CN102019241B - Combined nozzle for preparing supercritical fluid nano-micron materials - Google Patents

Abstract

The invention relates to a device for preparing nano-micron materials or superfine powder, in particular to a combined nozzle for preparing supercritical fluid nano-micron materials, comprising the basic members of an end cover, an inner mixing disc, an outer mixing disc, a nozzle disc, a crystallizer (or called as a collector), a regulating nut, a fastening nut, a whirl stopping pin, a stop screw and a seal ring. According to the requirements of the preparation process of the supercritical fluid nano-micron materials or the superfine powder, the basic members with the uniform installing dimensions are selected to assemble a multi-channel inner mixing type nozzle, a multi-channel outer mixing type nozzle, a multi-channel inner and outer mixing type nozzle and a rapid expansion nozzle. Compared with the traditional combined nozzle for preparing the supercritical fluid nano-micron materials, the invention simplifies structure, shortens volume, saves raw materials, optimizes machining process properties, reduces cumulated errors of the members and processing and manufacturing cost and increases installation accuracy. When used, the combined nozzle for preparing the supercritical fluid nano-micron materials simplifies regulating processes and operating process and greatly increases production quality and work efficiency.

Description

Combination nozzle for preparation of supercritical fluid nano-micron materials

1. Technical field

The invention relates to equipment for preparing nano-micron materials and ultrafine powders, in particular to a combined nozzle for preparing supercritical fluid nano-micron materials.

2. Background technology

Authorized by the China Intellectual Property Office on March 17, 2010, the authorized announcement number is CN 100594070C (patent number is ZL200610045286.0), and the patent named "combined nozzle for supercritical fluid nano-micron material preparation" better solves the problem of At present, the common problems in the supercritical fluid nano-micron material or ultrafine powder preparation nozzle are that the micropore is difficult to process, the aperture cannot be adjusted, the nozzle is easy to block, and the production efficiency is low.

The nozzle disclosed in this patent is an axial combined adjustable annular gap nozzle, which consists of an end cover, a moving ring, an inner mixing and static ring, an outer mixing and static ring, a crystallizer (also known as a collector), an adjusting nut, a distance sleeve, Sealing rings, connectors, etc., according to the requirements of the supercritical fluid nano-micron material or ultrafine powder preparation process, select the aforementioned basic components with uniform installation dimensions to assemble multi-channel internal mixing nozzles, multi-channel external mixing nozzles, multi-channel Mixed internal and external nozzles, and rapid expansion nozzles. Analyzing this patent, although it has many advantages in structure and application compared with the prior art, there are complex structures in manufacturing and application, poor processing technology, complex assembly process, large accumulation error, and poor positioning when the components cooperate. , to adjust the shortcomings of long operating procedures and inconvenient, which not only increases the processing difficulty and processing cost of the patented product, but also seriously affects the uniformity of the distribution of the annular gap, reducing the atomization quality of the nozzle and nano-micron materials or ultra-micro The quality of powder preparation.

3. Contents of the invention

The purpose of the present invention is to overcome the shortcomings of the above invention, simplify the components, reduce the cost of processing and manufacturing, and provide a nozzle with simple structure, small volume, good processing technology, simple assembly and assembly process, high overall installation accuracy, and convenient application and operation. The inner fluid flow effect is good, and the axial combined adjustable ring gap supercritical fluid nano-micron material or ultrafine powder with excellent atomization quality is sprayed with a combined nozzle.

The basic concept of the present invention is: it is composed of end cover, inner mixing plate, outer mixing plate, spout plate, crystallizer also known as collector, adjusting nut, fastening nut, anti-rotation pin, limit screw, sealing ring basic components.

The end cover is a combination of a disc-shaped cylinder and a thin cylindrical nozzle core coaxially connected. There is a fluid center channel at the axial center of the combination. The orifice of the fluid center channel on the end face of the disc-shaped cylinder is a fluid inlet; The thread is processed on the cylindrical surface of the disc-shaped cylinder, and the anti-rotation pin hole is processed on the end surface of the disc-shaped cylinder coaxially connected with the nozzle core and matched with the anti-rotation pin hole on the matching part. The outer edge of the end surface is along the ring A half-groove is processed toward the limit; a sealing groove is processed on the cylindrical surface of the nozzle core, and a nozzle core cone composed of a small cylinder and a cone is formed at the end of the nozzle core, and the fluid nozzle hole is processed in the center of the nozzle core cone to communicate with the fluid center channel.

The inner mixing disc is a combination of a disc-shaped cylinder and a thin cylindrical nozzle core coaxially connected. The inner hole and the fluid center channel are processed at the axial center of the combination. The bottom of the inner hole is tapered; The middle part of the cylindrical surface is processed with undercut grooves, the upper and lower positions of the undercut grooves are respectively processed with left and right-handed threads, and the fluid side channels are processed along the radial direction to communicate with the bottom of the inner hole, and the fluid side channel openings are fluid inlets; disc shape There are anti-rotation pin holes on both ends of the cylinder, which are matched with the anti-rotation pin holes of the matching parts; the outer edges of the two ends of the disc-shaped cylinder are respectively machined with half grooves along the ring direction; the cylindrical surface of the nozzle core is processed to seal There is a nozzle core cone composed of a small cylinder and a cone at the end of the nozzle core, and the fluid side nozzle hole is processed on the small cylinder of the nozzle core cone to communicate with the fluid central channel.

The outer mixing disc is a combination of a disc-shaped cylinder and a thin cylindrical nozzle core coaxially connected. The inner hole and the fluid center channel are processed at the axial center of the combination. The bottom of the inner hole is tapered; The middle part of the cylindrical surface is processed with undercut grooves, the upper and lower positions of the undercut grooves are respectively processed with left and right-handed threads, and the fluid side channels are processed along the radial direction to communicate with the bottom of the inner hole, and the fluid side channel openings are fluid inlets; disc shape There are anti-rotation pin holes on both ends of the cylinder, which are matched with the anti-rotation pin holes of the matching parts; the outer edges of the two ends of the disc-shaped cylinder are respectively machined with half grooves along the ring direction; the cylindrical surface of the nozzle core is processed to seal There is a nozzle core cone composed of a small cylinder and a cone at the end of the nozzle core, and a fluid nozzle hole is processed in the center of the nozzle core cone to communicate with the fluid center channel.

The nozzle disc is a combination of the upper and lower end faces of the disc-shaped cylinder, which are connected coaxially with the connecting end cover, the inner mixing disc and the outer mixing disc joint, and the crystallizer joint connecting the crystallizer, respectively. The inner hole and the conical fluid injection hole are processed coaxially at the central part of the shaft, and the bottom of the inner hole is conical; the cylinder at one end of the inner hole is the disc cover joint, and the connecting thread is processed on the disc cover joint. The diameter and direction of rotation match the diameter and direction of rotation of the threads on the connection and installation parts of the matching end cap, inner mixing disc, and outer mixing disc; The lateral channel of the processing fluid communicates with the bottom of the inner hole, and there are anti-rotation pin holes on the end surface, which match correspondingly with the anti-rotation pin holes on the matching parts; The seal groove is processed on the joint, and its diameter matches the inner cavity diameter of the crystallizer installation part; the thread is processed on the surface of the disc-shaped cylinder, and its diameter and direction of rotation match the connection part of the crystallizer. The connection part corresponds to the anti-rotation pin hole.

The crystallizer is a pressure-bearing cylinder. The anti-rotation pin hole is processed on the end face connected with the nozzle plate, and the thread is processed on the cylindrical surface connected with the nozzle plate.

The diameter and depth of the inner hole on the end cover, the inner mixing plate, the outer mixing plate, and the nozzle plate, and the taper at the bottom, and the outer diameter, length, and taper of the nozzle core of the end cover, the inner mixing plate, and the outer mixing plate Matching and interchangeable, the matching relationship between the outer diameter of the nozzle core and the inner hole of each matching part is a tight fit.

The internal thread of the adjusting nut is two sections of thread in opposite directions, separated by a relief groove in the middle, and matched with the threads of the end cover, the inner mixing plate, the outer mixing plate, and the nozzle plate respectively. There are screw holes on the nut wall and Install the set screw.

The internal thread of the fastening nut is two sections of threads in opposite directions, separated by a relief groove in the middle, and matched with the threads of the spout plate and the crystallizer interface respectively. There are screw holes on the nut wall and limit screws are installed.

End caps, inner mixing discs, outer mixing discs, spout discs, and the outer edge of each end face of the crystallizer are processed along the circumferential limit half groove, which is an unclosed half groove less than 360 degrees in the circumferential direction, and the two corresponding connecting fittings The half grooves are matched with each other to form a complete limit groove. The limit screw guide column on the wall of the adjusting nut or the fastening nut is inserted into the limit groove to prevent excessive adjustment of the adjusting nut or loosening of the fastening nut, which may cause damage to the fittings. separate.

The anti-rotation pins installed in the anti-rotation pin holes corresponding to the end faces of each fitting are sliding fits, and the effect of this structure is to prevent the connecting parts from rotating when the adjusting nut or fastening nut is rotated.

The end cover, the inner mixing plate, the outer mixing plate, the fluid center channel or the hole wall of the fluid side channel on the nozzle plate, and the fluid side nozzle hole of the inner mixing plate, the fluid center nozzle hole of the outer mixing plate, the nozzle plate The hole wall of the conical fluid nozzle is smooth or with helix; since the hole wall with helix helps to increase the turbulence of the fluid and optimize the atomization quality, it is better to have a helix on the hole wall.

