed to have a tapered structure, which can increase the light transmission of the incident light and the outgoing light, and greatly increase the optical signal intensity.

5. The two seals in the utility model adopt self-tightening seals, so there is no need to use a large pre-tightening force to achieve the sealing effect when installing the sight glass, which makes installation and disassembly more convenient.

6. The mirror structure of the utility model can bear pressure not less than 20MPa at room temperature, can work stably below 327°C, and can meet the parameter conditions of high temperature and high pressure experiments. Currently, the mirror structure is used under the conditions of 12.7MPa and 285°C no problems found.

Description of drawings

Figure 1 is an assembly diagram of the mirror structure.

In the figure, 1. Pressure cap; 2. Butterfly washer; 3. Flat washer; 4. Lens; 5. O-ring; 6. Lens barrel; 7. Mirror holder; 8. Graphite washer; , gland; 11, threaded hole; 12, socket; 13, autoclave.

Detailed ways

As shown in Figure 1, the utility model can realize the in-situ optical observation under the environment of high temperature and high pressure liquid, and the structure of the mirror is as follows:

The mirror structure includes a pressure cap 1, a butterfly washer 2, a flat washer 3, a lens 4, an O-ring 5, a lens barrel 6, a lens holder 7, a graphite gasket 8, a pressure ring 9 and a gland 10. The connection relationship is as follows: the O-ring 5 is placed in the groove on the end face of the lens barrel 6; the lens 4 is placed on the O-ring 5; the flat washer 3 and the butterfly washer 2 are placed on the lens 4 in turn; the pressure cap 1 and the The front part of the lens barrel 6 is threaded, so that the lens 4, the O-ring 5 and the end surface of the lens barrel 6 are tightly attached to each other and the butterfly gasket 2 is flattened, so that when the pressure of the liquid in the autoclave 13 rises, the liquid passes through the lens further Compress the O-ring 5, resulting in the deformation of the O-ring 5, so that the contact between the O-ring 5 and the lens 4 is tightly sealed, and a certain number of graphite gaskets 8 and pressure rings 9 are set on the cylindrical surface of the rear of the lens barrel 6, A lens barrel assembly is formed. In this embodiment, the number of graphite gaskets 8 is 7 to 9 pieces. Mirror holder 7 is welded on the still wall of autoclave 13, and it is the foundation that whole lens barrel structure is installed; Assembled lens barrel assembly (pressure cap 1, butterfly washer 2, flat washer 3, lens 4, O-ring 5 , lens barrel 6, etc.) one end extends into the autoclave 13 through the lens base 7, and the middle end face is close to the inner end face of the mirror base 7; the gland 10 is screwed onto the mirror base 7 by threads until the pressure ring is pressed 9 and the graphite gasket 8; like this, when the pressure of the liquid in the autoclave 13 rises, the high-pressure liquid will make the contact between the lens barrel 6, the graphite gasket 8, the pressure ring 9 and the gland 10 more tightly, thereby ensuring the sealing firm.

In order to ensure that the lens barrel structure can work stably for a long time in a high-temperature liquid environment and can achieve high-quality in-situ observation, the lens 4 is made of a single-crystal sapphire plate with high high-temperature strength, good corrosion resistance, and excellent optical performance. .

In order to solve the sealing problem of the sight glass structure under high temperature and high pressure environment, Kalrez O-ring 5 (perfluoroether rubber O-ring produced by DuPont Company of the United States) was selected. The material of this O-ring is high-temperature fluorinated rubber. It can reach 327°C.

In order to solve the sealing problem of the sight glass structure under high temperature and high pressure environment, graphite gasket 8 is selected, which is made of flexible graphite and has excellent high temperature sealing performance.

In order to ensure that the lens 4 and the O-ring 5 can still keep sealed when the mirror structure returns from the high temperature and high pressure environment to the normal temperature and pressure environment, the butterfly gasket 2 and the flat gasket 3 made of Inconel 718 alloy are selected and placed in front of the lens. Inconel Alloy 718 has good corrosion resistance and high temperature elasticity.

The lens barrel 6 is a variable cross-section member, the front part is the thinnest, the upper part is threaded, the middle part is the thickest, and the middle part is processed into an external hexagon to facilitate tightening, and the tail part is processed into a smooth cylindrical surface for placing the pressure ring 9 and graphite Washer 8; the diameter of the inner surface of the lens barrel gradually decreases from the tail (the diameter of the tail of this embodiment is 33.66mm) to the front until a suitable size (the diameter of the front of this embodiment is 15mm), in the shape of a bell mouth. The structure can effectively increase the amount of light transmission; there is a small groove on the front surface of the lens barrel for placing the O-ring 5 .

The gland 10 is a member with a variable cross-section. Its front part is a smooth cylindrical surface, and its end face is in direct contact with the pressure ring 9. The middle part has threads to cooperate with the mirror holder 7. The tail part has the largest cross-sectional diameter, and four sockets 12 are opened on the side for easy fitting The upper force rod is tightened, and the end face has four threaded holes 11 so as to fix the probe; The bell mouth in the tube 6 is adapted to increase the amount of light transmission.

