Static crystallizer for benzotriazole

Abstract

The utility model relates to a static crystallizer for benzotriazole. Comprising a bottom frame, a box body fixed in the bottom frame, a liquid inlet pipe which is vertically inserted into the top of the box body and is communicated with the interior of the box body, a liquid discharge pipe which is transversely inserted into the lower part of one side of the box body and is communicated with the interior of the box body, and a discharge pipe which is vertically inserted into the bottom of the box body and is communicated with the interior of the box body, the at least one temperature adjusting assembly is arranged in the box body; the temperature adjusting assembly comprises a plurality of temperature adjusting devices which are vertically arranged and are sequentially distributed at equal intervals from front to back, and two liquid guiding units which are arranged above the temperature adjusting devices and are distributed in a central symmetry mode; according to the device disclosed by the utility model, the form stability of the benzotriazole crystal is effectively improved, so that the benzotriazole crystal with higher purity can be obtained, and the yield is effectively improved; in addition, the method has a wide application range.

Description

TECHNICAL FIELD

[0001] The utility model relates to a static crystallizer of benzotriazole. BACKGROUND

[0002] The o-diaminobenzene method is the most classic method for preparing benzotriazole, and has the advantage of high purity of the prepared benzotriazole; the main steps of the o-diaminobenzene method are as follows: o-diaminobenzene is reacted with sodium nitrite in glacial acetic acid to generate o-aminobenzene diazonium salt, which is then immediately cyclized to obtain crude benzotriazole, and then the crude product is crystallized and dried to obtain the pure product; the existing benzotriazole mostly adopts a dynamic crystallization process, and the dynamic crystallization has the advantages of saving time and energy, because the dynamic crystallization directly occurs in the process of reaction, but it is difficult to control the temperature change, resulting in unstable morphology of the benzotriazole crystal, and thus it is impossible to obtain a benzotriazole crystal with high purity, and the yield is also low; in addition, the types of required equipment are more, the structure is relatively complex, the volume is large, and the cost is high, so it is only suitable for large-scale production, and thus the application range is small, and further improvement is needed. SUMMARY

[0003] In view of the above-mentioned status of the prior art, the technical problem to be solved by the utility model is to provide a static crystallizer of benzotriazole which effectively improves the morphological stability of the benzotriazole crystal, can obtain a benzotriazole crystal with high purity and effectively improve the yield, and has a large application range.

[0004] The utility model adopts the technical scheme that a static crystallizer of benzotriazole is provided, characterized in that the static crystallizer comprises a bottom frame, a box body fixed in the bottom frame, a liquid inlet pipe vertically inserted at the top of the box body and in communication with the inside of the box body, a liquid outlet pipe horizontally inserted below one side of the box body and in communication with the inside of the box body, a discharge pipe vertically inserted at the bottom of the box body and in communication with the inside of the box body, and at least one temperature adjusting assembly arranged in the box body.

[0005] The temperature adjusting assembly comprises a plurality of temperature adjusters vertically arranged and equally spaced from front to back, and two liquid guiding units symmetrically arranged above the temperature adjusters.

[0006] The liquid guiding unit comprises a first shunt pipe and a second shunt pipe horizontally arranged and parallel to each other, a plurality of through pipes horizontally arranged between the first shunt pipe and the second shunt pipe and equally spaced along the length direction of the first shunt pipe or the second shunt pipe, and an external connecting pipe vertically inserted in the second shunt pipe and in communication with the inside of the second shunt pipe, the end opening of the external connecting pipe is sealed upward through the top of the box body and extends above the box body, and the two end openings of each through pipe are respectively inserted in the first shunt pipe and the second shunt pipe and in communication with the inside of the first shunt pipe and the second shunt pipe.

[0007] The temperature regulator comprises a vertically arranged plate-shaped circulating tank and two vertically inserted connecting pipes which are arranged on the top of the plate-shaped circulating tank and are in communication with the interior of the plate-shaped circulating tank.

[0008] The end opening of one of the connecting pipes in each temperature regulator is inserted into and in communication with the interior of the first shunt pipe in one of the liquid guiding units, and the end opening of the other connecting pipe in each temperature regulator is inserted into and in communication with the interior of the first shunt pipe in the other liquid guiding unit.

[0009] Preferably, the interior of the plate-shaped circulating tank is further fixed with a vertically arranged partition plate which divides the interior of the plate-shaped circulating tank into two front and back symmetrically arranged and equal volume shunt cavities, and the root opening of each connecting pipe is in communication with the interior of the two shunt cavities.