The axis of the fluid lateral channel on the inner mixing plate, the outer mixing plate, and the nozzle plate intersects or does not intersect with the axis of the component, and the axis of the fluid lateral orifice of the inner mixing plate intersects or does not intersect with the axis of the component, and the intersecting or non-intersecting two The axes are perpendicular or non-perpendicular to each other. The axis of the fluid lateral channel on the inner mixing plate, the outer mixing plate, and the nozzle plate and the axis of the component, and the fluid lateral orifice axis of the inner mixing plate and the axis of the component are non-intersecting vertical or non-perpendicular structures, and the fluid formed The tangential entry or ejection of the fluid helps to increase the turbulence of the fluid, which is conducive to optimizing the atomization quality; therefore, the axis of the fluid side channel on the inner mixing plate, the outer mixing plate, and the nozzle plate is related to the axis of the component, and the inner mixing plate. The fluid lateral orifice axis of the disk is preferably in a non-intersecting configuration with the axis of the member.

According to the requirements of the preparation process of supercritical fluid nano-micron materials or ultrafine powder, select the basic components with uniform installation dimensions above to assemble multi-channel internal mixing nozzles, multi-channel external mixing nozzles, multi-channel internal and external mixing nozzles and rapid expansion nozzles .

The multi-channel internal mixing nozzle is composed of an end cover, at least one internal mixing plate, nozzle plate, and crystallizer. After installing the sealing ring in the nozzle core sealing groove of the end cover, it is installed into the inner hole of the internal mixing plate, and the internal mixing plate Install the sealing ring in the sealing groove of the nozzle core and then install it into the inner hole of the secondary inner mixing plate or the inner hole of the spout plate, install the sealing ring in the sealing groove on the crystallizer joint of the spout plate and then install it into the inner cavity of the crystallizer, Install the anti-rotation pins in the anti-rotation pin holes corresponding to the end faces between the fittings; use the adjusting nut to connect the end cover with the inner mixing plate, the inner mixing plate and the nozzle plate, and screw in the limit screw on the adjusting nut to make The guide column is inserted into the limit groove formed by the two fittings; the spout plate and the crystallizer are connected together with a fastening nut, and the limit screw on the fastening nut is screwed in so that the guide post is inserted into the limit groove composed of the two fittings. limit groove.

The multi-channel external mixing nozzle is composed of an end cover, at least one external mixing plate, nozzle plate, and crystallizer. After installing the sealing ring in the nozzle core sealing groove of the end cover, it is installed into the inner hole of the external mixing plate. After installing the sealing ring in the sealing groove of the nozzle core, install it into the inner hole of the secondary outer mixing plate or the inner hole of the nozzle plate, install the sealing ring in the sealing groove on the crystallizer joint of the nozzle plate, and then install it into the inner cavity of the mold. Install the anti-rotation pins in the anti-rotation pin holes corresponding to the end faces between the fittings; use the adjusting nut to connect the end cover with the outer mixing plate, the outer mixing plate and the nozzle plate, and screw in the limit screw on the adjusting nut to make it The guide column is inserted into the limit groove formed by the two fittings; the spout plate and the crystallizer are connected together with a fastening nut, and the limit screw on the fastening nut is screwed in so that the guide post is inserted into the limit groove formed by the two fittings. bit groove.

The multi-channel internal and external mixing nozzle is composed of an end cover, at least one inner mixing plate, at least one outer mixing plate, nozzle plate, and crystallizer; install the sealing ring in the sealing groove of the nozzle core of the end cover and then install it into the inner mixing plate Install the sealing ring in the nozzle core sealing groove of the inner mixing plate and then install it into the inner hole of the outer mixing plate, install the sealing ring in the nozzle core sealing groove of the outer mixing plate and install it into the inner hole of the nozzle plate, Install the sealing ring in the sealing groove on the crystallizer joint of the disc and install it into the inner cavity of the crystallizer, and install the anti-rotation pin in the corresponding anti-rotation pin hole on the end face between the fittings; use the adjusting nut to connect the end cover and the inner mixing disc. , The inner mixing plate and the outer mixing plate, the outer mixing plate and the spout plate are connected together, and the limit screw on the adjusting nut is screwed in so that the guide column is inserted into the limit groove formed by the two matching parts; the spout is fixed with the fastening nut The disk and the crystallizer are connected together, and the limit screw on the fastening nut is screwed in so that the guide column is inserted into the limit groove formed by the two matching parts.

The rapid expansion nozzle is composed of an end cover, a spout plate, and a crystallizer; install a sealing ring in the sealing groove of the nozzle core of the end cover and then install it into the inner hole of the spout plate, and install a sealing ring in the sealing groove on the crystallizer joint of the spout plate Finally, install it into the inner cavity of the crystallizer; install the anti-rotation pin in the corresponding anti-rotation pin hole on the end face between the fittings; use the adjustment nut to connect the end cover and the nozzle plate together, and screw in the limit screw on the adjustment nut The guide column is inserted into the limit groove formed by the two fittings; the spout plate and the crystallizer are connected together with a fastening nut, and the limit screw on the fastening nut is screwed in so that the guide post is inserted into the limit groove composed of the two fittings. limit groove. The connection between the spout plate and the crystallizer can also adopt other forms such as flange type, clamp type, toothed type, threaded ferrule or threaded pressure sleeve.

After installation, the nozzle core cone on the end cover, inner mixing disc, and outer mixing disc nozzle core of the combined nozzle is in linear contact with the matching inner hole conical bottom. Turning the adjusting nut can precisely adjust the nozzle core cone and the inner hole conical bottom. The annulus formed can meet the requirement of nozzle annulus for the preparation of nano-micron materials or ultrafine powders, realize simple injection of one material, internal mixing, external mixing, internal and external mixing and rapid expansion of two or more materials A variety of composite jets.

Compared with the existing combined nozzle for supercritical fluid nano-micron material preparation, the present invention simplifies the structure, reduces the volume, and saves raw materials; optimizes the processing performance, reduces the cumulative error of components, improves the installation accuracy and reduces the cost. Processing and manufacturing costs; when applied, it simplifies the adjustment procedure and operation process, and greatly improves the production quality and work efficiency.

4. Description of drawings

Figure 1 is a schematic diagram of the structure of a four-channel internal and external mixed nozzle;

Fig. 2 is a schematic diagram of the structure of the end cap;

Figure 3 is a schematic diagram of the structure of the internal mixing disk;

Figure 4 is a schematic diagram of the structure of the external mixing disk;

Fig. 5 is a schematic diagram of the nozzle plate structure;

Fig. 6 is a schematic diagram of the structure of the adjusting nut;

Fig. 7 is a structural schematic diagram of a fastening nut;

Fig. 8 is a schematic diagram of crystallizer interface structure;

Fig. 9 is a structural schematic diagram of a three-channel internal mixing combined nozzle;

Fig. 10 is a structural schematic diagram of a three-channel external mixing type combined nozzle;

Fig. 11 is a structural schematic diagram of a two-channel rapid expansion nozzle;

Fig. 12 is a schematic diagram of the geometric relationship between the nozzle core cone and the nozzle opening in Fig. 1I;

Fig. 13 is a schematic diagram of the hole wall structure of the fluid side channel partially enlarged at the part II of Fig. 3;

Fig. 14 is a partially enlarged schematic view of the structure of the central channel of the fluid in the part III of Fig. 3;

Fig. 15 is a partially enlarged schematic view of the wall structure of the fluid side nozzle hole in the IV portion of Fig. 3;

Fig. 16 is a schematic diagram of the wall structure of the tapered nozzle hole in the center of the fluid partially enlarged at the part V of Fig. 5;

Fig. 17 is a partially enlarged schematic diagram of the structure of a non-intersecting fluid lateral channel at the II portion of Fig. 3;

Fig. 18 is a partially enlarged schematic view of the wall structure of the lateral injection hole of the non-intersecting fluid in the IV portion of Fig. 3 .

Reference signs:

1 end cover, 1-1 fluid inlet, 1-2 fluid center channel, 1-3 right-hand thread, 1-4 anti-rotation pin hole, 1-5 sealing groove, 1-6 nozzle core, 1-7 nozzle core cone , 1-8 fluid center nozzle, 1-9 limit half groove; 2 inner mixing plate, 2-1 fluid inlet, 2-2 fluid side channel, 2-2-1 helix, 2-3 limit half Groove, 2-4 inner hole, 2-5 nozzle opening, 2-6 anti-rotation pin hole, 2-7 left-handed thread, 2-8 relief groove, 2-9 right-handed thread, 2-10 anti-rotation pin hole, 2-11 fluid center flow channel, 2-11-1 helix, 2-12 sealing groove, 2-13 nozzle core, 2-14 nozzle core cone, 2-15 fluid side nozzle hole, 2-16 limit half Groove; 3 outer mixing disc, 3-1 fluid inlet, 3-2 fluid side channel, 3-3 limit half groove, 3-4 inner hole, 3-5 nozzle opening, 3-6 anti-rotation pin hole, 3 -7 left-handed thread, 3-8 relief groove, 3-9 right-handed thread, 3-10 anti-rotation pin hole, 3-11 fluid center channel, 3-12 sealing groove, 3-13 nozzle core, 3-14 nozzle Core cone, 3-15 fluid center nozzle hole, 3-16 limit half groove; 4 nozzle plate, 4-1 fluid inlet, 4-2 fluid side channel, 4-3 limit half groove, 4-4 inner hole , 4-5 nozzle mouth, 4-6 anti-rotation pin hole, 4-7 left-handed thread, 4-8 relief groove, 4-9 right-handed thread, 4-10 anti-rotation pin hole, 4-11 sealing groove, 4 -12 conical fluid nozzle, 4-12-1 helix, 4-13 crystallizer joint, 4-14 limit half groove; 5 adjusting nut, 5-1 left-handed thread, 5-2 limit screw hole, 5 -3 right-hand thread, 5-4 undercut, 5-5 knurling; 6 fastening nut, 6-1 right-hand thread, 6-2 limit screw hole, 6-3 left-hand thread, 6-4 retract Groove, 6-5 knurling; 7 crystallizer, 7-1 limit half groove, 7-2 inner cavity, 7-3 anti-rotation pin hole, 7-4 left-handed thread, 7-5 retreat groove; 8 anti-rotation Pin; 9 small sealing ring; 10 large sealing ring; 11 limit screw; 12 fluid connection.