The utility model can realize the application of the mirror structure for in-situ optical observation under high temperature and high pressure liquid environment, including the following steps:

1. Place the lens barrel vertically on a plane, and place the O-ring 5 in the slot on the front end of the lens barrel 6;

2. Put the lens 4 flat on the O-ring 5 and keep the two evenly aligned;

3. Put the flat washer 3 and the butterfly washer 2 on the lens 4 in sequence;

4. Slowly screw the pressure cap 1 into the front of the lens barrel 6 by hand, be careful not to touch the placed lens 4 and O-ring 5 when screwing in, until the inner end surface of the pressure cap 1 is in contact with the lens 4 until the mirror surface of the mirror touches and feels that the hand cannot be twisted;

5. Turn the lens barrel 6 assembled at the front up and down, put a certain number (7 to 9 pieces) of graphite gaskets 8 on the smooth cylindrical surface at the end of the lens barrel, and then set the pressure ring 9 on the outermost layer;

6. Place the assembled lens barrel assembly horizontally, and slowly extend into the autoclave 13 through the lens base 7 until the middle end surface of the lens barrel 6 contacts the inner end surface of the lens base 7;

7. Slowly screw the gland 10 into the mirror holder 7 by hand, so that the gland 10 is in contact with the pressure ring 9 and pressed tightly. Tighten with internal force, the torque used is about 5N m, do not tighten too tightly;

8. After the mirror structure is installed, the sample can be installed in the autoclave, the lid of the autoclave is sealed, the reaction medium is introduced, pressurized and heated, and after reaching the parameters required for the experiment, the long-focus microscope or Raman spectrometer can be used to see through it. The sight glass observes in situ the change of the surface state of the sample in the autoclave or detects the composition change of the product on the surface of the sample.

Example

In the embodiment, pure water is introduced into the autoclave 13, the pressure is increased to 12.7MPa by a high-pressure pump, the temperature is raised to 285°C and kept for 44 hours, and no problems are found during the whole experiment, indicating that the structure of the mirror is Can work safely and stably under this condition.

Claims (7)

1, a kind of visor that can realize original position optical observation under the high temperature high pressure liquid environment, it is characterized in that, this visor structure comprises pressure cap (1), butterfly gasket (2), plain washer (3), eyeglass (4), O type circle (5), lens barrel (6), microscope base (7), graphite gasket (8), pressure ring (9) and gland (10), annexation between the each several part is as follows: O type circle (5) is placed in the fluting of lens barrel (6) end face, eyeglass (4) lies on the O type circle (5), plain washer (3) and butterfly gasket (2) lie on the eyeglass (4) successively, pressure cap (1) is anterior by being threaded with lens barrel (6), make butterfly gasket (2), plain washer (3), eyeglass (4), O type circle (5) and lens barrel (6) end face are adjacent to mutually, graphite gasket (8) and pressure ring (9) are enclosed within on the face of cylinder of lens barrel (6) afterbody, form barrel assembly; Microscope base (7) is welded on the autoclave (13), and it is the basis that whole lens barrel structure is installed; Barrel assembly one end that assembles extend in the autoclave (13) by microscope base (7), and its other end abuts against with microscope base (7) inner face; Gland (10) is screwed on the microscope base (7) by screw thread, compresses pressure ring (9) and graphite gasket (8).

According to the described visor of claim 1, it is characterized in that 2, eyeglass (4) is selected the elevated temperature strength height for use, corrosion stability is good and single crystal sapphire sheet excellent in optical properties grinds and forms.

According to the described visor of claim 1, it is characterized in that 3, select butterfly gasket (2) and plain washer (3) for use, two kinds of packing ring materials are Inconel 718 alloys, have corrosion stability and high temperature elasticity preferably.

4, according to the described visor of claim 1, it is characterized in that, select Kalrez O type circle (5) for use, this O type circle material is a high-temperature fluorination rubber, and maximum operation (service) temperature reaches 327 ℃.

According to the described visor of claim 1, it is characterized in that 5, select graphite gasket (8) for use, this packing ring material is a soft graphite.

According to the described visor of claim 1, it is characterized in that 6, lens barrel (6) is a non-uniform member, the front portion is the thinnest, above car screw thread is arranged, the middle part is the thickest, the centre is processed to outer-hexagonal, the face of cylinder that afterbody is processed into is to place pressure ring (9) and graphite gasket (8); Lens barrel (6) inner surface diameter reduces to the front portion gradually from afterbody, is a bell mouth shape, has groove on the lens barrel front end face and is used for placing O type circle (5).

7, according to the described visor of claim 1, it is characterized in that, gland (10) is a non-uniform member, its front portion is the face of cylinder, end face directly contacts with pressure ring (9), and the middle part car has screw thread to cooperate afterbody diameter of section maximum with microscope base (7), the side has jack (12), and end face has threaded hole (11); Gland (10) inside surface is the hole that has tapering, and the hydraucone in its tapering and the lens barrel (6) adapts.

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