[0010] Preferably, the interior of each shunt cavity is further provided with a drainage module which comprises a rectangular frame fixed between the corresponding side outer wall of the partition plate and the corresponding side inner wall of the plate-shaped circulating tank and an L-shaped baffle arranged in the interior of the rectangular frame.

[0011] Preferably, one end of the L-shaped baffle is fixed on the upper side inner wall of the rectangular frame, and the other end of the L-shaped baffle is arranged towards and spaced apart from the left or right side inner wall of the rectangular frame, and the L-shaped baffle divides the interior of the shunt cavity into an L-shaped flow channel and a rectangular cavity, and the root opening of each connecting pipe is in communication with the interior of the L-shaped flow channel and the rectangular cavity, respectively.

[0012] Preferably, the interior of the rectangular cavity is further provided with a plurality of first straight baffles which are transversely arranged and sequentially arranged from top to bottom, one end of each first straight baffle is fixed on the right or left side inner wall of the rectangular frame, and the other end of each first straight baffle is spaced apart from the right or left outer wall of the L-shaped baffle.

[0013] Preferably, the upper side of each first straight baffle is further provided with a second straight baffle which is transversely arranged, each second straight baffle is arranged in the interior of the rectangular cavity, one end of each second straight baffle is fixed on the right or left outer wall of the L-shaped baffle, and the other end of each second straight baffle is spaced apart from the right or left inner wall of the rectangular frame.

[0014] Preferably, the plurality of first straight baffles and the plurality of second straight baffles form a serpentine flow channel in the interior of the rectangular cavity.

[0015] Preferably, a plurality of uniformly distributed sink cavities are formed on the front and rear outer walls of the plate-shaped circulation tank.

[0016] Preferably, a protective frame is further fixed outside the plate-shaped circulation tank, and the two connecting pipes are both connected to the upper side of the protective frame.

[0017] Preferably, a top frame is further fixed on the top opening of the bottom frame and covers the top periphery of the tank body; a perforated plate is further arranged inside the tank body and horizontally distributed and located directly below the liquid inlet pipe; and a plurality of positioning columns are further fixed between the perforated plate and the top inner wall of the tank body.

[0018] Compared with the prior art, the utility model has the advantages that: the utility model adopts the static crystallization mode, that is, the benzotriazole crude product solution is placed in the tank body, and the temperature of the benzotriazole crude product solution is slowly and uniformly reduced by the cooling medium in the temperature adjusting assembly to realize the precipitation of the benzotriazole crystal; since the benzotriazole crude product solution is in a relatively static state, it is very beneficial to the growth and purification of the crystal, thereby effectively improving the morphological stability of the benzotriazole crystal; at the same time, the temperature, concentration and other conditions of the crystallization are easy to control, thereby obtaining the benzotriazole crystal with high purity and effectively improving the yield; in addition, the structure is simple, the volume is small, the cost is low, it is suitable for large-scale production and small-scale production, thereby having a larger application range. BRIEF DESCRIPTION OF DRAWINGS

[0019] Fig. 1 It is a left front side overhead exploded structure diagram of the utility model;

[0020] Fig. 2 It is a right rear side overhead exploded structure diagram of the utility model;

[0021] Fig. 3 It is a left front side structure diagram of the temperature adjusting assembly of the utility model;

[0022] Fig. 4 It is a left front side exploded structure diagram of the temperature adjuster of the utility model. DETAILED DESCRIPTION

[0023] Unless otherwise defined, technical terms or scientific terms used in the present application shall have the ordinary meaning as understood by a person of ordinary skill in the art to which the present application pertains. The terms "first", "second", and similar terms in the present application do not denote any order, quantity, or importance, but are merely used to distinguish different components. The terms "comprising" or "including" or similar terms mean that the elements or objects before the term encompass the elements or objects listed after the term and their equivalents, without excluding other elements or objects. The terms "connected" or "linked" or similar terms are not limited to physical or mechanical connections, but can include electrical connections, whether direct or indirect. The terms "upper", "lower", "left", "right", and the like are merely used to indicate relative positional relationships, which can change accordingly when the absolute positions of the described objects change.

[0024] In order to keep the following description of the embodiments of the present application clear and concise, detailed descriptions of known functions and known components are omitted.