5. Specific implementation

Describe the embodiment of the present invention in detail in conjunction with accompanying drawing:

1. Embodiment 1: Select basic components to assemble a set of four-channel internal and external mixing nozzles.

As shown in Figure 1, the four-channel inner and outer mixing nozzle is composed of an end cover 1, an inner mixing plate 2, an outer mixing plate 3, a nozzle plate 4, three adjusting nuts 5, a fastening nut 6, and a mold 7. Four anti-rotation pins 8, three small sealing rings 9, one large sealing ring 10, and four limit screws 11; the limit screw consists of a screw rod with a screwdriver and a cylinder whose tail diameter is smaller than the screw rod Composition, the cylinder is the guide column.

The installation process is:

Screw in the limit screw 11 in the limit screw holes 5-2 and 6-2 on the adjustment nut 5 and the fastening nut 6, and then screw the limit screw 11 into the sealing groove 1-5 and the inner seal groove 1-5 on the nozzle core 1-6 of the end cover 1. The sealing groove 2-12 on the nozzle core 2-13 of the mixing disc 2 and the sealing groove 3-12 of the nozzle core 3-13 of the outer mixing disc 3 are set with a small sealing ring 9; The sealing groove 4-11 on the 13 is equipped with a large sealing ring 10 for subsequent use.

Align the right-handed thread 5-1 of the first adjusting nut 5 with the right-handed thread 1-3 on the end cover 1, insert one end of the anti-rotation pin 8 into the anti-rotation pin hole 2-6 of the inner mixing disc 2, Install the nozzle core 1-6 of the end cover 1 into the inner hole 2-4 of the inner mixing plate 2, insert the other end of the anti-rotation pin 8 into the anti-rotation pin hole 1-4 of the end cover 1, and adjust the left-hand rotation of the nut 5 The thread 5-3 is aligned with the left-handed thread 2-7 of the inner mixing disc 2, and the adjusting nut 5 is turned to connect the end cover 1 and the inner mixing disc 2 at the same time. At this time, the nozzle cores of the nozzle cores 1-6 on the end cover 1 The cone 1-7 is in linear contact with the nozzle opening 2-5 at the conical bottom of the inner hole 2-4 of the inner mixing disc 2 without an annular gap. The limit half-groove 1-9 on the outer edge of the end face of the end cover 1 and the limit half-groove 2-3 on the end face outer edge of the inner mixing disc 2 form a limit groove, and the limit screw 11 on the adjustment nut 5 Correspondingly, the limit screw 11 is rotated, and the guide column of the limit screw 11 is inserted into the limit groove.

Then, align the right-handed thread 5-1 of the second adjusting nut 5 with the right-handed thread 2-9 on the inner mixing disc 2, insert one end of the anti-rotation pin 8 into the anti-rotation pin hole 3- of the outer mixing disc 3 6, install the nozzle core 2-13 of the inner mixing disc 2 into the inner hole 3-4 of the outer mixing disc 3, insert the other end of the anti-rotation pin 8 into the anti-rotation pin hole 2-10 of the inner mixing disc 2, The left-handed thread 5-3 of the adjusting nut 5 is aligned with the left-handed thread 3-7 of the outer mixing disc 3, and the adjusting nut 5 is turned to connect the inner mixing disc 2 and the outer mixing disc 3 together, at this time the nozzle core of the inner mixing disc 2 The nozzle core cone 2-14 on the 2-13 is in linear contact with the nozzle opening 3-5 at the conical bottom of the inner hole 3-4 of the outer mixing disc 3 without an annulus. The limit half-groove 2-16 on the outer edge of the end face of the inner mixing disc 2 and the limit half-groove 3-3 on the outer edge of the end face of the outer mixing disc 3 form a limit groove, and the limit screw on the adjusting nut 5 Corresponding to 11, turn the limit screw 11, and the guide column of the limit screw 11 is inserted into the limit groove.

Then align the right-handed thread 5-1 of the third adjusting nut 5 with the right-handed thread 3-9 on the outer mixing disc 3, insert one end of the anti-rotation pin 8 into the anti-rotation pin hole 4-6 of the spout disc 4 , install the nozzle core 3-13 of the outer mixing disc 3 into the inner hole 4-4 of the nozzle disc 4, insert the other end of the anti-rotation pin 8 into the anti-rotation pin hole 3-10 of the outer mixing disc 3, adjust the nut 5 The left-handed thread 5-3 is aligned with the left-handed thread 4-7 of the spout disc 4, and the adjusting nut 5 is turned to connect the outer mixing disc 3 and the spout disc 4 at the same time. At this time, the nozzle on the nozzle core 3-13 of the outer mixing disc 3 The core cone 3-14 is in linear contact with the nozzle opening 4-5 at the conical bottom of the inner hole 4-4 of the nozzle disk 4 without an annular gap. The limit half-groove 3-16 on the outer edge of the outer mixing disc 3 end face and the limit half-groove 4-3 on the end face outer edge of the spout plate 4 form a limit groove, and the limit screw 11 on the adjustment nut 5 Correspondingly, the limit screw 11 is rotated, and the guide column of the limit screw 11 is inserted into the limit groove.

When connecting the end cap 1 and the inner mixing disc 2 or the inner mixing disc 2 and the outer mixing disc 3 or the outer mixing disc 3 and the spout disc 4 with the adjusting nut 5, the number of threads screwed into the two connected parts is equal.

Finally, align the right-handed thread 6-1 of the fastening nut 6 with the right-handed thread 4-9 on the disc-shaped cylinder of the nozzle plate 4, and insert one end of the anti-rotation pin 8 into the anti-rotation pin hole 7- of the crystallizer 7 3, insert the crystallizer connector 4-13 of the spout plate 4 into the inner cavity 7-2 of the crystallizer 7, insert the other end of the anti-rotation pin 8 into the anti-rotation pin hole 4-10 of the spout plate 4, and tighten the nut The left-handed thread 6-3 of 6 is aligned with the left-handed thread 7-4 of the crystallizer 7, and the fastening nut 6 is turned to connect the spout plate 4 and the crystallizer 7 together; when the fastening nut 6 connects the spout plate 4 and the crystallizer 7 , the number of screw threads screwed into the two connected parts is equal. The limiting half-groove 4-14 on the outer edge of the end face of the nozzle plate 4 and the limiting half-groove 7-1 on the outer edge of the crystallizer 7 form a limiting groove, corresponding to the limiting screw 11 on the fastening nut 6 , turn the limit screw 11, and the guide column of the limit screw 11 is inserted into the limit slot.

The limit half grooves 1-9, 2-3, 2-16, 3-3, 3-16, 4-3, 4-14, 7-1 processed along the circumferential direction on the outer edge of each end face are less than 360 in the circumferential direction. degrees, such as 355 degrees or 350 degrees and other unclosed half grooves. A set of four-channel internal and external mixed nozzles is installed, and the fluid connection pipe 12 is connected to the fluid inlets 1-1, 2-1, 3-1, 4-1 by welding. The anti-rotation pin 8 ensures that when the adjusting nut 5 and the fastening nut 6 are rotated, the end cover 1 and the inner mixing disc 2, the inner mixing disc 2 and the outer mixing disc 3, the outer mixing disc 3 and the spout disc 4, the spout disc 4 and the crystal There is no rotation between the devices 7.

The installed four-channel internal and external mixing nozzle consists of the nozzle core cone 1-7 of the end cover 1 and the nozzle opening 2-5 of the inner mixing disc 2, the nozzle core cone 2-14 of the inner mixing disc 2 and the nozzle of the outer mixing disc 3 The mouth 3-5, the nozzle core cone 3-14 of the outer mixing plate 3 and the nozzle opening 4-5 of the nozzle plate 4 constitute three nozzle ring gaps, and the three nozzle ring gaps can be adjusted by turning the three adjusting nuts 5 respectively. The size of the gap.

In order to facilitate the adjustment of the ring gap, the nozzle core cone 1-7 and the nozzle port 2-5 or the nozzle core cone 2-14 and the nozzle port 3-5 or the nozzle core cone 3-14 and the nozzle port 4-5 are respectively connected in the adjusting nut 5. After adjusting to linear contact without annular gap, simultaneously describe the joint positions of the first adjusting nut 5 and the end cover 1, the second adjusting nut 5 and the inner mixing plate 2, and the third adjusting nut 5 and the outer mixing plate 3 "0" reference line, and then according to the pitch of the adjusting nut 5 and the taper of each nozzle core cone, it is calculated that after the adjusting nut 5 is loosened in the opposite direction, each nozzle core cone and nozzle opening will have a difference such as 5 μm, 10 μm, ..., 50 μm For the ring gap, the rotation angle of the unit ring gap is adjusted according to the adjusting nut 5 as the unit scale value, and the scale line is drawn on the adjusting nut 5 starting from the "0" reference line and moving toward the loosening direction as the measurement basis for adjusting the size of the ring gap.

As shown in Figure 12, the relationship between the annular gap formed between the nozzle core cone and the nozzle opening, the pitch of the adjusting nut and the angle turned toward the loosening direction of the adjusting nut is shown in the following formula:

$\mathrm{<span\; class="notranslate">\; \&delta;</span>}<span\; class="notranslate">\; =</span>\frac{\mathrm{<span\; class="notranslate">\; 2</span>}\mathrm{<span\; class="notranslate">\; \&beta;<figure-callout\; id="360"\; label="t"\; filenames="HSA00000314784000051.png"\; state="\{\{state\}\}">t</figure-callout></span>}}{\mathrm{<span\; class="notranslate">\; 360</span>}}<span\; class="notranslate">\; \&times;</span>\mathrm{<span\; class="notranslate">\; sin</span>}\mathrm{<span\; class="notranslate">\; \&alpha;</span>}$

In the formula: δ is the annular gap formed between the nozzle core cone and the nozzle mouth; α is the cone angle of the nozzle core cone; t is the pitch of the adjusting nut; β is the angle turned toward the loosening direction of the adjusting nut.

The process of preparing nano-micron materials or ultra-fine powders with supercritical fluids using four-channel internal and external mixing nozzles: Take the preparation of single-material nano-micron materials or ultra-fine powders with coatings as an example. The carbon dioxide gas is produced through the usual supercritical carbon dioxide production method, that is, the carbon dioxide is refrigerated and liquefied first, pressurized by a booster pump to reach a critical pressure, and then enters a heater to raise the carbon dioxide temperature above the critical temperature to form supercritical carbon dioxide. Dissolve the material to be prepared into a solvent that is miscible with supercritical carbon dioxide, and then drive it into the fluid inlet 2-1 and the fluid side channel 2-2 of the inner mixing plate 2 through the fluid connection pipe 12 through the booster pump, from the end cover 1 The annular gap formed between the nozzle core cone 1-7 and the nozzle opening 2-5 of the inner mixing plate 2 is ejected, and the formed mist fluid is sprayed from the fluid side to the nozzle hole 2-15 through the fluid center flow channel 2-11 Enter the mixing chamber formed between the inner mixing plate 2 and the outer mixing plate 3, that is, the space formed by the nozzle core 2-13 and the inner hole 3-4; 3. The fluid inlet 3-1 and the fluid side channel 3-2 enter the space formed by the nozzle core 2-13 and the inner hole 3-4, and the sprayed material to be prepared is sprayed from the fluid side to the nozzle hole 2-15. Solution mixing; after mixing, continue to quickly spray into the crystallizer volume space from the annular gap formed between the nozzle core cone 2-14 of the inner mixing plate 2 and the nozzle opening 3-5 of the outer mixing plate 3, and enter the nozzle plate from the fluid connection 12 The fluid inlet 4-1 of 4 passes through the supercritical carbon dioxide of the fluid side channel 4-2, and the annular gap formed between the nozzle core cone 3-14 of the outer mixing disc 3 and the nozzle opening 4-5 of the nozzle disc 4 is sprayed rapidly to Crystallizer volume space; two mist fluids meet on the way to the crystallizer volume space, supercritical carbon dioxide takes away the solvent, that is, the two are mixed outside the nozzle, and the material to be prepared crystallizes to form a coated nano-micron material or super Micropowder. The fluid inlet 1-1 is used as an auxiliary channel to feed supercritical carbon dioxide or porous material suspension according to the process requirements, so as to enhance the atomization and crystallization of the material fluid to be prepared or achieve the effect of infiltrating into the porous material.

In order to increase the degree of turbulence when the material solution to be prepared, supercritical carbon dioxide and coating solution pass through the fluid side channels 2-2, 3-2, 4-2 and the fluid central channel 1-2, and facilitate these fluids to pass through the nozzle annulus When mixing or atomizing, the fluid side channels 2-2, 3-2, 4-2 preferably adopt the structure of the hole wall with a helix 2-2-1 shown in Figure 13, and the fluid center channel 1-2 preferably adopts the The hole wall shown in Figure 15 has a helical line 2-11-1 structure; in order to strengthen the degree of turbulence of the fluid after atomization and facilitate the further mixing or crystallization of the fluid, the hole walls of the fluid center channel 2-11 and 3-11 are the best The helical structure shown in 2-11-1 is adopted, and the fluid side spray hole 2-15 preferably adopts the structure of the hole wall with a helical line 2-15-1 shown in Figure 16, and the tapered fluid spray hole 4-12 is the best It is better to adopt the 4-12-1 hole wall band helical structure shown in Figure 18.

In order to make the material solution to be prepared, supercritical carbon dioxide and coating solution rotate after passing through the fluid side channels 2-2, 3-2, 4-2, and facilitate the mixing or atomization of these fluids when they pass through the nozzle annular gap, the best Preferably adopt the vertical or non-perpendicular structure that the axis of fluid lateral channel 2-2,3-2,4-2 shown in Figure 14 and the axis of inner hole 2-4,3-4,4-4 do not intersect; The atomized fluid is further rotated to improve the mixing degree of the mixed fluid. It is preferable to adopt the vertical or non-intersecting axis of the fluid side spray hole 2-15 shown in FIG. 17 and the axis of the nozzle core cone 2-14. vertical structure.

The fluid side channels 2-2, 3-2, 4-2 and the fluid side spray holes 2-15 preferably adopt the hole wall band helical structure and the axis non-intersecting vertical or non-vertical structure to further enhance the spraying or spraying. The degree of turbulence or rotation of the mixed fluid is conducive to the atomization, mixing and crystallization of the fluid.

2. Embodiment 2: Select basic components to assemble a three-channel internal mixing nozzle.

As shown in Figure 9, the three-channel internal mixing nozzle is composed of an end cover 1, an internal mixing plate 2, a nozzle plate 4, two adjusting nuts 5, a fastening nut 6, a crystallizer 7, and three anti-rotation pins 8. Two small sealing rings 9, one large sealing ring 10, and three limit screws 11 form.

The installation process is:

Screw in the limit screw 11 in the limit screw holes 5-2 and 6-2 on the adjustment nut 5 and the fastening nut 6, and then screw the limit screw 11 into the sealing groove 1-5 and the inner seal groove 1-5 on the nozzle core 1-6 of the end cover 1. A small sealing ring 9 is set in the sealing groove 2-12 on the nozzle core 2-13 of the mixing disc 2; a large sealing ring 10 is set in the sealing groove 4-11 on the crystallizer joint 4-13 of the spout plate 4 for standby.

Align the right-handed thread 5-1 of the first adjusting nut 5 with the right-handed thread 1-3 on the end cover 1, insert one end of the anti-rotation pin 8 into the anti-rotation pin hole 2-6 of the inner mixing disc 2, Install the nozzle core 1-6 of the end cover 1 into the inner hole 2-4 of the inner mixing plate 2, insert the other end of the anti-rotation pin 8 into the anti-rotation pin hole 1-4 of the end cover 1, and adjust the left-hand rotation of the nut 5 The thread 5-3 is aligned with the left-handed thread 2-7 of the inner mixing disc 2, and the adjusting nut 5 is turned to connect the end cover 1 and the inner mixing disc 2 at the same time. At this time, the nozzle cores of the nozzle cores 1-6 on the end cover 1 The cone 1-7 is in linear contact with the nozzle opening 2-5 at the conical bottom of the inner hole 2-4 of the inner mixing disc 2 without an annular gap. The limit half-groove 1-9 on the outer edge of the end face of the end cover 1 and the limit half-groove 2-3 on the end face outer edge of the inner mixing disc 2 form a limit groove, and the limit screw 11 on the adjustment nut 5 Correspondingly, the limit screw 11 is rotated, and the guide column of the limit screw 11 is inserted into the limit groove.

Then align the right-handed thread 5-1 of the second adjusting nut 5 with the right-handed thread 2-9 on the inner mixing disc 2, insert one end of the anti-rotation pin 8 into the anti-rotation pin hole 4-6 of the spout disc 4 , install the nozzle core 2-13 of the inner mixing disc 2 into the inner hole 4-4 of the nozzle disc 4, insert the other end of the anti-rotation pin 8 into the anti-rotation pin hole 2-10 of the inner mixing disc 2, adjust the nut 5 The left-handed thread 5-3 of the left-handed thread 5-3 is aligned with the left-handed thread 4-7 of the nozzle disc 4, and the adjusting nut 5 is turned to connect the inner mixing disc 2 and the nozzle disc 4 at the same time. At this time, the nozzle core 2-1 of the inner mixing disc 2 The nozzle core cone 2-14 is in linear contact with the nozzle opening 4-5 at the conical bottom of the inner hole 2-4 of the nozzle disk 4 without an annular gap. The limit half-groove 2-16 on the outer edge of the end face of the inner mixing disc 2 and the limit half-groove 4-3 on the end face outer edge of the spout plate 4 form a limit groove, and the limit screw 11 on the adjustment nut 5 Correspondingly, the limit screw 11 is rotated, and the guide column of the limit screw 11 is inserted into the limit groove.

When connecting the end cap 1 and the inner mixing disc 2 or the inner mixing disc 2 and the spout disc 4 with the adjusting nut 5, the number of threads screwed into the two connected parts is equal.

Finally, align the right-handed thread 6-1 of the fastening nut 6 with the right-handed thread 4-9 on the disc-shaped cylinder of the nozzle plate 4, and insert one end of the anti-rotation pin 8 into the anti-rotation pin hole 7- of the crystallizer 7 3, insert the crystallizer connector 4-13 of the spout plate 4 into the inner cavity 7-2 of the crystallizer 7, insert the other end of the anti-rotation pin 8 into the anti-rotation pin hole 4-10 of the spout plate 4, and tighten the nut The left-handed thread 6-3 of 6 is aligned with the left-handed thread 7-4 of the crystallizer 7, and the fastening nut 6 is turned to connect the spout plate 4 and the crystallizer 7 together; when the fastening nut 6 connects the spout plate 4 and the crystallizer 7 , the number of screw threads screwed into the two connected parts is equal. The limiting half-groove 4-14 on the outer edge of the end face of the nozzle plate 4 and the limiting half-groove 7-1 on the outer edge of the crystallizer 7 form a limiting groove, corresponding to the limiting screw 11 on the fastening nut 6 , turn the limit screw 11, and the guide column of the limit screw 11 is inserted into the limit slot.