[0025] As shown in Figs. 1-4 A static crystallizer of benzotriazole comprises a bottom frame 1, a box body 2 fixed inside the bottom frame 1, a liquid inlet pipe 3 vertically inserted at the top of the box body 2 and in communication with the inside of the box body 2, a liquid outlet pipe 4 horizontally inserted below one side of the box body 2 and in communication with the inside of the box body 2, a discharge pipe 5 vertically inserted at the bottom of the box body 2 and in communication with the inside of the box body 2, and at least one temperature adjusting assembly 6 arranged inside the box body 2.

[0026] The temperature adjusting assembly 6 comprises a plurality of temperature adjusters 61 vertically arranged and equally spaced from front to back, and two liquid guiding units arranged above the plurality of temperature adjusters 61 and in central symmetry.

[0027] The liquid guiding unit comprises a first shunt pipe 62 and a second shunt pipe 64 horizontally arranged and parallel to each other, a plurality of through pipes 63 horizontally arranged between the first shunt pipe 62 and the second shunt pipe 64 and equally spaced along the length direction of the first shunt pipe 62 or the second shunt pipe 64, and an external pipe 65 vertically inserted on the second shunt pipe 64 and in communication with the inside of the second shunt pipe 64, the end opening of the external pipe 65 is sealed upward through the top of the box body 2 and extends above the box body 2, and the two end openings of each through pipe 63 are respectively inserted on the first shunt pipe 62 and the second shunt pipe 64 and in communication with the inside of the first shunt pipe 62 and the second shunt pipe 64.

[0028] The temperature adjuster 61 comprises a plate-shaped circulating box 611 vertically arranged, and two connecting pipes 612 vertically inserted at the top of the plate-shaped circulating box 611 and in communication with the inside of the plate-shaped circulating box 611 and respectively distributed left and right.

[0029] The end opening of one of the connection pipes 612 in each temperature regulator 61 is inserted into the first shunt pipe 62 in one of the liquid guide units and communicates with the interior of the first shunt pipe 62, and the end opening of the other connection pipe 612 in each temperature regulator 61 is inserted into the first shunt pipe 62 in the other liquid guide unit and communicates with the interior of the first shunt pipe 62.

[0030] The interior of the plate-shaped circulation tank 611 is also fixed with a vertical partition plate 613, which divides the interior of the plate-shaped circulation tank 611 into two front and back symmetrical shunt cavities 6111 with equal volumes, and the root opening of each connection pipe 612 communicates with the interior of the two shunt cavities 6111.

[0031] The interior of each shunt cavity 6111 is also provided with a drainage module, which includes a rectangular frame 614 fixed between the corresponding side outer wall of the partition plate 613 and the corresponding side inner wall of the plate-shaped circulation tank 611, and an L-shaped baffle 615 arranged in the interior of the rectangular frame 614, one end of the L-shaped baffle 615 is fixed on the upper inner wall of the rectangular frame 614, the other end of the L-shaped baffle 615 is arranged towards the left or right inner wall of the rectangular frame 614 and spaced a certain distance from the left or right inner wall of the rectangular frame 614, the L-shaped baffle 615 divides the interior of the shunt cavity 6111 into an L-shaped flow channel 618 and a rectangular cavity 619, and the root openings of the two connection pipes 612 respectively communicate with the interiors of the L-shaped flow channel 618 and the rectangular cavity 619.

[0032] The interior of the rectangular cavity 619 is also provided with a plurality of first straight baffles 616 transversely distributed and arranged in sequence from top to bottom, one end of each first straight baffle 616 is fixed on the right or left inner wall of the rectangular frame 614, and the other end of each first straight baffle 616 is spaced a certain distance from the right or left outer wall of the L-shaped baffle 615.

[0033] The upper side of each first straight baffle 616 is also provided with a second straight baffle 6112 transversely distributed, each second straight baffle 6112 is arranged in the interior of the rectangular cavity 619, one end of each second straight baffle 6112 is fixed on the right or left outer wall of the L-shaped baffle 615, and the other end of each second straight baffle 6112 is spaced a certain distance from the right or left inner wall of the rectangular frame 614.

[0034] The plurality of first straight baffles 616 and the plurality of second straight baffles 6112 form a serpentine flow channel 6110 in the interior of the rectangular cavity 619.

[0035] A plurality of evenly distributed sunken cavities 61101 are formed on the front and back outer walls of the plate-shaped circulation tank 611.

[0036] The plate-shaped circulation box 611 is also fixed with a protective frame 617, and two connecting pipes 612 are inserted and connected to the upper side of the protective frame 617.

[0037] A top frame 7, which covers the outer perimeter of the top of the box body 2, is also fixed at the top opening of the bottom frame 1.