The limiting half grooves 1-9, 2-3, 2-16, 4-3, 4-14, 7-1 processed along the circumferential direction on the outer edge of each end face are less than 360 degrees in the circumferential direction, such as 355 degrees or 350 degrees Unclosed half grooves. A set of three-channel internal mixing combined nozzles has been installed, and the fluid connection pipe 12 is connected to the fluid inlets 1-1, 2-1, and 4-1 by welding. The anti-rotation pin 8 guarantees that when rotating the adjusting nut 5 and the tightening nut 6, no rotation occurs between the end cover 1 and the inner mixing disc 2, the inner mixing disc 2 and the spout disc 4, the spout disc 4 and the crystallizer 7.

The installed three-channel internal mixing nozzle, the nozzle core cone 1-7 of the end cover 1 and the nozzle opening 2-5 of the inner mixing plate 2, the nozzle core cone 2-14 of the inner mixing plate 2 and the nozzle opening 4 of the nozzle plate 4 -5 constitutes the annular gaps of the two nozzles, and the two adjusting nuts 5 are rotated respectively to adjust the size of the annular gaps of the two nozzles.

In order to facilitate the adjustment of the annular gap, after the adjusting nut 5 adjusts the nozzle core cone 1-7 and the nozzle port 2-5 or the nozzle core cone 2-14 and the nozzle port 4-5 to a linear contact without an annular gap, respectively in the first The connecting position of the first adjusting nut 5 and the end cover 1, and the second adjusting nut 5 and the inner mixing plate 2 are simultaneously described as the "0" reference line, and then the adjusting nut 5 is calculated according to the pitch of the adjusting nut 5 and the taper of each nozzle core cone. After loosening in the opposite direction, each nozzle core cone and nozzle mouth will produce different ring gaps such as 5μm, 10μm, ..., 50μm, and the angle of rotation of the unit ring gap according to the adjustment nut 5 is used as the unit scale value, and the adjustment nut 5 Starting from the "0" reference line, draw scale lines in the direction of loosening sequentially, as the measurement basis for adjusting the size of the annular gap.

As shown in Figure 12, the relationship between the annular gap formed between the nozzle core cone and the nozzle opening, the pitch of the adjusting nut and the angle turned toward the loosening direction of the adjusting nut is shown in the following formula:

$\mathrm{<span\; class="notranslate">\; \&delta;</span>}<span\; class="notranslate">\; =</span>\frac{\mathrm{<span\; class="notranslate">\; 2</span>}\mathrm{<span\; class="notranslate">\; \&beta;<figure-callout\; id="360"\; label="t"\; filenames="HSA00000314784000051.png"\; state="\{\{state\}\}">t</figure-callout></span>}}{\mathrm{<span\; class="notranslate">\; 360</span>}}<span\; class="notranslate">\; \&times;</span>\mathrm{<span\; class="notranslate">\; sin</span>}\mathrm{<span\; class="notranslate">\; \&alpha;</span>}$

In the formula: δ is the annular gap formed between the nozzle core cone and the nozzle mouth; α is the cone angle of the nozzle core cone; t is the pitch of the adjusting nut; β is the angle turned toward the loosening direction of the adjusting nut.

The process of preparing nano-micron materials or ultra-fine powders with supercritical fluids using three-channel internal mixing nozzles: Take the preparation of single-material nano-micron materials or ultra-fine powders as an example. The carbon dioxide gas is produced through the usual supercritical carbon dioxide production method, that is, the carbon dioxide is refrigerated and liquefied first, pressurized by a booster pump to reach a critical pressure, and then enters a heater to raise the carbon dioxide temperature above the critical temperature to form supercritical carbon dioxide.

Dissolve the material to be prepared into a solvent that is miscible with supercritical carbon dioxide, and then drive it into the fluid inlet 2-1 and the fluid side channel 2-2 of the inner mixing plate 2 through the fluid connection pipe 12 through the booster pump, from the end cover 1 The annular gap formed between the nozzle core cone 1-7 and the nozzle opening 2-5 of the inner mixing plate 2 is ejected, and the formed mist fluid is sprayed from the fluid side to the nozzle hole 2-15 through the fluid center flow channel 2-11 Enter the mixing chamber formed between the inner mixing disc 2 and the nozzle disc 4, that is, the space formed by the nozzle core 2-13 and the inner hole 4-4; supercritical carbon dioxide enters the fluid inlet 4- 1 and the fluid side channel 4-2, mixed with the mist-like material solution to be prepared sprayed from the fluid side to the nozzle hole 2-15; after mixing, continue to mix from the nozzle core cone 2-14 of the inner mixing plate 2 and the nozzle plate 4 The annulus formed between 4-5 of the nozzles is quickly sprayed into the volume space of the crystallizer; the supercritical carbon dioxide takes away the solvent, and the materials to be prepared crystallize to form nano-micron materials or ultrafine powders. The fluid inlet 1-1 is used as an auxiliary channel to feed supercritical carbon dioxide or porous material suspension according to the process requirements, so as to enhance the atomization and crystallization of the material fluid to be prepared or achieve the effect of infiltrating into the porous material.

In order to increase the degree of turbulence when the material solution to be prepared, supercritical carbon dioxide and coating solution pass through the fluid side channels 2-2, 4-2 and the fluid center channel 1-2, and facilitate the mixing or mixing of these fluids when they pass through the nozzle annular gap For atomization, the fluid side channels 2-2 and 4-2 preferably adopt the structure of the hole wall with a helix 2-2-1 as shown in Figure 13, and the fluid central channel 1-2 preferably adopts the structure of the hole wall with a helix as shown in Figure 15 Line 2-11-1 structure; in order to strengthen the degree of turbulence of the fluid after atomization, to facilitate the further mixing or crystallization of the fluid, the fluid central channel 2-11 preferably adopts the helical line 2-11-1 on the hole wall as shown in Figure 15 Structure, the fluid side nozzle hole 2-15 preferably adopts the hole wall belt helix 2-15-1 structure shown in Figure 16, and the tapered fluid nozzle hole 4-12 preferably adopts the hole wall belt helix line shown in Figure 18 4-12-1 structure.

In order to make the material solution to be prepared, supercritical carbon dioxide, and coating solution rotate after passing through the fluid side channels 2-2, 4-2, and facilitate the mixing or atomization of these fluids when they pass through the nozzle annular gap, it is best to use Figure 14 Vertical or non-perpendicular configuration in which the axes of the fluid lateral passages 2-2, 4-2 do not intersect the axes of the inner bores 2-4, 4-4; enhance mixing with them in order to further swirl the atomized fluid The degree of mixing of the fluids is preferably a vertical or non-vertical structure in which the axes of the fluid side spray holes 2-15 and the axes of the nozzle core cone 2-14 do not intersect as shown in FIG. 17 .

The fluid side passages 2-2, 4-2 and the fluid side spray holes 2-15 preferably adopt the helical structure of the hole wall and the non-intersecting vertical or non-vertical structure of the axis to further enhance the turbulent flow of the fluid to be atomized or mixed The degree or degree of rotation is beneficial to the atomization, mixing and crystallization of the fluid.

3. Embodiment three: select basic components to assemble a three-channel external mixing nozzle.

As shown in Figure 10, the three-channel external mixing nozzle is composed of an end cover 1, an external mixing plate 3, a nozzle plate 4, two adjusting nuts 5, a fastening nut 6, a crystallizer 7, and three anti-rotation pins 8. Two small sealing rings 9, one large sealing ring 10, and three limit screws 11 form.

The installation process is:

First screw in the limit screw 11 in the limit screw holes 5-2, 6-2 on the adjustment nut 5 and the fastening nut 6, and seal the seal groove 1-5, outer Set small sealing ring 9 on the sealing groove 3-12 on the nozzle core 3-13 of mixing disc 3; Set large sealing ring 10 in the sealing groove 4-11 on the crystallizer joint 4-13 of spout plate 4 for standby.

Align the right-handed thread 5-1 of the first adjusting nut 5 with the right-handed thread 1-3 on the end cover 1, insert one end of the anti-rotation pin 8 into the anti-rotation pin hole 3-6 of the outer mixing disc 3, Install the nozzle core 1-6 of the end cover 1 into the inner hole 3-4 of the outer mixing disc 3, insert the other end of the anti-rotation pin 8 into the anti-rotation pin hole 1-4 of the end cover 1, and adjust the left-hand rotation of the nut 5 Thread 5-3 is aligned with the left-hand thread 2-7 of the outer mixing disc 3, and continue to turn the adjusting nut 5 to connect the end cover 1 and the outer mixing disc 3 together. At this time, the nozzle cores of the nozzle cores 1-6 on the end cover 1 The cone 1-7 is in linear contact with the nozzle opening 3-5 at the conical bottom of the inner hole 3-4 of the outer mixing disc 3 without an annular gap. The limit half groove 1-9 on the outer edge of the end cover 1 end face and the limit half groove 3-3 on the end face outer edge that the outer mixing disc 3 cooperates form a limit groove, and the limit screw 11 on the adjustment nut 5 Correspondingly, the limit screw 11 is rotated, and the guide column of the limit screw 11 is inserted into the limit groove.