[0038] The interior of the housing 2 is also provided with a perforated plate 8 that is horizontally distributed and located directly below the liquid inlet pipe 3. Multiple positioning posts 9 are also fixed between the perforated plate 8 and the top inner wall of the housing 2.

[0039] Several vertically arranged exhaust pipes 10 are also inserted into the top of the housing 2, all of which are connected to the interior of the housing 2.

[0040] Several sampling tubes 11, which are arranged horizontally and are all connected to the interior of the box 2, are also inserted into the outer side wall of the box 2.

[0041] Working principle:

[0042] The crude benzotriazole solution is introduced into the tank 2 through the inlet pipe 3. Due to the perforated plate 8, the crude benzotriazole solution entering the tank 2 will first contact the perforated plate 8 and be diverted by the holes in the perforated plate 8, thereby reducing the flow rate and impact force of the crude benzotriazole solution until the liquid level of the crude benzotriazole solution in the tank 2 is higher than the temperature controller 61 in each temperature control component 6. At this time, the drain pipe 4, the discharge pipe 5, each exhaust pipe 10 and each sampling pipe 11 are all in a closed state.

[0043] Cooling medium is introduced into the outer pipe 65 of one of the liquid guiding units in at least one temperature regulating component 6, and then enters the first branch pipe 62 through the second branch pipe 64 and each connecting pipe 63 in the liquid guiding unit. It then enters the plate-shaped circulation box 611 through one of the connecting pipes 612 in each temperature regulator 61, and is then divided into two streams by the partition 613 and enters two branch chambers 6111 respectively. Next, the cooling medium in each branch chamber 6111 enters the rectangular cavity 619 through the L-shaped flow channel 618, and then enters another connecting pipe 612 after flowing through the serpentine flow channel 6110. It then merges into the first branch pipe 62 in another liquid guiding unit, and then enters the outer pipe 65 through each connecting pipe 63 and the second branch pipe 64 for outward return, thereby achieving circulating cooling.

[0044] In the process of circulating the cooling medium, the benzotriazole crude product solution in the box 2 can enter the space between any two adjacent temperature regulators 61, and then the heat of the benzotriazole crude product solution is fully conducted to each temperature regulator 61, so that the circulating cooling medium takes away the heat to realize the process of cooling and precipitating benzotriazole crystals; in addition, since the front and rear outer walls of the plate-shaped circulating box 611 are formed with a plurality of uniformly distributed sink cavities 61101, the benzotriazole crude product solution also fills in each sink cavity 61101, thereby increasing the contact area of the benzotriazole crude product solution and the temperature regulator 61.

[0045] The precipitated benzotriazole crystals are deposited at the bottom of the box 2, and when the precipitated benzotriazole crystals reach a certain amount, the drain pipe 4 can be opened to discharge the upper layer of residual liquid in the box 2 to the outside and into the filtering equipment to separate a small amount of benzotriazole crystals; then the discharge pipe 5 can be opened to discharge a large amount of benzotriazole crystals deposited at the bottom of the box 2 to the outside to the filtering equipment to separate the benzotriazole crystals.

[0046] The utility model adopts the static crystallization mode, that is, the benzotriazole crude product solution is placed in the box 2, and the cooling medium in the temperature regulating assembly 6 slowly and uniformly reduces the temperature of the benzotriazole crude product solution to realize the precipitation of benzotriazole crystals, since the benzotriazole crude product solution is in a relatively static state, it is very beneficial to the growth and purification of the crystals, thereby effectively improving the morphological stability of the benzotriazole crystals, and the temperature, concentration and other conditions of the crystallization are easy to control, thereby obtaining benzotriazole crystals with high purity and effectively improving the yield; in addition, the structure is simple, small in size and low in cost, suitable for large-scale production and small-scale production, thereby having a wide range of applications.

[0047] Finally, it should be noted that: the above examples are only used to illustrate the technical solutions of the utility model, but not to limit them; although the utility model has been described in detail with reference to the foregoing examples, those skilled in the art should understand that they can modify the technical solutions recorded in the foregoing examples, or make equivalent replacement for part of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the utility model.