Then align the right-handed thread 5-1 of the second adjusting nut 5 with the right-handed thread 3-9 on the outer mixing disc 3, insert one end of the anti-rotation pin 8 into the anti-rotation pin hole 4-6 of the spout disc 4 , install the nozzle core 3-13 of the outer mixing disc 3 into the inner hole 4-4 of the nozzle disc 4, insert the other end of the anti-rotation pin 8 into the anti-rotation pin hole 3-10 of the outer mixing disc 3, adjust the nut 5 The left-handed thread 5-3 of the nozzle plate 4 is aligned with the left-handed thread 4-7 of the nozzle disc 4, and the adjusting nut 5 is turned to connect the outer mixing disc 3 and the nozzle disc 4 at the same time. At this time, the nozzle core 3-1 of the outer mixing disc 3 The nozzle core cone 3-14 is in linear contact with the nozzle opening 4-5 at the conical bottom of the inner hole 4-4 of the nozzle disk 4 without an annular gap. The limit half-groove 3-16 on the outer edge of the outer mixing disc 3 end face and the limit half-groove 4-3 on the end face outer edge of the spout plate 4 form a limit groove, and the limit screw 11 on the adjustment nut 5 Correspondingly, the limit screw 11 is rotated, and the guide column of the limit screw 11 is inserted into the limit groove.

When connecting the end cap 1 and the outer mixing disc 3 or the outer mixing disc 3 and the spout disc 4 with the adjusting nut 5, the number of threads screwed into the two connected parts is equal.

Finally, align the right-handed thread 6-1 of the fastening nut 6 with the right-handed thread 4-9 on the disc-shaped cylinder of the nozzle plate 4, and insert one end of the anti-rotation pin 8 into the anti-rotation pin hole 7- of the crystallizer 7 3, insert the crystallizer connector 4-13 of the spout plate 4 into the inner cavity 7-2 of the crystallizer 7, insert the other end of the anti-rotation pin 8 into the anti-rotation pin hole 4-10 of the spout plate 4, and tighten the nut The left-handed thread 6-3 of 6 is aligned with the left-handed thread 7-4 of the crystallizer 7, and the fastening nut 6 is turned to connect the spout plate 4 and the crystallizer 7 together; when the fastening nut 6 connects the spout plate 4 and the crystallizer 7 , the number of screw threads screwed into the two connected parts is equal. The limiting half-groove 4-14 on the outer edge of the end face of the nozzle plate 4 and the limiting half-groove 7-1 on the outer edge of the crystallizer 7 form a limiting groove, corresponding to the limiting screw 11 on the fastening nut 6 , turn the limit screw 11, and the guide column of the limit screw 11 is inserted into the limit slot.

The limiting half grooves 1-9, 3-3, 3-16, 4-3, 4-14, 7-1 processed along the circumferential direction on the outer edge of each end face are less than 360 degrees in the circumferential direction, such as 355 degrees or 350 degrees Unclosed half grooves. A set of three-channel external mixing combined nozzles has been installed, and the fluid connection pipe 12 is connected to the fluid inlets 1-1, 3-1, and 4-1 by welding. The anti-rotation pin 8 guarantees that when rotating the adjusting nut 5 and the fastening nut 6, no rotation occurs between the end cover 1 and the outer mixing disc 3, the outer mixing disc 3 and the spout disc 4, the spout disc 4 and the crystallizer 7.

The installed three-channel external mixing nozzle, the nozzle core cone 1-7 of the end cover 1 and the nozzle opening 3-5 of the external mixing plate 3, the nozzle core cone 3-14 of the external mixing plate 3 and the nozzle opening 4 of the nozzle plate 4 -5 constitutes the annular gaps of the two nozzles, and the two adjusting nuts 5 are rotated respectively to adjust the size of the annular gaps of the two nozzles.

In order to facilitate the adjustment of the annular gap, after the adjusting nut 5 adjusts the nozzle core cone 1-7 and the nozzle port 3-5 or the nozzle core cone 3-14 and the nozzle port 4-5 to linear contact without an annular gap, respectively, in the first The connecting position of the first adjusting nut 5 and the end cover 1, and the second adjusting nut 5 and the outer mixing plate 3 are simultaneously described as the "0" reference line, and then the adjusting nut 5 is calculated according to the pitch of the adjusting nut 5 and the taper of each nozzle core cone. After loosening in the opposite direction, each nozzle core cone and nozzle mouth will produce different ring gaps such as 5μm, 10μm, ..., 50μm, and the angle of rotation of the unit ring gap according to the adjustment nut 5 is used as the unit scale value, and the adjustment nut 5 Starting from the "0" reference line, draw scale lines in the direction of loosening sequentially, as the measurement basis for adjusting the size of the annular gap.

As shown in Figure 12, the relationship between the annular gap formed between the nozzle core cone and the nozzle opening, the pitch of the adjusting nut and the angle turned toward the loosening direction of the adjusting nut is shown in the following formula:

$\mathrm{<span\; class="notranslate">\; \&delta;</span>}<span\; class="notranslate">\; =</span>\frac{\mathrm{<span\; class="notranslate">\; 2</span>}\mathrm{<span\; class="notranslate">\; \&beta;<figure-callout\; id="360"\; label="t"\; filenames="HSA00000314784000051.png"\; state="\{\{state\}\}">t</figure-callout></span>}}{\mathrm{<span\; class="notranslate">\; 360</span>}}<span\; class="notranslate">\; \&times;</span>\mathrm{<span\; class="notranslate">\; sin</span>}\mathrm{<span\; class="notranslate">\; \&alpha;</span>}$

In the formula: δ is the annular gap formed between the nozzle core cone and the nozzle mouth; α is the cone angle of the nozzle core cone; t is the pitch of the adjusting nut; β is the angle turned toward the loosening direction of the adjusting nut.

The process of preparing nano-micron materials or ultra-fine powders with supercritical fluids using three-channel external mixing nozzles: Take the preparation of single-material nano-micron materials or ultra-fine powders as an example. The carbon dioxide gas is produced through the usual supercritical carbon dioxide production method, that is, the carbon dioxide is refrigerated and liquefied first, pressurized by a booster pump to reach a critical pressure, and then enters a heater to raise the carbon dioxide temperature above the critical temperature to form supercritical carbon dioxide. Dissolve the material to be prepared in a solvent miscible with supercritical carbon dioxide, and then drive it into the fluid inlet 3-1 and the fluid side channel 3-2 of the outer mixing plate 3 through the fluid connection pipe 12 through the booster pump, from the end cover 1 The annular gap formed between the nozzle core cone 1-7 and the nozzle port 3-5 of the outer mixing disc 3 is ejected, and the formed mist fluid is sprayed to the crystallizer 7 volume space through the fluid center channel 3-11; supercritical carbon dioxide Drive into the fluid inlet 4-1 and the fluid side channel 4-2 of the nozzle plate 4 through the fluid connecting pipe 12, from the ring formed between the nozzle core cone 3-14 of the outer mixing plate 3 and the nozzle opening 4-5 of the nozzle plate 4 The gap is quickly sprayed to the volume space of the crystallizer 7; the two mist fluids meet on the way to the volume space of the crystallizer 7, and the supercritical carbon dioxide takes away the solvent, that is, the two are mixed outside the nozzle, and the materials to be prepared are crystallized to form nano-micron materials or ultrafine powder. The fluid inlet 1-1 is used as an auxiliary channel to feed supercritical carbon dioxide or porous material suspension according to the process requirements, so as to enhance the atomization and crystallization of the material fluid to be prepared or achieve the effect of infiltrating into the porous material.

In order to increase the degree of turbulence when the material solution to be prepared, supercritical carbon dioxide and coating solution pass through the fluid side channels 3-2, 4-2 and the fluid center channel 1-2, and facilitate the mixing or mixing of these fluids when they pass through the nozzle annular gap Atomization, the fluid lateral channel 3-2,4-2 preferably adopts the hole wall band helix 2-2-1 structure shown in Figure 13, and the fluid center channel 1-2 preferably adopts the hole wall band spiral line shown in Figure 15 Line 2-11-1 structure; in order to strengthen the degree of turbulence of the fluid after atomization and facilitate the further mixing or crystallization of the fluid, the fluid central channel 3-11 preferably adopts the helical line 2-11-1 on the hole wall as shown in Figure 15 Structure, and the conical fluid nozzle hole 4-12 preferably adopts the hole wall belt helix 4-12-1 structure shown in Figure 18.

In order to make the material solution to be prepared, supercritical carbon dioxide, and coating solution rotate after passing through the fluid side channels 3-2, 4-2, and facilitate the mixing or atomization of these fluids when they pass through the nozzle annular gap, it is best to use Figure 14 A vertical or non-perpendicular structure in which the axes of the fluid lateral passages 3-2, 4-2 and the axes of the inner holes 3-4, 4-4 are non-intersecting are shown.

The fluid side passages 3-2 and 4-2 preferably adopt the helical structure of the hole wall and the non-intersecting vertical or non-vertical structure of the axis to further enhance the degree of turbulence or rotation of the fluid to be atomized or mixed, which is beneficial to the mist of the fluid. liquefied, mixed and crystallized out.

4. Embodiment 4: select basic components to assemble a two-channel rapid expansion nozzle.

As shown in Figure 11, the two-channel rapid expansion nozzle is composed of an end cover 1, a nozzle plate 4, an adjusting nut 5, a fastening nut 6, a crystallizer 7, two anti-rotation pins 8, and a small sealing ring 9. A large sealing ring 10 and two limit screws 11 are formed.

The installation process is:

Screw in the limit screw 11 in the limit screw holes 5-2 and 6-2 on the adjusting nut 5 and the fastening nut 6, and set it on the sealing groove 1-5 on the nozzle core 1-6 of the end cover 1 Small sealing ring 9; Set large sealing ring 10 in the sealing groove 4-11 on the crystallizer joint 4-13 of spout plate 4 for subsequent use.

Align the right-handed thread 5-1 of the adjusting nut 5 with the right-handed thread 1-3 on the end cover 1, insert one end of the anti-rotation pin 8 into the anti-rotation pin hole 4-6 of the spout plate 4, and place the end cover 1 The nozzle core 1-6 is installed into the inner hole 4-4 of the nozzle plate 4, the other end of the anti-rotation pin 8 is inserted into the anti-rotation pin hole 1-4 of the end cover 1, and the left-hand thread 5-3 of the adjustment nut 5 is aligned The left-hand thread 4-7 of the nozzle plate 4, turn the adjusting nut 5 and connect the end cover 1 and the nozzle plate 4 together, at this time, the nozzle core 1-6 on the end cover 1 and the nozzle core cone 1-7 of the nozzle plate 4 The nozzle mouth 3-5 at the bottom of the inner hole 4-4 is in linear contact with no annular gap. The limit half-groove 1-9 on the outer edge of the end cover 1 end face and the limit half-groove 4-3 on the end face outer edge that the spout disc 4 cooperates form a limit groove, and the limit screw 11 on the adjusting nut 5 is in phase. Correspondingly, the limit screw 11 is rotated, and the guide column of the limit screw 11 is inserted into the limit slot. When connecting the end cover 1 and the spout plate 4 with the adjusting nut 5, the number of threads screwed into the two connected parts is equal.

Finally, align the right-handed thread 6-1 of the fastening nut 6 with the right-handed thread 4-9 on the disc-shaped cylinder of the nozzle plate 4, and insert one end of the anti-rotation pin 8 into the anti-rotation pin hole 7- of the crystallizer 7 3, insert the crystallizer connector 4-13 of the spout plate 4 into the inner cavity 7-2 of the crystallizer 7, insert the other end of the anti-rotation pin 8 into the anti-rotation pin hole 4-10 of the spout plate 4, and tighten the nut The left-handed thread 6-3 of 6 is aligned with the left-handed thread 7-4 of the crystallizer 7, and the fastening nut 6 is turned to connect the spout plate 4 and the crystallizer 7 together; when the fastening nut 6 connects the spout plate 4 and the crystallizer 7 , the number of screw threads screwed into the two connected parts is equal. The limiting half-groove 4-14 on the outer edge of the end face of the nozzle plate 4 and the limiting half-groove 7-1 on the outer edge of the crystallizer 7 form a limiting groove, corresponding to the limiting screw 11 on the fastening nut 6 , turn the limit screw 11, and the guide column of the limit screw 11 is inserted into the limit slot.

The limiting half-grooves 1-9, 4-3, 4-14, 7-1 processed in the circumferential direction on the outer edge of each end face are non-closed half-grooves less than 360 degrees in the circumferential direction, such as 355 degrees or 350 degrees. A set of two-channel rapid expansion combined nozzles is installed, and the fluid connection pipe 12 is connected to the fluid inlets 1-1, 4-1 by welding. The anti-rotation pin 8 guarantees that when the adjusting nut 5 and the fastening nut 6 are rotated, no rotation occurs between the end cover 1 and the nozzle disc 4, the nozzle disc 4 and the crystallizer 7.

The installed two-channel rapid expansion nozzle forms a nozzle annular gap by the nozzle core cone 1-7 of the end cover 1 and the nozzle opening 4-5 of the nozzle plate 4, and the adjusting nut 5 is rotated to adjust the size of the nozzle annular gap.

In order to facilitate the adjustment of the annular gap, the adjusting nut 5 adjusts the nozzle core cone 1-7 and the nozzle mouth 4-5 to linear contact without an annular gap, and at the same time the adjusting nut 5 and the end cover 1 draw a "0" reference line at the same time, Then according to the pitch of the adjusting nut 5 and the taper of the nozzle core cone, it is calculated that after the adjusting nut 5 is loosened in the opposite direction, different annular gaps such as 5 μm, 10 μm, ..., 50 μm will be produced between the nozzle core cone and the nozzle mouth, according to the adjusting nut 5 Adjust the rotation angle of the unit ring gap as the unit scale value, start from the "0" reference line on the adjustment nut 5, and draw the scale line in the direction of loosening sequentially, as the measurement basis for adjusting the size of the ring gap.

As shown in Figure 12, the relationship between the annular gap formed between the nozzle core cone and the nozzle opening, the pitch of the adjusting nut and the angle turned toward the loosening direction of the adjusting nut is shown in the following formula:

$\mathrm{<span\; class="notranslate">\; \&delta;</span>}<span\; class="notranslate">\; =</span>\frac{\mathrm{<span\; class="notranslate">\; 2</span>}\mathrm{<span\; class="notranslate">\; \&beta;<figure-callout\; id="360"\; label="t"\; filenames="HSA00000314784000051.png"\; state="\{\{state\}\}">t</figure-callout></span>}}{\mathrm{<span\; class="notranslate">\; 360</span>}}<span\; class="notranslate">\; \&times;</span>\mathrm{<span\; class="notranslate">\; sin</span>}\mathrm{<span\; class="notranslate">\; \&alpha;</span>}$

In the formula: δ is the annular gap formed between the nozzle core cone and the nozzle mouth; α is the cone angle of the nozzle core cone; t is the pitch of the adjusting nut; β is the angle turned toward the loosening direction of the adjusting nut.

The process of preparing nano-micron materials or ultra-fine powders by using two-channel rapid expansion nozzles for rapid expansion of supercritical fluids: Take the preparation of single-material nano-micron materials or ultra-fine powders as an example. The carbon dioxide gas is produced through the usual supercritical carbon dioxide production method, that is, the carbon dioxide is refrigerated and liquefied first, pressurized by a booster pump to reach a critical pressure, and then enters a heater to raise the carbon dioxide temperature above the critical temperature to form supercritical carbon dioxide.

First let the supercritical carbon dioxide pass through the dissolving kettle containing the materials to be prepared, so that the prepared materials are dissolved into the supercritical carbon dioxide, and then enter the fluid inlet 4-1 and the fluid side channel 4-2 of the nozzle plate 4 through the fluid connection pipe 12, and dissolve to be dissolved. The supercritical carbon dioxide solution of the prepared material is quickly sprayed into the volume space of the crystallizer 7 from the annular gap formed between the nozzle core cone 1-7 of the end cover 1 and the nozzle opening 4-5 of the nozzle plate 4; the supercritical carbon dioxide fluid suddenly decompresses and expands , the material to be prepared is precipitated to form polycrystalline nano-micron material or ultrafine powder. The fluid inlet 1-1 is used as an auxiliary channel, and carbon dioxide can be introduced according to the process requirements to strengthen the atomization and crystallization of the materials to be prepared.

In order to increase the degree of turbulence when the supercritical carbon dioxide solution and supercritical carbon dioxide of the materials to be prepared pass through the fluid side channel 4-2 and the fluid central channel 1-2, and facilitate the mixing or atomization of these fluids when they pass through the nozzle annular gap, the fluid side The channel 4-2 preferably adopts the structure of the hole wall with a helix 2-2-1 shown in Figure 13, and the fluid center channel 1-2 preferably adopts the structure of the hole wall with a helix 2-11-1 shown in Figure 15; To enhance the turbulence of the fluid after atomization, it is convenient for further mixing or crystallization of the fluid. The tapered fluid nozzle 4-12 preferably adopts the structure of the hole wall with a helix 4-12-1 as shown in FIG. 18 .

In order to make the supercritical carbon dioxide solution of the material to be prepared and the supercritical carbon dioxide rotate through the fluid side channel 4-2, and facilitate the mixing or atomization of these fluids when they pass through the nozzle annulus, it is best to use the fluid side channel 4-2 shown in Figure 14. A vertical or non-perpendicular structure in which the axis of the channel 4-2 does not intersect the axis of the inner hole 4-4.

The fluid side channel 4-2 preferably adopts the helical structure of the hole wall and the non-intersecting vertical or non-vertical structure of the axis to further enhance the degree of turbulence or rotation of the fluid to be atomized or mixed, which is beneficial to the atomization, mixing and Crystallized out.

5. Embodiment five: Select basic components to assemble a two-channel external mixing nozzle.

As shown in Figure 11, the two-channel internal mixing nozzle is assembled according to the same components and installation steps as in the fourth embodiment. The difference is that:

Dissolve the material to be prepared into a solvent that is miscible with supercritical carbon dioxide, and drive the solution of the material to be prepared and supercritical carbon dioxide into the fluid inlet 1-1 of the end cover 1 and the nozzle plate 4 respectively through the fluid connection pipe 12 through the booster pump Fluid inlet 4-1, the material solution to be prepared is sprayed from the fluid center nozzle hole 1-8 through the fluid center channel 1-2 of the end cover 1; and the fluid inlet 4-1 from the nozzle plate 4 and the fluid side channel 4- 2 enters, the supercritical carbon dioxide ejected rapidly through the annular gap formed between the nozzle core cone 1-7 of the end cover 1 and the nozzle opening 4-5 of the nozzle plate 4 meets, and the supercritical carbon dioxide takes away the solvent, that is, the two are in the nozzle Mixing is realized externally, and the materials to be prepared crystallize to form nano-micron materials or ultrafine powders.

The above combined nozzles have a simplified structure and a small volume, saving a large amount of raw materials. The manufacturing and processing technology has excellent performance, the cumulative error of components is small, the installation accuracy is high, and the processing and manufacturing cost is low. In application, the adjustment procedure is simple, the operation is convenient, the production quality is excellent, and the work efficiency is high.