Claims

1. A static crystallizer of benzotriazoles, characterized in that, The device comprises a bottom frame, a box fixed inside the bottom frame, a liquid inlet pipe vertically inserted into the top of the box and communicating with the inside of the box, a liquid outlet pipe horizontally inserted into the lower side of the box and communicating with the inside of the box, a discharge pipe vertically inserted into the bottom of the box and communicating with the inside of the box, and at least one temperature adjusting assembly arranged in the inside of the box. The temperature adjusting assembly comprises a plurality of temperature adjusters vertically arranged and equally spaced from front to back, and two liquid guiding units arranged above the temperature adjusters and symmetrically distributed. The liquid guiding unit comprises a first shunt pipe and a second shunt pipe horizontally arranged and parallel to each other, a plurality of through pipes horizontally arranged between the first shunt pipe and the second shunt pipe and equally spaced along the length direction of the first shunt pipe or the second shunt pipe, and an external pipe vertically inserted into the second shunt pipe and communicating with the inside of the second shunt pipe, the end opening of the external pipe is upwardly sealed through the top of the box and extends above the box, and the two end openings of each through pipe are respectively inserted into the first shunt pipe and the second shunt pipe and communicate with the inside of the first shunt pipe and the second shunt pipe. The temperature adjuster comprises a plate-shaped circulating box vertically arranged, and two connecting pipes vertically inserted into the top of the plate-shaped circulating box and communicating with the inside of the plate-shaped circulating box and respectively distributed on the left and right sides. The end opening of one of the connecting pipes in each temperature adjuster is inserted into the first shunt pipe in one of the liquid guiding units and communicates with the inside of the first shunt pipe, and the end opening of the other connecting pipe in each temperature adjuster is inserted into the first shunt pipe in the other liquid guiding unit and communicates with the inside of the first shunt pipe.

2. A static crystallizer of benzotriazoles according to claim 1, characterized in that, The inside of the plate-shaped circulating box is further fixed with a partition plate vertically arranged, the partition plate divides the inside of the plate-shaped circulating box into two shunt cavities symmetrically arranged from front to back and having equal volumes, and the root openings of the two connecting pipes communicate with the inside of the two shunt cavities.

3. A static crystallizer of benzotriazoles according to claim 2, characterized in that, The inside of each shunt cavity is further provided with a drainage module, the drainage module comprises a rectangular frame fixed between the corresponding side outer wall of the partition plate and the corresponding side inner wall of the plate-shaped circulating box, and an L-shaped baffle arranged in the inside of the rectangular frame.

4. A static crystallizer of benzotriazoles according to claim 3, characterized in that, One end of the L-shaped baffle is fixed on the upper side inner wall of the rectangular frame, the other end of the L-shaped baffle is arranged towards the left side or right side inner wall of the rectangular frame and spaced a certain distance from the left side or right side inner wall of the rectangular frame, and the L-shaped baffle divides the inside of the shunt cavity into an L-shaped flow channel and a rectangular cavity, and the root openings of the two connecting pipes respectively communicate with the inside of the L-shaped flow channel and the rectangular cavity.

5. A static crystallizer of benzotriazoles according to claim 4, characterized in that, The inside of the rectangular cavity is further provided with a plurality of first linear baffles horizontally distributed and arranged in sequence from top to bottom, one end of each first linear baffle is fixed on the right side or left side inner wall of the rectangular frame, and the other end of each first linear baffle is spaced a certain distance from the right side or left side outer wall of the L-shaped baffle.

6. A static crystallizer of benzotriazoles according to claim 5, characterized in that, The upper side of each first straight baffle is also provided with a second straight baffle which is horizontally distributed, each second straight baffle is arranged inside the rectangular cavity, one end of each second straight baffle is fixed on the right or left outer wall of the L-shaped baffle, and the other end of each second straight baffle is spaced apart from the right or left inner wall of the rectangular frame by a certain distance.

7. A static crystallizer of benzotriazoles according to claim 6, characterized in that, The first straight baffles and the second straight baffles form a serpentine flow channel inside the rectangular cavity.

8. A static crystallizer of benzotriazoles according to claim 1, characterized by the fact that, A plurality of evenly distributed sink cavities are formed on the front and rear outer walls of the plate-shaped circulating tank.

9. A static crystallizer of benzotriazoles according to claim 1, characterized by the fact that, A protection frame is further fixed outside the plate-shaped circulating tank, and the two connecting pipes are connected to the upper side of the protection frame.

10. The static crystallizer of a benzotriazole according to claim 1, characterized by, A top frame is further fixed on the top of the box and covers the outer periphery of the top of the box, a hole plate is further arranged inside the box and horizontally distributed and located directly below the liquid inlet pipe, and a plurality of positioning columns are further fixed between the hole plate and the top inner wall of the box.

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