Claims (2)

1. A combined nozzle for the preparation of supercritical fluid nano-micron materials, characterized in that it consists of an end cover, an inner mixing disc, an outer mixing disc, a spout disc, a crystallizer, also known as a collector, an adjusting nut, a fastening nut, and a stop pin , limit screw, sealing ring basic components; The end cover is a combination of a disc-shaped cylinder and a thin cylindrical nozzle core coaxially connected. There is a fluid center channel at the axial center of the combination. The orifice of the fluid center channel on the end face of the disc-shaped cylinder is a fluid inlet; The thread is processed on the cylindrical surface of the disc-shaped cylinder, and the anti-rotation pin hole is processed on the end surface of the disc-shaped cylinder coaxially connected with the nozzle core and matched with the anti-rotation pin hole on the matching part. The outer edge of the end surface is along the ring A half-groove is machined to limit; the sealing groove is processed on the cylindrical surface of the nozzle core, and there is a nozzle core cone composed of a small cylinder and a cone at the end of the nozzle core, and the fluid nozzle hole is processed in the center of the nozzle core cone to communicate with the fluid center channel; The inner mixing disc is a combination of a disc-shaped cylinder and a thin cylindrical nozzle core coaxially connected. The inner hole and the fluid center channel are processed at the axial center of the combination. The bottom of the inner hole is tapered; The middle part of the cylindrical surface is processed with undercut grooves, the upper and lower positions of the undercut grooves are respectively processed with left and right-handed threads, and the fluid side channels are processed along the radial direction to communicate with the bottom of the inner hole, and the fluid side channel openings are fluid inlets; disc shape There are anti-rotation pin holes on both ends of the cylinder, which are matched with the anti-rotation pin holes of the matching parts; the outer edges of the two ends of the disc-shaped cylinder are respectively machined with half grooves along the ring direction; the cylindrical surface of the nozzle core is processed to seal There is a nozzle core cone composed of a small cylinder and a cone at the end of the nozzle core, and the fluid side nozzle hole is processed on the small cylinder of the nozzle core cone to communicate with the fluid central channel; The outer mixing disc is a combination of a disc-shaped cylinder and a thin cylindrical nozzle core coaxially connected. The inner hole and the fluid center channel are processed at the axial center of the combination. The bottom of the inner hole is tapered; The middle part of the cylindrical surface is processed with undercut grooves, the upper and lower positions of the undercut grooves are respectively processed with left and right-handed threads, and the fluid side channels are processed along the radial direction to communicate with the bottom of the inner hole, and the fluid side channel openings are fluid inlets; disc shape There are anti-rotation pin holes on both ends of the cylinder, which are matched with the anti-rotation pin holes of the matching parts; the outer edges of the two ends of the disc-shaped cylinder are respectively machined with half grooves along the ring direction; the cylindrical surface of the nozzle core is processed to seal There is a nozzle core cone composed of a small cylinder and a cone at the end of the nozzle core, and the fluid nozzle hole is processed in the center of the nozzle core cone to communicate with the fluid center channel; The spout disc is a combination of a disc-shaped cylinder coaxially connected with a disc-shaped cylinder, a disc-cover joint, and a crystallizer joint. The joint is used to connect the end cover, the inner mixing plate or the outer mixing plate, and the crystallizer joint is used to connect the crystallizer; the inner hole and the conical fluid spray hole are coaxially processed at the axial center of the combination, and the bottom of the inner hole is Conical; the cylinder at one end of the inner hole is the disc cover joint, and the connecting thread is processed on the disc cover joint. Matching; the outer edge of the end face of the disc cover joint is processed along the circumferential direction to limit the half groove, and along its radial direction, the lateral passage of the fluid is communicated with the bottom of the inner hole. The anti-rotation pin holes are correspondingly matched; the cylinder at one end of the tapered fluid injection hole is the mold joint, and the sealing groove is processed on the mold joint, and its diameter matches the inner cavity diameter of the mold installation part; the disc-shaped cylinder cylinder The thread is processed on the top, and its diameter and direction of rotation match the connecting part of the crystallizer, and the anti-rotation pin hole is correspondingly processed on the connecting part of the end face matched with the crystallizer; The crystallizer is a pressure-bearing cylinder, and the anti-rotation pin hole is correspondingly processed on the end face connected with the spout plate, and the thread is correspondingly processed on the cylindrical surface connected with the spout plate, and the limit half groove is opened on the edge of the end face of the crystallizer; The inner hole diameter, depth and taper of the bottom of the inner mixing plate, outer mixing plate, and nozzle plate match the outer diameter, length, and taper of the nozzle core of the end cover, inner mixing plate, and outer mixing plate. , interchangeable, the matching relationship between the outer diameter of the nozzle core and the inner hole of each fitting is a close fit; The internal thread of the adjusting nut is two sections of thread in opposite directions, separated by a relief groove in the middle, and matched with the threads of the end cover, the inner mixing plate, the outer mixing plate, and the nozzle plate respectively. There are screw holes on the nut wall and Install the limit screw; the internal thread of the fastening nut is two opposite threads, separated by a relief groove in the middle, and matches the threads of the spout plate and the crystallizer interface installation part respectively. There are screw holes on the nut wall and installed limit screw; According to the requirements of the preparation process of supercritical fluid nano-micron materials or ultrafine powders, the above-mentioned basic components with uniform installation dimensions are selected to assemble multi-channel internal mixing nozzles, multi-channel external mixing nozzles, multi-channel internal and external mixing nozzles or rapid expansion nozzles ; The multi-channel internal mixing nozzle is composed of an end cover, at least one internal mixing plate, nozzle plate, and crystallizer. After installing the sealing ring in the nozzle core sealing groove of the end cover, it is installed into the inner hole of the internal mixing plate, and the internal mixing plate Install the sealing ring in the sealing groove of the nozzle core and then install it into the inner hole of the secondary inner mixing plate or the inner hole of the spout plate, install the sealing ring in the sealing groove on the crystallizer joint of the spout plate and then install it into the inner cavity of the crystallizer, Install the anti-rotation pins in the anti-rotation pin holes corresponding to the end faces between the fittings; use the adjusting nut to connect the end cover with the inner mixing plate, the inner mixing plate and the nozzle plate, and screw in the limit screw on the adjusting nut to make The guide column is inserted into the limit groove formed by the two fittings; the spout plate and the crystallizer are connected together with a fastening nut, and the limit screw on the fastening nut is screwed in so that the guide post is inserted into the limit groove composed of the two fittings. limit groove; The multi-channel external mixing nozzle is composed of an end cover, at least one external mixing plate, nozzle plate, and crystallizer. After installing the sealing ring in the nozzle core sealing groove of the end cover, it is installed into the inner hole of the external mixing plate. After installing the sealing ring in the sealing groove of the nozzle core, install it into the inner hole of the secondary outer mixing plate or the inner hole of the nozzle plate, install the sealing ring in the sealing groove on the crystallizer joint of the nozzle plate, and then install it into the inner cavity of the mold. Install the anti-rotation pins in the anti-rotation pin holes corresponding to the end faces between the fittings; use the adjusting nut to connect the end cover with the outer mixing plate, the outer mixing plate and the nozzle plate, and screw in the limit screw on the adjusting nut to make it The guide column is inserted into the limit groove formed by the two fittings; the spout plate and the crystallizer are connected together with a fastening nut, and the limit screw on the fastening nut is screwed in so that the guide post is inserted into the limit groove formed by the two fittings. bit groove; The multi-channel internal and external mixing nozzle is composed of an end cover, at least one inner mixing plate, at least one outer mixing plate, nozzle plate, and crystallizer; install the sealing ring in the sealing groove of the nozzle core of the end cover and then install it into the inner mixing plate Install the sealing ring in the nozzle core sealing groove of the inner mixing plate and then install it into the inner hole of the outer mixing plate, install the sealing ring in the nozzle core sealing groove of the outer mixing plate and install it into the inner hole of the nozzle plate, Install the sealing ring in the sealing groove on the crystallizer joint of the disc and install it into the inner cavity of the crystallizer, and install the anti-rotation pin in the corresponding anti-rotation pin hole on the end face between the fittings; use the adjusting nut to connect the end cover and the inner mixing disc. , The inner mixing plate and the outer mixing plate, the outer mixing plate and the spout plate are connected together, and the limit screw on the adjusting nut is screwed in so that the guide column is inserted into the limit groove formed by the two matching parts; the spout is fixed with the fastening nut The plate and the crystallizer are connected together, and the limit screw on the fastening nut is screwed in so that the guide column is inserted into the limit groove formed by the two matching parts; The rapid expansion nozzle is composed of an end cover, a spout plate, and a crystallizer; install a sealing ring in the sealing groove of the nozzle core of the end cover and then install it into the inner hole of the spout plate, and install a sealing ring in the sealing groove on the crystallizer joint of the spout plate Finally, install it into the inner cavity of the crystallizer; install the anti-rotation pin in the corresponding anti-rotation pin hole on the end face between the fittings; use the adjustment nut to connect the end cover and the nozzle plate together, and screw in the limit screw on the adjustment nut The guide column is inserted into the limit groove formed by the two fittings; the spout plate and the crystallizer are connected together with a fastening nut, and the limit screw on the fastening nut is screwed in so that the guide post is inserted into the limit groove composed of the two fittings. limit groove. 2. according to the described combination nozzle of a kind of supercritical fluid nanometer material preparation of claim 1, it is characterized in that described end cap, inner mixing disc, outer mixing disc, fluid center channel or fluid side channel on the spout disc The hole wall of the inner mixing plate, the fluid side nozzle hole of the outer mixing plate, the fluid central nozzle hole of the outer mixing plate, and the hole wall of the conical fluid nozzle hole of the nozzle plate are smooth or with helical lines; the inner mixing plate, the outer mixing plate The axis of the fluid lateral channel on the mixing plate and the nozzle plate intersects or does not intersect with the axis of the component, and the axis of the fluid lateral orifice of the inner mixing plate intersects or does not intersect with the axis of the component, and the intersecting or non-intersecting two axes are perpendicular to each other or non-vertical. the

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